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2K views189 pages

PackedColumn PDF

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amadan64
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You are on page 1/ 189

PACKED COLUMN

TECHNOLOGY

ChevronTexaco Energy Research and Technology


Company

Richmond, California

August 2002
PRINTING HISTORY

PACKED COLUMN TECHNOLOGY

First Edition June 1994


Reprinted August 2002

Restricted Material
Technical Memorandum

This material is transmitted subject to


the Export Control Laws of the United
States Department of Commerce for
technical data. Furthermore, you hereby
assure us that the material transmitted
herewith shall not be exported or re-
exported by you in violation of these
export controls .
This publication was developed by A. E. Ravicz of the ChevronTexaco
Energy Research and Technology Process Engineering Team as part of
the Distillation Expert/Technology Transfer Program sponsored by CUSA
Refining and Chevron Chemical. Sections were issued separately as
each was finished, beginning in January 1992. General updating was
done before issue of this combined edition. Publishing services were
provided by CRTC’s Technical Standards Team.

Copyright  1994, 2002 ChevronTexaco Corporation. All rights reserved. This


document contains proprietary information for use by ChevronTexaco Corporation, its
subsidiaries and affiliates. All other uses require written permission.
Table of Contents
Section 100 Packing Capacity and Pressure Drop 1
110 Introduction ................................................................................................1
120 Design Recommendations........................................................................2
130 Packing Hydraulics....................................................................................2
140 General Pressure Drop Models for Random Packings .........................3
150 General Pressure Drop Models for Structured Packings .....................3
160 Performance of Grids................................................................................4
170 Computer Programs Available from Vendors........................................5
171 "Glitsch Tray and Packing Design/Rating Program"......................... 5

172 "Koch Tower Design, Tray and Packing Rating Software"................ 5

173 "Norton Packed Tower Design Program" ......................................... 6

174 "Nutter Electronic Design Manual" ................................................... 6

180 Computer Programs from Other Sources................................................7


190 References ..................................................................................................7
Tables and Figures ................................................................................................9
Appendix 100-A Random Packing Pressure Drop Program...........................14
Appendix 100-B Structured Packing Pressure Drop Program .......................18

Section 200 Efficiency of Packed Columns 25


210 Introduction ..............................................................................................25
220 HETP Versus Loading ...............................................................................26
230 Efficiency Data from Plant Columns .....................................................26
240 Laboratory and Pilot-Plant Efficiency Data ..........................................27
241 Derating for "Plant Environment" ................................................... 27
242 Accounting for Bed Depth .............................................................. 27

243 Effect of Density of Liquid Distribution Points................................ 28

244 Adjusting Random-Packing Efficiency for Packing Size................. 28

245 Adjusting Structured-Packing Efficiency for Packing Size ............. 29

246 Adjusting Efficiency for a Change of System ................................. 30


250 Predicting Efficiency in the Absence of Data.......................................30
251 Rough Rules................................................................................... 30

252 Simple Correlations for Packing Efficiency .................................... 30

253 Rigorous Correlations for Packing Efficiency................................. 31

254 Computer Programs for Packing Efficiency.................................... 32

260 References................................................................................................33
Tables and Figures ..............................................................................................34
Appendix 200-A FRI Random-Packing Efficiency Program............................37
Appendix 200-B Structured-Packing Pressure-Drop and
Efficiency Program ..................................................................................41

Section 300 Liquid And Vapor Distributors for Packed Columns 48


310 Introduction ..............................................................................................48
311 Importance of Good Distribution .................................................... 48

312 Good Liquid Distribution Defined ................................................... 49

320 Types of Liquid Distributors...................................................................50


321 Pan Distributor................................................................................ 50

322 Trough Distributor .......................................................................... 50

323 Combination ................................................................................... 51

324 Manifold or "Ladder" Distributor .................................................... 51

325 Spray Distributor ............................................................................ 51

330 Liquid Distribution Practice....................................................................52


331 Placement of Liquid Distributors.................................................... 52

332 Liquid Flow Control and Turndown ................................................ 52

333 Design Equations ........................................................................... 53

334 Liquid Redistribution ...................................................................... 54

340 Vapor Distribution Background.............................................................54


341 The Energy of a High Velocity Stream ............................................ 55

342 Pressure Drop Through Risers....................................................... 55

343 Free Jet Behavior............................................................................ 56

350 Vapor Distribution Practice ....................................................................56


351 When Internal Vapor Distributors are Needed ................................ 56

352 Clearance Above Vapor Entry......................................................... 57


353 Proposed Practice and Example Problem....................................... 57

354 Entrainment of Liquid by Vapor Below a Bed ................................. 58

360 Stream Entries to Columns.....................................................................59


361 Liquid Stream Entry ........................................................................ 59

362 Vapor Stream Entry ........................................................................ 59

363 Two-Phase Stream Entry ................................................................ 59

364 Line Sizes ....................................................................................... 61

365 Manifolds ........................................................................................ 61

366 Maximum Discharge Velocity ......................................................... 62

370 References................................................................................................62
Figures and Drawings .........................................................................................63

Section 400 Selection, Specification, Bid Review and Inspection 69


410 Introduction ..............................................................................................69
420 Packing vs Trays......................................................................................69
430 Packing Selection ....................................................................................69
431 Structured Packing vs Random Packing ........................................ 69

432 When to Consider Grid ................................................................... 70

433 Which Size Packing? ...................................................................... 70

434 Efficiency (Hetp) Estimation ........................................................... 70

440 Suppliers and Brand Names of Packing ...............................................71


450 Specifying a Packing Installation...........................................................71
451 New Construction and Major Revamps........................................... 71

452 Smaller Projects ............................................................................. 72

460 Reviewing Bids and Budget Cost Estimates........................................72


470 Reviewing Detailed Designs...................................................................73
471 Column (Vessel) Drawing ............................................................... 73

472 Installation Drawing........................................................................ 74

473 Liquid (Gravity) Distributor Drawings ............................................. 74

474 Spray Distributor Drawings ............................................................ 75

475 Hold-Down Plate and Bed-Limiter Drawings................................... 76

476 Packing Support Tray Drawings..................................................... 76


477 Collector/Drawoff Tray Drawings.................................................... 77

478 Grid Installation Drawings .............................................................. 77

480 Process Inspection ..................................................................................78


481 Recommended Equipment.............................................................. 78

482 In General ....................................................................................... 78

483 Gravity Distributors ........................................................................ 79

484 Spray Distributors........................................................................... 79

485 Hold-Down Plates and Bed Limiters ............................................... 79

486 Packing Support Trays ................................................................... 79

487 Collector/Drawoff Trays.................................................................. 79

488 Grid Installations ............................................................................ 80

490 References................................................................................................80
Tables and Figures ..............................................................................................81
Appendix 400-A Packed Tower Data Sheet and Process Specifications......83

Section 500 Packed-Column Troubleshooting and Testing 92


510 Introduction ..............................................................................................92
520 Tools for Diagnosing Problems.............................................................92
530 Organization of Troubleshooting Material............................................93

540 Symptoms and The Possible Mechanisms Causing Them ................93


541 Symptom: Column Does Not Make the Expected Separation ......... 93

542 Symptom: Column Product Rates are Unsteady............................. 94

543 Symptom: Column Pressure Drop i s Higher than Expected and/or


Unsteady......................................................................................... 94
544 Symptom: Column Operating (Top) Pressure is Unsteady ............. 95

545 Symptom: Column Condenser is out of Heat Balance.................... 95

550 Mechanisms and the Conditions Causing Them .................................95


551 Mechanism: Packing Has Lower Capacity (Higher Pressure Drop)
than It Should ................................................................................. 95
552 Mechanism : Packing Has Lower Efficiency than It Should; Capacity
is Okay............................................................................................ 95
553 Mechanism: Liquid Distribution is Poor.......................................... 96

554 Mechanism: Vapor Distribution is Poor .......................................... 96


555 Mechanism: Liquid i s Held Up On Packing Support Plate .............. 96

556 Mechanism: High Pressure Drop in Chimneys ............................... 96

557 Mechanism: Liquid is Entrained Out of the Top of the Column ...... 96

560 Fixes for the Most Common Conditions...............................................97


561 Condition: Plugging of Liquid Distributors and Packing ................ 97

562 Condition: Collapse, Softening, Breakage of Random Packing...... 97

563 Condition: Excessive Bed Depth .................................................... 97

570 Conducting a Test Run ...........................................................................97


580 Analyzing Test Data.................................................................................98
581 Material Balance ............................................................................. 98

582 Heat Balance................................................................................... 98

583 Making the Computer Model........................................................... 99

584 An Alternative Computer Model...................................................... 99

585 Comparing Computed Separation with Test Data ........................... 99

586 Computing Packing Loading ........................................................ 100

590 References..............................................................................................102
Appendix 500-A Testing of Plant Scale Distillation Columns ......................103
Appendix 500-B Performance Evaluation Rlop Hnc Vacuum Column........128

Section 600 Packed Liquid/Liquid Extraction Guide 140


610 Introduction ............................................................................................140
620 Comparison of Flooding Models..........................................................140
621 Norton Correlations (9, 11, 15)...................................................... 141

622 Seibert and Fair Correlation (13,14) .............................................. 142

623 Results and Discussion ................................................................ 142

630 Phase Separation Considerations .......................................................142


640 Packed Liquid/Liquid Extraction Flooding Design and Rating
Program, "LLFLOOD"............................................................................143
650 Interfacial Tension .................................................................................143
660 Mass-Transfer Considerations.............................................................144
670 Extraction Column Internals.................................................................144
671 Packing Size................................................................................. 144
672 Packing Material and Wetting Characteristics .............................. 145

673 Packing Shapes............................................................................ 145

674 Vessel Outline Drawings............................................................... 145

675 Packing Support Plates ................................................................ 145

676 Distributors................................................................................... 146

677 Redistributors............................................................................... 146

678 Bed Limiters ................................................................................. 146

679 Coalescing Pads........................................................................... 146

680 References..............................................................................................146
Tables and Figures ............................................................................................148
Appendix 600-A Other Flooding Models.........................................................162
Appendix 600-B More Information on the Seibert and Fair Model...............167
Appendix 600-C Prediction of Interfacial Tension .........................................170
Section 100 Packing Capacity and Pressure Drop

110 Introduction
This section presents
• Methods for predicting pressure drop in packings
• Recommendations on maximum design pressure drops when sizing columns or choosing
among alternative sizes of packin gs.
Models for the flooding point or for maximum usable capacity are not contained here; these
points are difficult to define and identify and have not been correlated satisfactorily. Designing
for a given percentage of flooding or maximum usable capacity is not recommended.
The actual pressure change through the packing of a packed bed in normal operation (ignoring
other internals such as support plates and distributors) is the sum of the "friction loss" through the
bed plus the head of (continuous phase) vapor in the column. Ordinarily, the second term is
negligible and is ignored; however, in high pressure columns it is significant. The prediction
methods and design recommendations given here relate only to frictional pressure drop.
Prediction of pressure drop in packings is not nearly as exact as in the case of trays. Results from
the various models vary significantly. The method in which a column is loaded (wet or dry), even
a change in dry loading technique affects pressure drop. Most laboratory data are for air-water;
where hydrocarbon system data are available, most is from low pressure operations. In this
author's experience, correlations generally underestimate the pressure drop that occurs in higher
pressure applications.
Packings are usually classified as
• Random or "dumped" packings.
• Sheet metal structured packings.
• Structured packings made of knitted or woven wire.
• Grid packings.
The term "structured packing" is usually reserved for only the sheet metal types, such as Gempak
(Glitsch), Max-Pak (Jaeger), Flexipac (Koch), Intalox Structured Packing (Norton), Montz
Structured Packing (sold in the U.S. by Nutter), and Mellapak (Sulzer, in Europe).
In this section, random packings are restricted mainly to metal rings, the type most often used in
ChevronTexaco installations. Metal ring packings fall into three categories, as follows:
• P: The original generic Pall rings (Norton), also known as Ballast rings (Glitsch) and
Flexirings (Koch).
• IP: "Improved" Pall rings, made of thinner metal and in slightly larger sizes than the
original, with ribs to reinforce the thinner metal.
• M: Modern ring packings, which offer small but significant capacity/efficiency
advantages over the first two categories.
Metal ring packings are listed in Table 100-1.

August 2002 © 2002 ChevronTexaco Corporation — CONFIDENTIAL Page 1 of 180


Packed Column Technology 100 Packing Capacity and Pressure Drop

120 Design Recommendations


For random packings, the maximum recommended pressure drop at the design point is 0.5 inches
of water column per foot of packing.
For structured packings in vacuum service, the maximum recommended pressure drop at the
design point is 0.3 in. wc per ft of packing.
For structured packings in service at pressures from atmospheric up to 100 psia (vapor density
around 1.0 lb/ft3 ), the maximum recommended pressure drop at the design point is 0.4 in. wc per
ft of packing.
Ask the vendor to confirm the estimated pressure drops before a design is finalized. In-house
correlations may be different from those in the vendor's brochure or computer program.
The best source of capacity/pressure drop information is a pilot plant test with packing and
process conditions as close as possible to those in the design. Ask the vendor for the data.
Structured packings are not recommended for distillation service at pressures above 100 psia or
liquid loads above 20 gpm/sq ft. A significant loss of efficiency has been observed at loadings
within the usual design range. (Note: structured packing has performed well in gas treating
applications at high pressure.)
Packed columns should not be designed based on percentage of maximum usable capacity or
flooding.

130 Packing Hydraulics


The ideal loading effects in packing are given in Figure 100-1. In the lower portion, pressure drop
is plotted on a log scale versus vapor rate, also on a log scale. The upper portion shows height
equivalent to a theoretical plate (HETP), the inverse of efficiency.
If the packing is dry, the pressure drop is described by a straight line with a slope of around 1.8.
If a constant low liquid loading is applied and the vapor rate is then raised from zero, the pressure
drop curve is initially parallel to the first curve and displaced upward. The increased pressure
drop is caused by liquid filling some of the void space of the packing (liquid holdup). The
quantity of liquid holdup and the displacement are functions only of the liquid load, not the vapor.
As vapor rate continues to increase, a point is reached where the pressure drop curve begins to
steepen. Fractionation Research, Inc. (FRI) calls this the "hydraulic transition point", but industry
practice is not uniform. From this point on, liq uid holdup is also a function of vapor rate. For
some distance beyond the hydraulic transition, the column may still have stable operation and
good efficiency.
As vapor rate increases further, the pressure drop curve continues to steepen. HETP, which
(ideally) has been constant up to this point, may then go through a minimum (maximum
efficiency) point before suddenly increasingrapidly. This point is sometimes called the "load
point". The vapor loading at which HETP again passes through its earlier value on the way up is
sometimes called the "maximum operating point" or "maximum usable capacity". In actual
operating data, these last two points are usually indistinguishable from one another.
In short order the pressure drop curve approaches the vertical and the column floods. The
pressure drop corresponding to flooding is indeterminate.
For a higher constant liquid loading, the initial portion of the pressure drop curve is displaced
higher yet, the hydraulic transition is reached at a lower value of vapor rate, and flooding also

August 2002 © 2002 ChevronTexaco Corporation — CONFIDENTIAL Page 2 of 180


Packed Column Technology 100 Packing Capacity and Pressure Drop

occurs earlier. At sufficiently high liquid loading, no portion of the pressure drop curve is below
the hydraulic transition.
The most comprehensive pressure drop models, to be described later, are based on the above
description.

140 General Pressure Drop Models for Random Packings


The best known model is the Generalized Pressure Drop Correlation (GPDC), also known as the
Sherwood-Eckert-Norton chart. The most recent version appears in References 1, 2, and 3. In
Figure 100-2 (taken from Reference 2) variables used as axes are defined. Capacities of various
packings are related to one another through the packing factor, F, which is listed as "Coefficient
F".
Table 100-1 contains packing factors for the more common metal ring packings used in
ChevronTexaco plants. Table 100-2 covers some older packings still in use. The GPDC has
limited accuracy; some authors have recommended one packing factor for a given packing at high
liquid loadings, another for low liquid loadings; one factor for vacuum systems, another for above
atmospheric pressure, etc. This correlation is simple and well known, and suitable for rough
estimates. See Section 173 for further detail.
The packing factor used in the GPDC serves as an approximate way to relate capacities of the
various packings. At given values of liquid:vapor ratio and pressure drop, capacities of two
packings are in inverse proportion to the square roots of their packing factors. For example, a
packing with F=10 has twice the capacity as one with F=40.
The Robbins correlation (4) is of the GPDC type with many of the same limitations.
Several vendors include column sizing information in a form similar to Figure 100-1 in their sales
brochures (5, 6, 7, 8). This too is for rough estimates.
FRI has released two random packing models (9, 10):
• The earlier one, contained in Topical Report 95, is in the FRI Design Handbook and in
both the main-frame and PC versions of the Packed Tower Rating Program, RPK.
• The second FRI model, TR 104, is an improvement over the first, and probably the best
general correlation available, but still not entirely satisfactory. Its data base does not
include high pressure data. This author has patched it in such a way that it agrees with
some FRI high pressure data. The model should be considered a reference rather than a
design tool for metal ring packings. It is available as a BASIC program for personal
computers. A listing is in Appendix 100-A.

150 General Pressure Drop Models for Structured Packings


Kister and Gill (11) developed a ve rsion of the GPDC for structured packings. Figure 100-3 was
replotted from a figure in that article. The abscissa of Figure 100-3, labeled "Flow Parameter", is
the same as the abscissa of Figure 100-2 for random packings. The ordinate of Figure 100- 3,
labe led "Capacity Parameter", is exactly equal to the square root of "Y", the quantity on the
ordinate of Figure 100-2 for random packings. (If the same quantity had been used, the figures
would be very similar.) Nomenclature is in Figure 100-2. Packing factor s for structured packings
are in Table 100-3.
The GPDC for structured packings has the same drawbacks as the one for random packings. To
improve accuracy, Reference 11 contains eight charts in which source data for a specific packing

August 2002 © 2002 ChevronTexaco Corporation — CONFIDENTIAL Page 3 of 180


Packed Column Technology 100 Packing Capacity and Pressure Drop

are plotted. This allows the user to see how well the generalized chart fits the data and to make a
"second order" correction if necessary.
Again, vendors include column sizing information in their sales brochures (12, 13, 14, 15). This is
useful for rough estimates.
Bravo, Rocha, and Fair (16) published a general model for structured packing pressure drop in the
region below the load point. Unfortunately, that excluded the region of most design interest. The
authors tried again recently (17) with better success. The new model still did not fit available high
pressure data. This author then added an automatic adjustment for the effect of pressure. The
result is a rather cumbersome model, which is useful for reference rather than routine design use.
A BASIC program is available, listed in Appendix 100-B.

160 Performance of Grids


Vendors include rating correlations in their sales literature (18, 19, 20, 21). Since grids are
frequently used in heat transfer (pumparound section) service, heat transfer formulas presented by
Bigot (22) are included here.
Q = h•V•LMTD
where Q = heat transfer duty of a (partially condensing) pumparound reflux
section, Btu/hr
h = heat transfer coefficient, Btu/(hr•°F•ft3 )
V = volume of grid or other packing, ft3
LMTD = log mean of temperature differences between passing vapor and
liquid streams at top and bottom of bed
h = K•C0.8 •(L/A) 0.58

where K = 360 for Glitsch Grid


450 for 60-mm Ballast (Pall) Rings
600 for Gempak 2A
C = capacity factor = VS•[ρ V/(ρ L-ρ V)]0.5
L = liquid rate, gpm
A = column (bed) cross sectional area, ft2
VS = superficial vapor velocity, ft/sec
ρV = vapor density, lb/ft3
ρL = liquid density, lb/ft3

August 2002 © 2002 ChevronTexaco Corporation — CONFIDENTIAL Page 4 of 180


Packed Column Technology 100 Packing Capacity and Pressure Drop

170 Computer Programs Available From Vendors


Vendor programs can be very useful for preliminary work. In each case, the program rates only
that vendor's products. They usually come with elaborate disclaimers, are user friendly, and are
copy-protected. Descriptions and sources of several programs are given below.
Where FRI data are available for comparison with vendor program predictions, summaries of
these comparisons are given. In general, comparisons were made only at the upper end of the
pressure drop range of design interest. This is well above the hydraulic transition point described
in Section 130. The slope of the pressure drop curve in Figure 100-1 has increased significantly.
An error in pressure drop prediction of, for example, 30 to 40% would correspond to an error in
design loading of 10% and to an error in required diameter of 5%.
171 "Glitsch Tray and Packing Design/Rating Program"
The program was designed to do preliminary hydraulic designs for Glitsch's trays and packings.
Delivery has been delayed.
172 "Koch Tower Design, Tray and Packing Rating Software"
This program is available without charge from Koch Engineering Company Inc., 4111 East 37th
St. North, Wichita, Kansas 67220, telephone (316) 832-5110. The program rates Koch valve trays
and all of the packings marketed by Koch. Correlations used in the program are not revealed.
The random packing portion of the program was tested by comparing predicted pressure drops for
Flexirings (Pall rings) against FRI Pall ring data.
• For the cyclohexane/normal heptane system at 4 and 24 psia, predicted values were
50-60% of those observed.
• For the isobutane/normal butane system at pressures of 165 to 400 psia, predictions were
30% of those observed or lower yet.
The program might do better when rating Koch's more modern packings, but there are no
independently obtained data with which to make comparisons. The Koch program is not
recommended for random packings.
The structured packing portion of the Koch program was tested by making predictions for two
sizes of Flexipac, 1.6Y and 2Y, whose capacities are expected to bracket that of Mellapak 250.Y.
Results were compared with FRI data for Mellapak 250.Y. (Koch manufactures Flexipac under
license from Sulzer, maker of Mellapak. The two are similar.)
• With systems ranging from orthoxylene/paraxylene at 2 psia up to isobutane/normal
butane at 165 psia, predic tions for the two sizes of Flexipac did bracket the observed
Mellapak pressure drop in almost all cases; however, note that as the liquid loading of the
packing increased, the ratio of the two Flexipac pressure drops increased from 1.3 at
lowest pressure to a maximum ratio of 8.8 for a 165 psia case.
• In the next higher pressure system, butanes at 300 psia, the model was clearly beyond its
limits, all predictions being low by a factor of 2 to 5.
The Koch structured packing program is recommended for low to moderate pressures.

August 2002 © 2002 ChevronTexaco Corporation — CONFIDENTIAL Page 5 of 180


Packed Column Technology 100 Packing Capacity and Pressure Drop

173 "Norton Packed Tower Design Program"


This program is sold by Norton Chemical Process Products, P. O. Box 350, Akron, Ohio 44309,
telephone 216-673-5860. It rates all of the Norton packings. The 1988 version is the current one.
The instruction booklet, Reference 2, states that pressure drops for all packings, random and
structured, are calculated by the GPDC, 1985 revision.
Predicted pressure drops for Pall rings were compared to FRI test da ta.
• With cyclohexane/normal heptane at vacuum and moderate pressure, predictions were
adequate.
• With the butanes system at pressures of from 165 to 400 psia, predictions were low by 20
to 50%.
Predicted pressure drops for Intalox Structured Packing 2T were compared with FRI
measurements from a proprietary test of that packing. For this packing, the Norton program uses
a packing factor of 15.5 for operating pressures less than 10 psia and 20 for pressures above 10
psia.
• With the cyclohexane/normal heptane system at 24 psia, the program predictions were
high by a factor of 1.3 to 2.0.
• With the isobutane/normal butane system at 100 psia, the predictions were about right.
• With butanes at 165 psia, predictions were about 10% low.
• With butanes at 300 psia, predictions were 30-60% of measurements.
• With butanes at 400 psia, predictions were about 25% of measurements.
Reference 14, dated 1988, lists six packing factors for Intalox 2T, ranging from 19 to 34,
depending on liquid loading. These factors are not in the Norton program. Use of these liquid
load-dependent packing factors is not the answer to the problem detailed just above.
174 "Nutter Electronic Design Manual"
This rating program may be obtained without charge from Nutter Engineering, P. O. Box 700480,
Tulsa, OK 74170, telephone 918-446-6672. Version 2.0 is current. The method for rating random
packings is in Reference 8.
The program was tested against FRI data from tests of No. 2 and No. 2.5 Nutter Rings.
• Predictions compared very well for low and moderate pressure systems.
• At higher pressures, comparison was okay in total reflux operation, but the program
underpredicted by up to 40% at L/V of around 2.0.
• At the highest pressure tested, butanes at 400 psia, prediction was 20% low at total reflux.
• When tested against FRI data for Montz B1 200 structured packing, the Nutter program
predicted high by a factor of 2 to 5. Nutter's in-house program has been corrected and
will be revised for customers later.
In general, the Nutter program performed better on random packing than any other vendor
program. Although it rates only Nutter Ring random packing, others may be estimated by
interpolating between the packing factors shown in Table I00-1. The program in its present form is not
recommended for structured packings.

August 2002 © 2002 ChevronTexaco Corporation — CONFIDENTIAL Page 6 of 180


Packed Column Technology 100 Packing Capacity and Pressure Drop

180 Computer Programs From Other Sources


FRI has just released a PC version of its packed-column rating program. The program is menu-
driven and user-friendly. It contains FRI correlations for random-packing capacity, efficiency,
and pressure drop. The pressure drop model in this program is the older one, not the one in
Appendix 100-A.
Simulation Sciences Inc. markets PROCESS for main frame computers and PRO II for PCs. They
contain the GPDC (1, 2, 3) and also the Tsai correlation (23). These are for rough estimates.
HYSIM by Hyprotech contains the Robbins correlation (4), also for rough estimates.
The Separations Research Program (SRP) distributed "Packed Section Design", a PC program, in
1986. It contains the GPDC and other pressure drop correlations. It is rather inconvenient to use.
A program listing and instructions for use are in Reference 24.

190 References
1. Strigle, R. F., "Random Packings and Packed Towers", Gulf Publ. Co., Houston, 1987.
2. "Packed Tower Design Program Users Manual", Norton Co. Chemical Process Products,
P. O. Box 350, Akron, OH 44309.
3. Kister, H. Z., "Distillation Design", p. 493, McGraw Hill Inc., New York, 1992.
4. Robbins, L. A., Chem. Eng. Prog., May 1991, p 87-91.
5. Glitsch Bulletins 345 (Cascade Mini-Rings) and 217 (Ballast Rings).
6. Koch Bulletins KRP-2 (Random Packing), KFM- (Fleximax), and KPAC-1 (K-Pac).
7. Norton Bulletins IHP-1 (Intalox) and MTP-1 (Metal Tower Packing).
8. Nutter Bulletin NR-2 (Nutter Rings).
9. Fractionation Research, Inc., Topical Report 95, Dec. 1984.
10. Fractionation Research, Inc., Topical Report 104, Mar. 1988.
11. Kister, H. Z., and Gill, D. R., IChemE Symposium Series No. 128, p A109-123.
12. Glitsch Bulletin 5140 (Gempak).
13. Koch Bulletin KFP-4 (Flexipac).
14. Norton Bulletin IS-1 (1988) and unnumbered 1992 bulletin (Intalox Structured Packing).
15. Nutter Bulletin B-1 (Montz Structured Packings).
16. Bravo, J. L., Rocha, J. A., and Fair, J. R., Hydrocarbon Processing 65(3), 45 (1986).
17. Rocha, J. A., Bravo, J. L., and Fair, J. R., Ind. Eng. Chem. Res., 32, 641-51, (1993).
18. Glitsch Bulletin 423 (Glitsch Grid and Grid/Ring Combination).
19. Koch Bulletin KFG-2 (Flexigrid).
20. Norton Bulletin IG-1 (Intalox Grid-Type Packing).
21. Nutter Bulletin SG-1 (Snap-Grid).
22. Bigot, P. C., "Observed Heat Transfer Coefficient in Glitsch Grid at the Pascagoula FCC
Main Fractionator", Chevron Internal Report, 2/9/88.

August 2002 © 2002 ChevronTexaco Corporation — CONFIDENTIAL Page 7 of 180


Packed Column Technology 100 Packing Capacity and Pressure Drop

23. Tsai, T. C., Oil and Gas J. 9/2/85, 77-80.


24. Fair, J. R. and Bravo, J. L., "Design Manual: Packed Columns for Distillation, Absorption,
and Stripping", Separations Research Program, The University of Texas at Austin.
25. Koch Bulletin FS-1, 1981.

August 2002 © 2002 ChevronTexaco Corporation — CONFIDENTIAL Page 8 of 180


Packed Column Technology 100 Packing Capacity and Pressure Drop

Table 100-1 Parameters For Common Metal Ring Packings


Supplier Product Name Type Size Packing Factor Surface Area,ft-1
Glitsch Ballast Ring P 5/8 in. 70 109
1 in. 48 63
1.5 in. 28 39
2 in. 20 31
3.5 in. 15 19
Ballast Plus IP No. 2 17 30
Cascade Mini-Ring M 0 55 103 (est)
1 40 76
1.5 29 57
2 22 47
2.5 19 38
3 14 32
4 10 24
5 8 15
Koch Flexiring P 5/8 in 78 105
1 in. 45 65
1.5 in. 28 40
2 in. 22 35
3.5 in. 18 28
K-Pac IP No. 1 42 54
No. 1.5 24 37
No. 2 17 28
No. 3 15 21
HcKp IP No. 1 32 (est) 27 (est)
No. 1.5 21 (est) 12 (est)
No. 2 19 (est) 9 (est)
No. 3 18 (est) 8 (est)
Fleximax M No. 300 24 (est) 41 (est)
No. 400 19 (est) 33 (est)
Norton Pall Ring P 5/8 in. 81 104
1 in. 56 63
1.5 in. 40 39
2 in. 27 31
3.5 in. 18 17
Hy-Pak IP No. 1 45 53
No. 1.5 29 35
No. 2 26 26
No. 3 16 12 (est)
Intalox Metal Tower Packing (IMTP) M No. 15 51 80 (est)
No. 25 41 62
No. 40 24 46
No. 50 18 30
No. 70 12 20 (est)
Nutter Nutter Ring M No. 0.7 44 (est) 77 (est)
No. 1.0 30** 52 (est)
No. 1.5 24** 41 (est)
No. 2.0 18** 30 (est)
No. 2.5 16 (est) 27 (est)
No. 3.0 12 (est) 20 (est)
* Types: P = Pall, IP = Improved Pall, M = Modern
** From Ref 4.

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Packed Column Technology 100 Packing Capacity and Pressure Drop

Table 100-2 Parameters For Older Random Packings


Supplier Product Name Size Packing Factor Surface Area,ft-1
Koch Raschig Ring (Metal, 1/16") 3/4 in. 185 81
1 in. 115 62
1-1/4 in. 110 48
1-1/2 in. 83 39
2 in. 57 29
3 in. 32 20
Koch Raschig Ring (Ceramic) 3/4 in. 255 74
1 in. 160 58
1-1/4 in. 125 45
1-1/2 in. 100 37
2 in. 65 28
3 in. 37 19
Koch Flexisaddles (Ceramic) 3/4 in. 145 102
1 in. 98 78
1-1/2 in. 52 59
2 in. 40 36
3 in. 22 28
Source: Reference 25

Table100-3 Parameters For Structured Packings


Supplier Product Name Size Packing Factor* Surface Area, ft-1
Glitsch Gempak 4A 32 138
3A 21 91
2A 16 68
1.5A 12 49
1A 9 35
0.5A 6 22 (est)
Jaeger Max-Pak 12 69
Koch Flexipac No. 1 30 170
No. 2 13 75
No. 3 8 33
No. 4 6 17
Nutter Montz Structured Packing B1-300 33 91
B1-250 20 76
B1-200 18 (est) 67
B1-100 11 (est) 30
BSH-250 19 (est) 73
Norton Intalox Structured Packing 1T 26 115 (est)
2T 17 65
3T 13 44 (est)
5T 10 27
Sulzer Mellapak 500.Y 34 152
350.Y 23 107
250.Y 20 79
125.Y 10 35
For use only with the Kister-Gill correlation.

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Packed Column Technology 100 Packing Capacity and Pressure Drop

Figure 100-1 Effect of Loading on Pacing Efficiency and Pressure Drop

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Packed Column Technology 100 Packing Capacity and Pressure Drop

Figure 100-2 Generalized Pressure Drop Correlation

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Packed Column Technology 100 Packing Capacity and Pressure Drop

Figure 100-3

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APPENDIX 100-A
RANDOM PACKING PRESSURE DROP PROGRAM
The program, written in GWBASIC, is based on a Pall-ring, pressure drop procedure contained in
Fractionation Research, Inc. (FRI) Topical Report 104 of March, 1988. Note that information
received from FRI is Confidential under terms of ChevronTexaco's membership agreement. This
information should not be distributed outside the Company.
The procedure contains models:
• For the load point described in Section 120.
• For the very high degree of vapor liquid interaction that occurs as the flooding point is
approached.
Packing-related parameters are as follows:
• The packing particle size (in.).
• The specific area (ft2 /ft3 ).
• The void fraction (or porosity).
If the packing is, in fact, one of the sizes of Pall rings, then the user may enter just the particle
size; the program will supply the other parameters. Alternatively, the user supplies the specific
area and void fraction of any metal ring; and the program will estimate the equivalent size of Pall
ring. Or supply just packing factor and all parameters will be estimated.
At the time the model was developed, the FRI staff was concerned about the validity of their
experimental data gathered when operating at higher pressures. Consequently, the data base for
the model contains no information for systems with a vapor density above 0.33 lb/ft3 . The model
appears to underestimate pressure drop at higher pressure. This author, in a purely empirical way,
has incorporated a correction factor for higher vapor density systems to bring the model more in
line with existing data.
A listing of the BASIC program follows. The program is on the enclosed diskette. Be sure to
observe the instructions given on the monitor when running the program.
Note: This is an old program which has been superceded by recent FRI and vendor work.
Contact Al Nelson ([email protected], 510 242-2562) for information on the
best computer tools to use for packed column evaluation or design.

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Packed Column Technology 100 Packing Capacity and Pressure Drop

APPENDIX 100-B
STRUCTURED PACKING PRESSURE DROP PROGRAM
The program, written in GWBASIC, is based on Reference 17. The model developed in the
article is in SI units; consequently, the program calls for input in English units, converts it to SI,
executes the model, and reconverts the result to English.
The geometry of structured packing is explained in Figure 100-B1. Individual sheets of the
packing have a corrugated or "washboard" appearance. The sheets do not lie flat; they stand on
edge and are arranged in such a way that the ridges of adjacent sheets cross one another. Viewed
end on, the cross sections created for flow appear triangular in shape. Actually, they alternate
between triangular and square or diamond shaped as ridges and valleys of the adjacent sheet are
crossed. Two triangles base-to-base create the square or diamond shape.
The apex angle is the angle at which sides of a ridge or valley come together. The usual angle is
nominally 90°, which creates a square cross section; however, some packings have significantly
more or less. This author has added a small correction to the program to account for apex angles
differing from 90°.
The crimp angle is the angle made by a valley or ridge measured from the horizontal. Most
structured packings have a crimp angle of about 45°; some, e.g., the "X" series of Flexipac or
Mellapak, have 60°. Other things being equal, a steeper crimp angle increases capacity.
Packing geometry may also be described by the side dimension, "a" in Figure 100-B1; the crimp
height, dimension "h"; or the specific area per unit volume. Porosity or void fraction is also
needed; however, it tends to vary little from 0.98.
Default values in the program are 90° apex angle, 45° crimp angle, and 0.98 void fraction. The
user must supply one of the following: side dimension, crimp height, or specific area.
The model was developed on the basis that the pressure drop at flooding is 1.25 in. wc per ft of
packing. That parameter can be changed by the user; there appears to be little point in doing so.
The equation for pressure drop is implicit in that variable; therefore, it must be solved by an
iterative procedure. The equation has multiple roots including imaginary ones. A successive
substitution procedure is used which is usually successful. The user is notified if the procedure
fails to converge. In this author's experience, that happens only at high loadings.
When compared with FRI data, the original model underestimated pressure drop in the higher
pressure systems. This author added an empirical correction factor based on the ratio of surface
tension to vapor density.
A listing of the BASIC program follows. The program is on the enclosed diskette. Be sure to
observe the instructions given on the monitor when running the program.
Note: This is an old program which has been superceded by recent FRI and vendor work.
Contact Al Nelson ([email protected], 510 242-2562) for information on the
best computer tools to use for packed column evaluation or design.

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Packed Column Technology 100 Packing Capacity and Pressure Drop

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Packed Column Technology 100 Packing Capacity and Pressure Drop

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Packed Column Technology 100 Packing Capacity and Pressure Drop

Figure 100-B1 Structured Packing Geometric Relationship

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Section 200 Efficiency of Packed Columns

210 Introduction
This section presents recommended methods for predicting efficiency of packed columns.
Of all the parameters that must be predicted when designing a packed column, efficiency is the
least reliable. Following are the possible sources of efficiency information, in decreasing order of
reliability:
• Test data from a similar industrial column making a similar separation with a similar
packing. See Section 230.
• Data from a vendor's pilot plant, also for a similar separation and packing. This data must
be "derated" to account for the suboptimal conditions of an industrial column. See
Section 240.
• Correlations of efficiency, from rough rules of thumb to highly developed theoretical
models, or anything in between. This option is in a distant third place. See Section 250.
Packed columns are generally designed by carrying out stagewise (ideal or theoretical stage)
separation calculations using one of the several computer programs available for the purpose.
These programs are rigorous in that
• They contain the best available models for vapor-liquid equilibrium.
• They make complete heat and material balances for each stage of separation.
The calculations are nonrigorous or artificial only in that packing operates as a continuous, not a
stagewise, separation process. Once the number of stages has been determined for each section of
the column, the packed-bed height is found by multiplying the number of stages by the packed
"height equivalent to a theoretical plate", known as the HETP.
An alternative method, known as the "transfer unit" calculation, is available but rarely used. In
one form, total vapor and liquid mole rates are assumed constant through the column, and two
key components are fractionated by equimolar counterdiffusion and transfer between vapor and
liquid. In another form, the method involves:
• A noncondensing carrier gas.
• A nonvolatile liquid stream.
• A mutually soluble component which transfers from carrier gas to liquid (absorption) or
from liquid to gas (stripping).
Having found the number of transfer units needed, the engineer then multiplies by the packed
"height of a transfer unit" or HTU. References 1 and 2 explain this technique.
In certain cases, the HETP of a packing equals the HTU; generally it does not. The HETP
approach is preferred because
• It is more easily understood.
• It requires fewer simplifying assumptions.
• Computerized, stage calculations are very convenient, particularly for multicomponent
systems.

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Packed Column Technology 200 Efficiency of Packed Columns

• The HETP of a given packing in a given service appears to vary less with loading than
the HTU. The remainder of this section will deal with prediction of HETP, not HTU.

220 HETP Versus Loading


The usual presentation of efficiency data is a plot of HETP versus loading, the data being taken at
total reflux. Total reflux operation greatly simplifies analysis of data; in addition, uncertainty due
to the occurrence of "pinch zones" is avoided. Figure 200-1 is an ideal plot because
• Scatter of actual data is not shown.
• The shape is typical of laboratory data using a high-quality liquid distributor.
In general, packing has a very wide operating range as shown in Figure 200-1. At the low - loading
end of the range, performance is affected by "dewetting", i.e., liquid rate insufficient to
completely wet the packing surface. For metal ring or structured packing in hydrocarbon service,
this limit is probably below liquid rates of 0.2 gpm/sq ft of column cross section. Note that this is
the actual liquid rate in the packed bed, not necessarily the irrigation rate from the distributor to
the top of the bed. In some applications, such as wash-oil beds in crude unit vacuum columns, the
wash-oil rate "shrinks" as it passes downward through the bed.
Most data sets are taken with one liquid distributor design intended to cover the complete
operating range. Their lower limit of efficient separation is set by the distributor's limitation
rather than the packing. As liquid head above the distribution orifices decreases to 1 inch or less,
evenness of distribution suffers. This, rather than packing limitation, accounts for poor efficiency
at low loading.
On the high-loading end, efficiency is decreased by entrainment of liquid by vapor within the
packing as flooding is approached. In rare instances, overloading the distributor (overflowing the
pan or troughs) is the cause.
Over most of the operating range, the curve of efficiency is flat. Near the high-loading end, there
may be a narrow region of extra-high efficiency just below the upper limit of operability. In
actual data, this region is poorly defined and often not seen. The various rules and correlations in
this section apply to the flat portion of the curve.

230 Efficiency Data From Plant Columns


The preferred source of packing efficiency is a valid test run of a plant column. In the following
discussion, we need to predict the efficiency of Column A; Column B provides the test run.
Obviously, the more similar Column B is to Column A, the better.
If the two columns do not have the same size of the same packing, then the two efficiencies can
be related by the methods of Sections 244 and 245.
If the two columns are not running the same group of chemical components (same system), then
see Section 246.
If Column B has a poor liquid distributor, while Column A has a good one, some credit may be
taken for this. In many cases, poor distribution doubled the HETP found with good distribution,
but no adequate methods exist for quantifying this effect. Be conservative when moving in the
reverse direction.

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Packed Column Technology 200 Efficiency of Packed Columns

Do not use a test-run result without first judging validity of the test run. Apply the procedure
given in Section 580, particularly Subsection 585. Some additional reasons for questioning
validity:
• Column B was not, in fact, separating between two key components. This tends to make
the number of theoretical stages, and therefore the efficiency, indeterminate.
• Column B was modeled with a different vapor-liquid equilibrium correlation than the one
used to design Column A. Relative volatilities, therefore efficiencies, are inconsistent.
• Column B was operated in a way that produced one or more "pinch zones" in the column.
(A pinch zone is a region in which the equilibrium and operating lines are very close
together. Figure 3 shows equilibrium and operating lines and a pinch zone.) The result is
that the computed separation is insensitive to the number of theoretical stages used in the
model and the efficiency is therefore questionable.

240 Laboratory and Pilot-Plant Efficiency Data


Laboratory or pilot-plant data on packing capacity or pressure drop may be directly applied to an
industrial column, provided that additional pressure losses caused by support plates, collector
trays, etc. are accounted for. This is not true of efficiency data. An industrial column is subject to
operating transients, upsets, manufacturing and installation tolerances, accumulation of debris in
distributors, etc. The packing efficiency found in the ideal conditions of the laboratory or pilot
plant must be derated. The following sections address derating for non-optimal conditions that
may be accepted for economic or operability reasons, not for conditions that are avoidable.
241 Derating for "Plant Environment"
Where efficiency is critical, where considerable effort will be expended on high-quality liquid
distribution, precise installation, inspection, commissioning, testing, maintenance, and any
necessary troubleshooting and rework, use a derating factor of 0.8. (Divide the laboratory HETP
by 0.8.) This recommendation is based on experience with random packing in the ethylbenzene
recycle column of the older styrene plant at ChevronTexaco Chemical Company, St. James. After
extensive troubleshooting, redesign of distributors, and modification of operating procedures, the
number of stages increased to 83% of the number predicted by direct application of the original
laboratory efficiency data. The complete story is in Reference 3.
For an installation of similar importance, but without rework, use a derating factor of 0.7. This is
based on experience with structured packing in another ethylbenzene recycle column of the newer
St. James plant. Using a similar system and a similar packing, Fractionation Research, Inc. (FRI)
measured an HETP of 15 in. At this time, the column has maldistribution problems. Planned
remedial measures have not yet been taken, and the measured HETP is 22 in. Thus, efficiency is
68% of what was measured by FRI. (The vendor guaranteed a total number of stages equivalent
to HETP of 18 in.)
For a column where maximum efficiency is less important, where the liquid distributor will be
less than top quality and where operating conditions are not expected to support top performance,
use a derating factor of 0.50.
242 Accounting for Bed Depth
The usual recommendation for maximum bed depth is 30 ft, limited by packing crush strength; or
10 theoretical stages, accounting for liquid maldistribution. The columns cited in Section 241
exceed the 10-stage recommendation. It is likely that a part of the "plant environment" derating
factor is the effect of bed depth; however, that is a small part, and it cannot be isolated at present.

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Packed Column Technology 200 Efficiency of Packed Columns

In 1992-93, FRI investigated the bed-depth effect, comparing performance of 8-ft and 32-ft beds
of 1-inch Pall rings. The effect was dramatic: the long bed had an HETP twice the value of the
short bed (derating factor of 0.5). Anomalies were found in the long-bed data, however, and the
situation is unresolved. For the present, we should disregard this data and continue to use the 30-
ft and 10-stage recommendation.
243 Effect of Density of Liquid Distribution Points
This topic is discussed in Section 312 also. The usual recommendations are 10 distribution points
per sq ft for structured packings and high-efficiency dumped packings; 5 per sq ft for the higher
capacity, less efficient dumped packings. These recommended values are conservative. In cases
where orifice distributors are used with low irrigation rates, there is incentive to reduce drip-point
density in order to keep orifice diameters from becoming too small. (The recommended minimum
orifice diameter is 1/4-in.)
In tests with 1-in. Pall rings, FRI found that reducing drip-point density to 3.3 points/sq ft had no
effect on efficiency (derating factor 1.0). At 2.4 points/sq ft, the factor was 0.90; at
1.1 points/sq ft, 0.6. Tests were done with one hydrocarbon system, 12-ft bed depth, and at three
liquid loadings, the lowest being about 2 gpm/sq ft. (The liquid-loading effect was negligible.)
An abbreviated group of tests were later done with 2-in. Pall rings and 17-ft bed depth. Results
were the same except that the derating factor was 0.8 for 2.4 points/sq ft and a density of 1.1
points/sq ft was not tested.
A 12-ft bed of Mellapak 250.Y structured packing was tested in the manner discussed above. The
derating factor was 1.0 at drip-point density down to 3.3 points/sq ft and 0.8 at 2.4 points/sq ft.
The recommended use of this information:
• Reduce drip-point density below the recommended values (10 and 5 points/sq ft) only if
necessary to keep orifice diameter from being too small.
• Do not use drip-point densities below 3.3 points/sq ft.
244 Adjusting Random-Packing Efficiency for Packing Size
Following are simple rules for starting with an HETP for a given random packing, Packing B, and
estimating the HETP of a different size packing, Packing A, of the same kind (same
manufacturer, same packing family). Strictly speaking, "size" means actual particle diameter, e.g.,
the diameter of an individual Pall ring, not numerical size designation. All comparisons include
the assumption that both packings operate on the flat portion of the efficiency versus loading
curve.
• Determine whether either packing size is the one of its family closest in capacity to a 2-
in. Pall ring. Refer to the packing factors in Tables 100-1 and 100-2 to make this
determination.
• If one of the sizes is close to the 2-in. Pall ring and the other is smaller, or if both sizes
are of lower capacity, then assume that HETP is proportional to the 0.4 power of packing
size. Use the formula.
Equation 200-1

HETPA= (Known HETP B)•(Size A/Size B)0.4


• If one of the sizes is close to the 2-in. Pall ring and the other is larger, or if both sizes are
of higher capacity, then assume that HETP is proportional (power of 1.0) to the packing
size. Use the formula.

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Packed Column Technology 200 Efficiency of Packed Columns

Equation 200-2
HETPA = (Known HETP B)•(Size A/Size B)
• If one of the sizes is of higher capacity and the other is of lower capacity than a 2-in. Pall
ring, then make the adjustment by the appropriate two-step process, using both equations.
For example, to estimate HETP for a 3-in. ring, based on a value for a 1-in. ring:
1. Relate the 1-in. ring to a 2- in. ring using Equation 200-1.
2. Then relate the 2-in. ring to a 3- in. ring using Equation 200-2.
If HETP of the 1-in. ring is 18 inches, then HETP of the 3-in. ring will be (18)x(2/1) 0.4x(3/2) or
36 inches.
At present, there is no good explanation for the change of exponent at 2-in. Pall-ring size, but the
effect is seen in data for two different families of metal-ring packing. The comparison applies
only when both packings are loaded at a point within the flat efficiency range shown on Figure
200-1. Be aware that the greater the size difference, the more uncertain the comparison. Finally,
when preparing to gain the efficiency advantage of a smaller size packing, note that the greater
the intrinsic efficiency of a packing, the more it suffers from less-than-ideal liquid distribution,
operating conditions, etc.
As an alternative to the above procedure, run the FRI packing efficiency program (Section 254)
for both packing sizes and multiply the known HETP by the appropriate ratio of the predicted
HETPs for the two packing sizes.
Equation 200-3
HETPA= (Known HETP B)•(Predicted HETP A)/(Predicted HETP B)

245 Adjusting Structured-Packing Efficiency for Packing Size


Efficiency comparison for two "sizes" or capacities of the same manufacturer's structured packing
requires care. The size most often used has:
• A crimp height of around 1/2-in.
• Specific area in the range 60-75 square feet per cubic foot of packing.
• A crimp angle of around 45°.
In the cases of Glitsch, Koch, and Norton, this size carries the "Number 2" designation. Beyond
that, there is no uniformity in the way U.S. manufacturers rate their packings. For Koch and
Norton, a larger number means a lower specific -surface area, a higher capacity, and a lower
efficiency; for Glitsch it means the opposite. In some cases, an increase of 1 in the "size number"
doubles (or halves) the crimp size; in other cases it does not. Manufacturers have not released
complete data on the pertinent dimensions of their products.
In the European system, approximate specific area (metric basis) is included in the packing
designation. Examples: Montz B1-200, Sulzer Mellapak 250.Y.
If you have the required dimensions, then approximate comparisons can be made with the
Bravo-Rocha -Fair structured-packing program (Section 254) in the manner discussed above for
random packings. This model originated in the Separations Research Program (SRP) at the
University of Texas at Austin. However, note that neither SRP nor FRI has completed testing of
structured packings with a range of capacities sufficient to give a good measure of the capacity
versus efficiency effect.

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Packed Column Technology 200 Efficiency of Packed Columns

The Norton computer program, Reference 4, provides HETP estimates for the various sizes of
Norton's structured packings. The programs of other vendors do not provide such estimates.
246 Adjusting Efficiency for a Change Of System
As in previous examples, we have an HETP for Column B operating with System B; we want
HETP for Column A with System A. Depending upon the completeness of property data, use the
material of either Section 252 or 253 to predict HETP for both systems. Then,
Equation 200-4
HETPA= (Known HETP B) • (Predicted HETP A)/(Predicted HETPB)

250 Predicting Efficiency in the Absence of Data


251 Rough Rules
For very preliminary estimates, use the recommendations in Table 200-1. Good liquid distribution is
assumed.
Unless noted, the random-packing information applies to modern random packings approximately
equivalent in capacity to 2-inch Pall rings. These include Glitsch No. 2 Cascade Mini-Rings,
Koch Fleximax 300, Norton No. 40 IMTP, and No. 1.5 Nutter Rings. This group has the potential
to provide about 25% better efficiency, at the same capacity, than the older 2-in. Pall rings.
Structured-packing information in Table 200-I applies to the common "Number 2" size discussed
in Section 245.
Derating for "plant environment" is included.
Kister (Reference 2) has an extensive collection of rules of thumb.
252 Simple Correlations for Packing Efficiency
Use equation 200-7, (below) for quick estimates of efficiency. It is also useful for adjusting a
measured efficiency for a change of system properties.
Strigle (Reference 1) presents a random-packing efficiency correlation developed at Norton and
based in part on published FRI and other literature data. This is a correlation of laboratory data;
results should be derated as discussed in Section 240.
Equation 200-5
ln HETP = n - 0.187 ln σ + 0.213 ln µ
where HETP is in feet
n is a constant for each type and size of packing,
σ is surface tension within the range 4-36 dynes/cm,
µ is viscosity within the range 0.08-0.83 cp.
The above equation is equivalent to one appearing in the Norton IMTP brochure (Reference 5)
and the Norton PC program (Ref. 4):
Equation 200-6
HETP = B•(σ/20) -0.19•(µ/0.2) 0.21
where HETP is now in inches,

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Packed Column Technology 200 Efficiency of Packed Columns

B is a constant for each size of packing,


σ and µ are restricted to somewhat different ranges.
With little effect on results, this equation can be simplified to the following recommended
equation. Surface tension and viscosity are subject to the original ranges of Equation 200-5. If σ
exceeds 36 dynes/cm, use 36.
Equation 200-7

HETP (inches) = 2.5•N•( µ /σ)0.2


where N is a constant for each size and type of packing and is equal to HETP in a
system with σ = 20 and µ = 0.2.
Values of N to be used in Equation 200- 7 are in Figure 200-2, plotted against packing factor, a
rough measure of capacity. Note the following curves:
• Pall and equivalent rings,
• Norton IMTP and the other more modern metal-ring packings.
• Sheet-metal structured packings.
Packing factors are found in Tables 100-1 through 100-3.
The Pall-ring curve is based on FRI data; however, the Strigle and Norton publications are in
good agreement. The modern-ring curve is from Norton (5); the FRI test of No. 2 Nutter rings is
in agreement. The structured-packing curve was derived from output of the Norton program (4);
again, FRI data on Norton 2T and other structured packings are in general agreement.
Individual vendors will argue that their proprietary packings outperform those of their
competitors; however, one curve for all "latest generation" random packings, and another for
structured packings, is fair enough for rough estimates.
253 Rigorous Correlations for Packing Efficiency
The rigorous approach is recommended when
• Experimental efficiency data are lacking.
• Time permits developing the extensive physical properties needed.
The basic framework of rigorous correlations is the "two-film" or "two-resistance" theory of mass
transfer, found in standard texts. A brief explanation is provided here as background for use of the
computer programs contained in the appendices.
The actual multicomponent system can be described as a binary system consisting of the key
components that define the desired separation. Mass transfer occurs in two ways:
• By counter-diffusion, through resistance, between the bulk composition of the gas and the
composition of the gas at the gas-liquid interface. The gas composition at the interface is
in equilibrium with the liquid composition at the interface (no resistance).
• By diffusion between the liquid composition at the interface and the bulk liquid
composition.
If the resistance in the gas phase is distinctly greater than that in the liquid phase, the system is a
"gas-phase resistance-controlled" one. Most distillation systems are in this category. Mass
transfer on structured packing is more gas-phase controlled than on random packing, possibly
because structured packing develops thinner liquid films.

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Phase resistances are usually correlated in terms of dimensionless groups. For example, the
vapor-phase Sherwood number, which involves the vapor-phase, mass-transfer coefficient, the
vapor-phase diffusion coefficient, and a characteristic length dimension, is correlated as a
function of the Reynolds number (mass velocity, viscosity, length) and the Schmidt number
(viscosity, diffusion coefficie nt, length).
The height of a vapor-phase transfer unit, HG, is related to the vapor superficial velocity, the
vapor-phase mass-transfer coefficient, and the "effective area for mass transfer", expressed as
square feet of effective surface per cubic foot of packing. Similarly, HL. Effective area is a
function of actual packing-surface area, liquid holdup in the packing, and other variables. How an
effective area is handled is one thing that distinguishes one current correlation from others.
The individual phase heights of transfer units (sometimes with additional resistances expressed as
heights) are combined as follows:
Equation 200-8
HOG = HG + λ•HL
where H OG is the height of an "overall" transfer unit, based on gas-phase compositions,
HG and HL are as defined in the paragraph above, and

λ is the ratio of the slope of the equilibrium line to the slope of the operating line (as on a
McCabe -Thiele diagram). See Figure 200-3.
Equation 200-9
In turn, λ = m/(L/V) = m•V/L
where m is the slope of the equilibrium line, and
L/V (in mole rates) is the slope of the operating line.
The combination m•V/L is sometimes referred to as the stripping factor. This is correct only at
the extreme left end of the diagram. The stripping factor is Ki•V/L, where Ki (the K-factor) is the
vapor -liquid equilibrium ratio of component i. Referring again to Figure 200- 3, which is drawn
for a constant relative volatility, α, of 2.0 between the keys, notice that m varies from α at the left
end of the diagram to 1/α at the right.
If λ = 1, then HETP = HOG. Otherwise,
Equation 200-10
HETP = (HOG)(ln λ)/(λ-1).
The rigorous correlations require a lot of physical and packing-property data and are practical
only for machine computation. They reproduce binary-system efficiency which was measured in
the near ideal conditions of the laboratory, in most cases at total reflux operation. Be sure that
results from the correlations are de rated as discussed in Section 240. Use them with caution,
especially when working outside the data base. In general, the data base is close-boiling binary
systems at low to moderate pressure.
254 Computer Programs for Packing Efficiency
Simulation Sciences Inc. markets PROCESS for main-frame computers and PRO II for personal
computers. The distillation module outputs estimated HETPs based on rules of thumb, which may
be found in Kister (2).

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As stated in Section 252, the Norton Program outputs an estimate of HETP for both random and
structured packings marketed by Norton, apparently based on Equation 200- 6.
The FRI random-packing efficiency correlation (Reference 6) is based on FRI Pall-ring data, and
this author has verified that it reproduces the data adequately. The correlation is available as a
separate BASIC program for the PC, described in detail in Appendix 200-A. It is also found as
part of a PC program for packed columns, recently released by FRI. The advantage of using the
separate BASIC program is that input is made a little less tedious.
SRP has updated its PC program for packing design and has reissued it as part of a program for
both tray and packed columns (Reference 7). The program includes a Packing Properties Data
Bank, which contains properties (dimensions) of many of the modern metal ring and structured
packings. For random packings, the program offers two 1982-vintage correlations (References 8
and 9), which are based on data in the open literature. For structured packings, the
Bravo-Rocha -Fair correlation is used in its original form (Reference 10). This author has tried out
the program; it is not yet bug-free.
The pressure-drop portion of the Bravo-Rocha-Fair article is in a BASIC program described in
Appendix 100-B. This author modified the original form to make it reproduce data from higher-
pressure systems more adequately. The mass-transfer (efficiency) portion has recently been
added, and the complete package is in Appendix 200-B. Use of the efficiency portion depends on
the liquid holdup calculated in the pressure-drop portion. Again, this author’s version is intended
to make input easier.

260 References
1. Strigle, R. F., "Random Packings and Packed Towers", Gulf Publ. Co., Houston, 1987.
2. Kister, H. Z., "Distillation Design", McGraw-Hill Inc., New York, 1992.
3. McMullan, B. D., Ravicz, A. E., and Wei, S. J., "Troubleshooting a Packed Vacuum Column
-- A Success Story", Chemical Engineering Progress, July 1991, pp 69-74.
4. "Packed Tower Design Program Users Manual", Norton Co. Chemical Process Products,
P. O. Box 350, Akron, OH 44309.
5. Norton Bulletins IHP-1 (Intalox) and MTP-1 (Metal Tower Packing).
6. Fractionation Research, Inc., Topical Report 92, July 1984.
7. “User's Guide, RATE Program for Designing Tray or Packed Columns", R. Macias and R. L.
Harvey, Separations Research Program, The University of Texas at Austin, May 1993.
8. Bolles, W. L., and J. R. Fair, Chem. Eng. 89(14):109 (July 12, 1982).
9. Bravo, J. L., and J. R. Fair, Ind. Eng. Chem., Proc. Des. Devel. 21:162 (1982).
10. Rocha, J. A., Bravo, J. L., and Fair, J. R., Ind. Eng. Chem. Res., 32, 641-51, (1993).
11. Koch Bulletin FS-1, 1981.

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Tables and Figures

Figure 200-1 HETP Versus Loading

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Figure 200-2 Standard System HETP (Parameter N in Equation 200-7)

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Figure 200-3 McCabe – Thiele Diagram


Table 200-1 Packing Efficiency Recommendations
HETP, ft
Application Random (1) Structured
Superfractionators, low relative volatility, clean service. Examples: ethylbenzene/styrene 2.0 1.5
separation, deisobutanizers.
Other fractionators in which fairly high tray efficiency would be expected if they were trayed. 2.5 2.0
Other fractionators of somewhat lower efficiency. Examples: light hydrocarbon separation 3.0 2.5
including upper portions of atmospheric crude column or FCC main fractionator.
Sidecut strippers, heavy oil sections of crude columns and coker fractionators 4.0 3.0
(2)
Amine absorbers, sponge absorbers, other very low efficiency services (regardless of packing 6.0
size).
Glycol (TEG) Dehydrators 6.0 (3) 6.0
Notes
1) This information applies to modern metal-ring packings approximately equivalent in capacity to 2-in. Pall rings. For Pall rings or
equivalent older packings, multiply listed HETPs by 1.25.
2) Not recommended at this time; however, there is one known retrofit application by Sulzer to gain capacity. Approach with caution
until more operating experience has been gained.
3) Random packing is not normally used. In this service, structured packing is not credited with an efficiency advantage.

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200 Efficiency of Packed Columns Packed Column Technology

APPENDIX 200-A
FRI RANDOM-PACKING EFFICIENCY PROGRAM
The program, written in GWBASIC, is based on a Pall-ring efficiency procedure contained in
Fractionation Research, Inc. (FRI) Topical Report 92 of July, 1984. Note that information
received from FRI is Confidential under terms of Chevron's membership agreement. This
information should not be distributed outside the Company.
The only packing-related parameter used in the correlation is the packing particle size (in.). For
Pall rings and equivalent, the particle size is in fact the particle diameter or height. Specify either
the particle size or the specific surface area (ft2/ft3) for Pall rings and equivalent; the two
properties are correlated. For a modern metal-ring packing, specify surface area (Tables 100-1
and 100-2). The program will compute the appropriate effective particle diameter and use that.
Required vapor data are the mass rate and the density. Molecular weight is needed only if the user
wants to compute the slope of the operating line (mole basis) rather than using a specified or
default value. The correlation uses vapor Schmidt number. Vapor viscosity, diffusivity, and
Schmidt number are all optional inputs; defaults are used otherwise.
Liquid mass rate, density, and viscosity are required. Molecular weight and diffusivity are
optional. Obviously, the more that the user can specify, the more likely that the predicted
efficiency will be useful.
In most cases, the user will not bother with any of the inputs needed to compute lambda, the ratio
of the slope of the equilibrium line to that of the operating line at the composition point in
question. In those cases, lambda will be assumed equal to 1.0; in close-boiling distillation
systems, it doesn't matter much anyway. However, one can specify either m or lambda. If alpha
(relative volatility of keys) and key ratio are given, then the slope of the equilibrium line will be
computed.
A listing of the program follows. The program is on the enclosed diskette. Be sure to observe the
instructions given on the monitor when running the program.

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200 Efficiency of Packed Columns Packed Column Technology

APPENDIX 200-B
STRUCTURED-PACKING PRESSURE-DROP AND
EFFICIENCY PROGRAM
The program, written in GWBASIC, is based on Reference 10. The efficiency portion is a small
add-on to the pressure-drop program describe d in Section 100. Efficiency prediction requires
estimating liquid holdup, which is done in the pressure-drop portion. The only additional phase-
property data needed for efficiency estimation are the vapor and liquid diffusivities, and input of
these is optional. Default procedures are available.
In regard to lambda, the same options are available as in the random-packing efficiency program.
The geometry of structured packing is explained in Figure 200-B1. Individual sheets of the
packing have a corrugated or "washboard" appearance. The sheets do not lie flat; they stand on
edge and are arranged in such a way that the ridges of adjacent sheets cross one another. Viewed
end-on, the cross sections created for flow appear triangular in shape. Actually, they alternate
between triangular and square or diamond-shaped as ridges and valleys of the adjacent sheet are
crossed. Two triangles base-to-base create the square or diamond shape.
The apex angle is the angle at which sides of a ridge or valley come together. The usual angle is
nominally 90°, which creates a square cross section; however, some packings have significantly
more or less. This author has added a small correction to the program to account for apex angles
differing from 90°.
The crimp angle is the angle made by a valley or ridge measured from the horizontal. Most
structured packings have a crimp angle of about 45°; some, e.g. the "X" series of Flexipac or
Mellapak, have 60°. Other things being equal, a steeper crimp angle increases capacity.
Packing geometry may also be described by the side dimension, "a" in Figure 200-B1; the crimp
height, dimension "h"; or the specific area per unit volume. Porosity or void fraction is also
needed; however, it tends to vary little from 0.98.
Note that this is not a seasoned, robust program. It does not contain procedures for screening out
inappropriate data. Given wrong input, the program will fail or give wrong output. If the
interative portion of the program fails to converge, it is likely that input data result in too high a
loading of the packing.
A listing of the program follows. Be sure to observe the instructions given on the monitor when
running the program.

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Figure 200-B1 Structured Packing Geometric Relationships

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Section 300 Liquid and Vapor Distributors for Packed
Columns

310 Introduction
This section covers:
• Liquid distribution and redistribution to packed beds.
• Liquid mixing between beds.
• Vapor distribution.
• Problems with bringing single and two phase streams into columns.
ChevronTexaco engineers seldom design the details of distributors. The material here is intended
to assist in preparing specifications and in reviewing the designs of vendors.
311 Importance of Good Distribution
Good distribution of both vapor and liquid streams to a packed bed is essential in order to obtain
best performance. "Performance" in this case means separation efficiency. Poor distribution, as
long as the packing remains clean, does not cause premature flooding or excessive pressure drop
in packed beds; it causes poor efficiency. On the other hand, packing which is subject to coking
conditions (hydrocarbons at high temperature) requires good liquid distribution and an adequate
irrigation rate to minimize coking.
Vapor and liquid interact through the mechanism of pressure drop. For example, if liquid
distribution to the top of a packed bed is uniform but vapor distribution to the bottom is not,
liquid will become maldistributed as it runs down through the bed.
The best performance that can be obtained from a given packing is called the "intrinsic"
efficiency. This is a function of the packing type and the "system" (the chemical components and
the process conditions).
If vapor or liquid distribution is not uniform across the horizontal cross section of a column,
various regions of the packing will operate at different liquid/vapor ratios and will produce
different degrees of separation. The result will be concentration differences within the same
horizontal cross section, "pinch zones" where little mass transfer takes place, and a decrease in
the separation produced by the column as a whole.
Flow nonuniformity in plant columns has been detected by placing thermocouples at several
different points at the same elevation in a packed bed. In one case, temperature differences of
10-20°F were measured in the same cross section. In another case, samples were collected at
different points as liquid ran from the bottom of a packed bed; the samples had different
compositions, equivalent to several theoretical stages of separation.
In 1987, Chevron Chemical installed improved liquid distributors in the ethylbenzene recycle
column of the older styrene plant at St. James, Louisiana. Packing efficiency improved by 25%
over the original distributors and by 50% over the original distributors during periods when they
were partially plugged by scale deposits. Details are in Reference 1.

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312 Good Liquid Distribution Defined


A good liquid distributor has the following characteristics:
• Assuming that the liquid will be distributed to discrete points on the top surface of the
packed bed, the points will be uniformly spaced over the complete column cross section,
including the region near the wall. In random (dumped) packing, the wall region is within
two packing diameters of the wall. If portions of the space near the wall are obstructed,
"drip tubes" or "guide pipes" will be used to ensure that those areas are irrigated.
• The "drip point density" (the number of points per sq. ft. of packing surface) will be 10
for structured packings and high performance dumped packings; 5 for the higher
capacity, less efficient dumped packings. But note that these criteria may have to be
compromised in some low liquid rate cases. When FRI tested the effect of drip point
density with 2-in. Pall rings, a random packing, efficiency was unaffected down to 3
points per sq. ft.
• The liquid rates to the various points will be as nearly uniform as practical, over the
complete design range. In particular, no sizable areas will have liquid rates generally
different from the average. A significant random variation from point to point is not
nearly as serious as "zonal maldistribution", having larger areas with rates generally
higher or lower than average. Example: in an orifice-pan distributor, random variation in
orifice size is much less harmful than cocking the pan so that liquid is deeper on one side.
Rules of thumb in specifying allowable variation:
• No more than 20% variation from highest to lowest discharge point anywhere in the
distributor.
• No more than 10% standard deviation in flowrates, as a percentage of the mean.
These measures are practical and can be demonstrated at a vendor's test facility. We recommend
that critical distributors be assembled and tested in this fashion.
• If flow occurs by gravity through orifices, orifice diameter will be at least 1/4 in. to
minimize the chance of plugging.
• The distributor will have the capacity to collect a reasonable amount of debris without
being plugged.
• In services where material tends to coke or polymerize, residence time in distributors will
be minimized.
• In columns where pressure surges are possible, the distributor will be resistant to upset or
mechanical damage.
• The distributor will be constructed to minimize the number of seams. Seams will be seal
welded wherever possible. Where flanged connections are used, mating pieces will be
made of plate at least 1/4-in. thick in order to minimize the chance of deformation and
leaks. In connections which do not hold pressure (in gravity distributors), gasketing is
optional.
A few authors have proposed numerical measures of quality of distribution. Reference 2 deals
with liquid rates to a fixed array of distribution points at the top of a packed bed; however, it does
not include composition or vapor distribution effects. Reference 3 treats the degree of regularity
in placement of drip points; it does not include uniformity of liquid rates to those points. So far,
none of the models is complete enough to be very useful. In addition, the quality of distribution
needed in a given case will vary, depending on intrinsic packing efficiency, the separation to be

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made, and the severity of operating conditions. For the present, we will use mainly qualitative
rather than quantitative measures of distribution.

320 Types of Liquid Distributors


The following brief descriptions are given for background. Illustrations may be found in vendors'
catalogs.
321 Pan Distributor
This type is common in columns up to 4 ft. in diameter and is occasionally found up to 10 ft. The
size limitation is the need to keep the floor flat and level, and to minimize seams.
The pan may cover the complete column cross section, or there may be an annular space 3 to 6 in.
wide for vapor flow around the pan. In any case, most of the vapor flows upward through risers in
the pan. Total cross section for vapor flow may be 10-25% of column cross section; 15% is
typical.
Liquid usually flows through orifices in the bottom of the pan. With low liquid rates, drip tubes
may be used to ensure that liquid streams fall exactly where intended. Orifices, slots, or V-
notches (rarely) in the sides of the risers may be used. Unless space for vapor flow is ample,
vapor may interfere with liquid flow in cases where the two phases pass countercurrently in
risers.
322 Trough Distributor
This distributor replaces the pan distributor in larger columns. Liquid is delivered (preferably
from a manifold, not from a single nozzle) to a center sump. It then runs out into branch troughs
constructed at right angles to the center sump and at the same elevation. Alternatively, one or
more parting boxes may be mounted above, and at right angles to, the troughs; in most cases, the
individual troughs are not hydraulically connected and the parting box(es) must meter the
appropriate rate of liquid flow into each trough. There are no vapor risers; the vapor passes
upward between the troughs. This type of distributor has the advantage that the individual troughs
can be precisely leveled with leveling screws.
In some models, the troughs are around 1 ft. wide, and liquid flows through orifices in the floor.
Newer models have narrower troughs, as narrow as 2 in., with orifices in the sidewalls an inch or
two up from the floor. (These troughs must be narrow in order to provide the required drip-point
density.) The volume in each trough below the orifices allows debris to settle without interfering
with liquid flow.
Drip tubes or other devices may conduct the liquid from each orifice partway to the packing
surface below.
A parting box or trough must be large enough in cross section that hydraulic gradient along its
length is negligible. In general, a flow velocity of 1-2 ft./sec is satisfactory. Gradient may be
checked by using methods for open channel flow in the Chemical Engineers' Handbook. Flow
disturbances such as eddy currents and inlet nozzle velocity head are usually more important than
gradient. Troughs often contain perforated baffles to dissipate this kinetic energy.
Trough distributors with V-notches in the sides are rarely used because the quality of distribution
is poor. See the discussion in Section 332.

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323 Combination
In one new distributor model, the cross section of a column is covered by many square or
triangular shaped pans, each with an area of about 1 sq ft. There is 2-3 in. clearance between
pans; vapor also flows through risers in the pans. The pans are individually leveled and are not
interconnected hydraulically. This is an advantage; the pans do not have to be at exactly the same
elevation. A parting box or predistributor meters the correct flow of liquid into each of the pans.
(This predistribution is critical--see the comparison of random versus zonal maldistribution in
Section 312.)
324 Manifold or "Ladder" Distributor
This device looks like a trough distributor with a center sump, but it's made of pipe and operates
under pressure. Liquid issues through holes along the bottom of the branch pipes. In order to
provide a reasonable drip point density, the branch pipes need to be as close together as 4-5 in.;
thus, this distributor is more often found in small columns. Pressure drop and kinetic energy
effects along the length of the branch pipes are another concern.
Manifolds used for bringing streams into columns are discussed in Section 365.
325 Spray Distributor
If the holes in the branch pipes of a manifold distributor are replaced by spray heads, the result is
a spray distributor. While the distributor types mentioned above (except the V-notch) can, if
properly constructed, provide good distribution, quality of a spray distributor is fair at best. This
is because:
• Each spray head's impact area on the packing (the "footprint") is irregular.
• The liquid rate to various areas within the footprint is uneven.
• The footprints must overlap to avoid leaving any part of the packing surface dry.
A spray distributor may be used
• In a coking service where residence time in the distributor must be minimized.
• In a large column with low liquid rate where distribution quality is less important.
• As a predistributor onto a pan type main distributor.
Although 120° spray angle heads have been used in the past, we now prefer 90° spray angle
heads, even though the number of heads in a given application is approximately tripled. Under the
process conditions existing inside a column, 120° angle patterns tend to "collapse" to 60-70°.
This leaves large areas of the packing surface unirrigated.
Spray heads are full-cone sprays selected from the catalogs of Spraying Systems Company or
Bete Fog Nozzle, Inc. See Section 332 for pressure drop recommendations.
Spray heads are usually on triangular spacing with one head on the column centerline. Layouts
with 7, 19, 37, 61, and 91 heads have been used. A recent design provided 91 spray heads on
triangular spacing in a 32-ft. diameter column, or approximately 9 sq. ft. of cross section per
spray head.
To avoid dry spots on the packing surface, there must be overlap of spray patterns. See Figure
300-1. Minimize triple coverage (overlap of three sprays) if possible. If the diameter of the spray
pattern at the top surface of the packed bed is d, then head-to-head spacing in equilateral triangles
of side 0.70d to 0.85d is recommended. Small dry spots near the wall are unavoidable. In recent
designs, spray heads on the perimeter of the layout have been spaced 0.35d to 0.45d from the

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column wall. Dry areas are approximately balanced by segments of spray patterns that hit the
wall.

330 Liquid Distribution Practice


331 Placement of Liquid Distributors
Place the pan, trough, and manifold distributors with about 6 in. clearance between the bottom of
the distributor and the top of the packed bed (or the holddown grid or bed limiter, if used). This is
a change from our previous recommendation of 12-24 in. There is considerable entrainment of
liquid upward from the top surface of the bed at higher vapor rates. In higher pressure systems, a
froth layer forms and carryover of spray or froth into the distributor may occur. It now appears
that
• The spacing used between bed and distributor has little effect on spray and froth
formation.
• The vapor rate at which spray and froth form is well above the efficient operating range
of most packings.
The new clearance of about 6 in. will allow vapor to flow uniformly upward through the top few
inches of packing and then make its way horizontally to the chimneys in the distributor.
The spray heads of a spray distributor should be 12-24 in. above the packed bed or holddown
device. Spacing much greater than 24 in. results in distortion (drooping) of the spray cones.
332 Liquid Flow Control and Turndown
Liquid flow through any restriction is controlled by pressure:
• Line pressure produced by a pump and regulated by a control valve.
• Pressure produced by liquid head in a pan or trough.
Suppose you need a turndown of 2:1, i.e., the distributor must handle rates from the design
(maximum) rate down to one half of design.
• For flow through spray heads, flowrate is proportional to the 0.5 power of pressure.
The recommended operating range ofspray heads is 5-30 psi. Below 5 psi, spray is rather
unstable but the distributor may function at 2 or 3 psi. Pressure drop above 30 psi tends to
atomize the liquid. Depending on available spray head sizes, you might choose an
operating pressure of 5 psi for the turndown case and 20 psi for design, 7.5 psi for
turndown and 30 psi for design, or some combination in between. But note that spray
heads do not easily provide turndown greater than 2:1.
• For flow through a submerged orifice, flowrate is proportional (approximately, since
discharge coefficient may vary) to the 0.5 power of liquid head. Minimum desired liquid
depth in an orifice distributor is usually 2 in. above the orifices. A turndown requirement
of 2:1 would mean liquid depth varying from 2 to 8 in. above the orifices. (Note that this
is only the liquid depth needed for discharge through the orifices. There might be
additional depth needed to overcome vapor phase pressure drop through the distributor.)
• For flow through a partially submerged slot (the slot being in a vertical plane, e.g., in the
side of a trough or a vapor riser), flowrate is proportional to the 1.5 power of head (depth
above the bottom of the slot). If minimum depth in the slot is 2 in., then 2:1 turndown
means maximum depth of 3.2 in. and even 4:1 turndown results in maximum depth of

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only 5.0 in. Clearly, turndown is more easily accommodated in vertical slots than in
submerged orifices.
• For flow through a V-notch, flowrate is proportional to the 2.5 power of head. A trough
distributor with notches 3 in. deep and minimum depth of 1 in. would provide turndown
of 16:1 from the point where notches were running full.
For pan and trough distributors, the reverse of turndown capability is the degree to which
distribution is affected by having the distributor out-of-level. Consider minimum depth of 2 in.
and a device which is out of level by plus or minus 1/4 in., a rather close tolerance in a large
column. The liquid depth then would be 1.75 in. minimum, 2.25 in. maximum.
• In a submerged orifice distributor, individual point flow would vary from 94% to 106%
of the base rate, still good distribution.
• In a slot distributor, point flow would vary from 82% to 119% of base, not so good.
• In a V-notch trough distributor, the rates would be 72% and 134%, not acceptable.
In summary, orifice distributors provide highest quality but are somewhat limited in turndown.
Slot distributors are often a good compromise, but precision manufacture is necessary to obtain
quality distribution. V-notch trough distributors are unlikely to qualify.
333 Design Equations
For discharge through submerged orifices,
Equation 300-1
Q = 676•A•h0.5
where Q = total flowrate, gpm
A = total cross sectional area of orifices, ft2
h = height of liquid above orifices, in.
An orifice discharge coefficient of 0.65 is incorporated in the above equation.
For discharge through a group of vertical slots, partially filled, where the height of liquid
in each slot is greater than the slot width,
Equation 300-2
Q = 33.4•L•h1.5
where Q = total flowrate, gpm
L = total width of the group of slots (length of crest), ft
h = height of liquid above bottom of slots, in.
Note that most slotted distributors made presently have very narrow slots. In these cases,
manufacturers' test data is preferable to general correlations such as the above.
For discharge through a group of triangular notches, partially filled:
If 60° angle at bottom of notches,

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Equation 300-3
Q = 1.292•n•h 2.5
If 90° angle at bottom of notches,
Equation 300-4
Q = 2.238•n•h2.5
where Q = total flowrate, gpm
n = number of notches
h = height of liquid above bottom of notches, in.
334 Liquid Redistribution
It is common practice to break a long packed bed into two or more sections with redistribution of
liquid in between. (In these cases, there is no feed added or product withdrawn between the beds.)
Maximum bed depth is usually the lesser of 30 ft. or the equivalent of 10 theoretical stages.
Strength of the packing is seldom a factor in maximum bed depth; the concern is deterioration of
liquid distribution quality (channeling) as liquid runs through the bed. The result is loss of
efficiency. Often overlooked is the fact that channeling produces composition differences from
point to point in the liquid flowing from the bottom of the bed. Composition gradients, if
uncorrected, decrease efficiency of the bed below.
In most redistribution cases, liquid from the bed above is collected and then fed to a distributor
for the bed below, with various degrees of mixing as in the following examples:
• If the distributor below had a center trough or parting box, there would be partial mixing
of the collected liquid before redistribution.
• If the collector and distributor were simple pans, there would be minimal mixing.
• If the liquid were withdrawn from the column and then pumped back to a spray
distributor (very unlikely in this case), there would be complete mixing.
In a case where maintaining high efficiency is crucial, liquid should be collected into a central
chamber where it is mixed (by flowing downward through mixing vanes) before being distributed
to the bed below.

340 Vapor Distribution Background


In contrast to liquid distribution, vapor distribution is less well understood in these areas:
• Measures of good vapor distribution.
• Effects of poor distribution.
• Methods of ensuring good distribution.
In attempting to explain the reasoning behind some recent developments in design practice, we
should differentiate between:
• The problem of vapor distribution.
• A related problem of getting good separation of liquid from vapor (deentrainment of
liquid).
The second problem is treated in Section 363.

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Uneven vapor distribution means that the vertical component of velocity is not the same at all
points in the column cross section. Sources of locally high velocity are partially or totally
vaporized feeds, reboiler return streams, stripping steam, and internal vapor flowing through
restrictions, such as the chimneys of collector trays or liquid distributors. Another possibility, not
proven, is that a change of column diameter between packed beds, involving either an increase or
a decrease in the cross sectional area available to the vapor stream, may disturb the even velocity
profile of that stream.
The energy in the locally higher velocit y currents may be dissipated by providing space for
turbulence or by providing resistance to flow (pressure drop). Devices for adding pressure drop
include chimney trays and "gas injection" packing support trays with lower-than-average total
cross sectional area of risers. Thus the effect of a large, high velocity stream may be neutralized
by a device which produces many small, high velocity streams. The small streams issuing from
the risers are oriented horizontally and in opposition to one another. (The risers are covered by
"hats".)
Crossflow trays seldom have vapor distribution problems. There is enough pressure drop through
a tray that any initial maldistribution of vapor is smoothed out. Pressure drop through a tray might
average 0.1 psi or more; pressure drop through an equivalent depth of packing could be only 10-
20% of that value. Therefore, vapor distribution is mainly a packed column concern.
341 The Energy of a High Velocity Stream
Three related measures of the kinetic energy of such a stream may be used:
• The product of vapor density and the square of velocity, ρV2.
• The square root of the above, which is called the "F factor".
• The kinetic energy term from the Bernoulli equation, V2/2gc. This expression is also
the definition of "a velocity head", which is the static head of fluid (in feet)
equivalent to the kinetic energy of a flowing stream. To convert to inches of water,
multiply this expression by
(12)(ρ V)
.
62.3
In the above expressions,
ρ V = vapor density, lb/ft3 ,
V = mean linear velocity, ft/sec.
gc = constant, 32.17 (lb mass)(ft)/(lb force)(sec 2)
For a two phase stream, depending on circumstances, use only the vapor phase or the bulk density
and velocity ("no slip" case).
342 Pressure Drop Through Risers
A riser on a liquid collector or packing support tray may be viewed as
• A vertical chimney with associated entrance head loss, plus
• A location just under the "hat" where the vapor makes an abrupt right angle, horizontal
turn, plus
• An exit area through which the vapor flows outward to the vapor space above the tray.

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Energy loss should then total about 2-1/2 velocity heads, from which the following equation is
derived.
Equation 300-5
∆P = 0.46•(ρV/ρ L)•V2

∆P = pressure drop in inches of liquid


ρ V = vapor density, lb/ft3

ρ L = liquid density, lb/ft3


V = mean vapor velocity, ft/sec
When using this equation, base the vapor velocity on the smallest cross section through which
vapor flows in the riser assembly. Note that equations used by others have coefficients up to 0.90
instead of the 0.46 in Equation 300-5. This suggests that although velocity is figured on one cross
section, such as total chimney area in the horizontal plane, there are other, more restricted cross
sections through which vapor flows before leaving the riser assembly.
343 Free Jet Behavior
Characteristics of a turbulent free jet are described in Perry's Chemical Engineers' Handbook, 6th
Edition. A jet is "free" if its own cross sectional area is less than one-fifth of the cross section
through which it is flowing. The streams considered here qualify. On the other hand, effects of
obstructions, cross currents, etc. are not known. For the present, make the following assumptions:
• Downstream distances are short enough, relative to jet diameter, that velocity on the jet
centerline is not attenuated.
• Apart from any changes in direction, the jet widens at an angle of 10° measured from the
centerline to the side in any direction.

350 Vapor Distribution Practice


Be aware that vapor distribution is not well understood and is an active area of research.
Experience and good engineering judgement are essential when designing or evaluating vapor
distributors.
351 When Internal Vapor Distributors are Needed
Different vendors recommend the following:
• If the F factor, V•(ρ V)0.5, of an entering vapor stream exceeds 22, then a vapor
distributing support plate should be used just above it. (If the entering stream is two
phase, then compute F for just the vapor portion, using the vapor density.)
• F = 15 is the limit beyond which vapor distribution control is needed.
• F should not exceed 52.4•(∆P)0.5 where ∆P is bed pressure drop in inches of water per
foot of packing (4).
• The velocity head at the inlet nozzle should not exceed 10% of the pressure drop through
the packed bed above.

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352 Clearance Above Vapor Entry


One vendor recommends a vertical clearance of one half column diameter between the top edge
of the vapor entry and the packing support plate above. This assumes a straight in vapor nozzle
without any internal distributor. This spacing is practical only for small columns. ChevronTexaco
has revamped columns, replacing trays with packing, where only 1 ft. clearance was available.
Other vapor distribution measures had to be employed.
353 Proposed Practice and Example Problem
Suppose that a large stream, such as stripping steam, feed gas, or a reboiler return, enters a
column with a velocity VE. Take these steps:
• Assume the "worst case", that this stream, at its initial velocity, impinges on some local
area of the packing support plate just above.
• Assume that the column is a superfractionator with high performance structured packing
and that vapor distribution must therefore be of high quality.
• Use bed depth, vapor density, etc. as shown in the following example.
The kinetic energy of the entering vapor will produce a higher-than-average vapor flow velocity
in the packing above the impingement point. The pressure drop of the packing will tend to even
out the vapor flow. We will design additional pressure drop into the risers of the packing support
plate, or a separate vapor distributor, in order to further assist vapor distribution. We will assume
that the impingement effect persists through the full depth of the packed bed and that the local
velocity above the impingement point must not be more than 5% above the average.
Let ρ V = 0.025 lb/ft 3
Let V E = 125 ft/sec

Let ∆P, the pressure drop per foot of packing, be 0.25 in. water.
∆PP = pressure drop through 25 ft of packing
= (0.25 in. water per ft of packing)(25 ft)
= 6.25 in. water.
∆P V = pressure equivalent of incoming vapor velocity

= [(125) 2/(2•32.17)][12•0.025/62.3]
= 1.17 in. water.
The maximum local velocity effect is stated as follows:
Equation 300-6
Flow ratio = ratio of maximum to average velocity
= [(∆PP + ∆P R + ∆P V)/(∆PP + ∆P R)]0.5
= 1.05
where ∆P R = pressure drop through risers of packing support plate.

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Substituting and solving for ∆P R:

[(6.25 + ∆P R + 1.17)/(6.25 + ∆PR)]0.5 = 1.05

∆P R = 5.16 in. water.


The risers can be designed using Equation 300- 5 and the average vapor flow rate. Note that if the
riser ∆P is 5.16 in. of water, the support plate will hold up liquid to a depth of (5.16)(62.3/ρ L)
inches in addition to whatever head is necessary to discharge liquid through the drain pipes or
holes.
If ∆PR turns out negative when computed from Equation 300-6, the packed bed already has
enough pressure drop to even out flow to the degree desired.
If the packing is of medium performance, such as the modern random packings, then the flow
ratio can be 1.10. If the packing is of low efficiency, such as a grid used for heat transfer, then a
ratio of 1.25 can be used. In fouling/coking service, such as deentrainment of residuum in a wash
oil section, the above technique for vapor distribution should not be used.
Suppose that the entering vapor stream is small compared to an internal vapor stream passing the
entry point and that the latter is evenly distributed already. An example would be the feed zone of
a fractionator operating at a high boilup ratio with a liquid collector/distributor below the feed
entry. The allowable flow ratio of 1.05 could be replaced by one calculated by Equation 300-7.
The most likely conclusion is that no additional pressure drop is necessary in the packing support
tray.
Flow ratio = 1.00 + (0.05)(Total vapor flow rate/Feed vapor flow rate)
Equation 300-7
Incidentally, F = VE•(ρV)0.5 = (125)(0.025) 0.5 = 19.8, and

52.4•∆P 0.5 = (52.4)(0.25) 0.5 = 26.2. Thus, two of the F factor criteria above are satisfied, but not
the other one.
354 Entrainment of Liquid By Vapor Below a Bed
If a gas injection type of packing support tray is used, then vapor will pass upward through the
tray in covered risers and liquid will collect on the tray and run down through orifices. Liquid
must collect to a depth which will overcome:
• Contraction loss through the orifices, plus
• Vapor pressure drop created by vapor passage through the risers.
Recently, a vendor stated that a certain liquid velocity through the orifices was required to
prevent entrainment of exiting liquid by vapor as vapor streamlines converged and entered the
risers. Riser diameter was 6 in. and orifices were about 2.5 in. from the edges of the risers.
Entrainment is possibly a valid concern, but only in extreme cases unlikely to occur under normal
operating conditions.
FRI recently tested an extremely high capacity structured packing. Vapor loadings were over
twice as high as those normally found in industrial columns. A special vane collector was used to
collect liquid from the bottom of the bed and conduct it downward past the reboiler vapor return.
Such devices may be needed but only in exceptional cases.

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360 Stream Entries to Columns


Previous sections have covered internals for distributing vapor and liquid streams within a packed
column. We now look at the details of bringing streams into columns.
361 Liquid Stream Entry
Reflux brought to a column is piped directly to a liquid distributor.
Mix the liquid feed to a fractionator with the internal liquid stream from the rectifying section
before it gets distributed to the stripping section. Instead of adding the feed to a redistributor
located just below the feed entry, it is better to collect the internal liquid stream, mix the feed with
it, and then distribute the mixture to the stripping section. Feed should be added to the collector
tray for the internal liquid stream. Liquid may be fed into a small pan distributor at one point near
the center, provided that velocity out of the feed pipe does not exceed 5 ft./sec and that the stream
does not impinge on any orifice. The inlet line should end about 2 in. above the pan rim, pointing
downward. A grid or other submerged structure to dissipate the velocity head is helpful. For a
larger pan, use a circular, triangular, or H shaped manifold, fitted between the chimneys. A spray
distributor discharging onto a collector tray or orifice pan is another possibility.
Do not feed a parting box or the center trough of a trough distributor at a single point; the concern
is turbulence and hydraulic gradient along the length of the trough. Symmetrical piping to several
points along the length of the trough is acceptable. A horizontal manifold positioned just above
the trough may be used. Again, discharge velocity should not exceed 5 ft./sec.
If plugging of distributors is a concern, liquid feed lines should have parallel basket strainers
without bypasses. Locate the strainers close to the column. Lines downstream of strainers should
be stainless steel. Maximum particle size passed by the strainers should be 1/32 in. if the
distributor has holes or passages 1/4 in. or smaller; otherwise, minimum particle size should be
1/16 in. Carefully flush the lines before startup.
362 Vapor Stream Entry
The standard entry for an all-vapor stream is a straight-in nozzle without any internals. Direct the
stream to hit on the opposite wall of the column, not on any internals. Assume that the stream
widens at a 10° angle from its centerline (free jet behavior). Minimal clearance of any
obstruction or liquid surface should be at least 1 ft. at the lower edge of the stream and at least 1.5
ft. above the nozzle. . In large columns, engineering judgment may call for larger dimensions.
Greater clearance above the nozzle would improve vapor distribution, but the quantitative effect
is not known.
Use of manifolds or "spargers" is occasionally proposed as a means for evenly distributing a
vapor feed. (These devices are not immersed in liquid.) In a small column, the manifold might be
a single pipe crossing the column horizontally on a diameter. In a larger column, the device
might be "H shaped", providing two parallel manifolds. The sparger is located at least a foot
below the packed bed, and the holes point downward and to the sides. Design of manifolds is
covered in Section 365. At this time, the effectiveness of these devices for vapor distribution is
not known.
Vapor distribution is more reliably controlled by riser pressure drop in the packing support tray
above as discussed in Sections 340 and 350.
363 Two -Phase Stream Entry
This is a difficult design problem. Ideally, the vapor and liquid phases of a feed stream should
separate completely. The vapor phase should mix with the internal vapor stream passing the feed

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point; similarly, the liquid phases. There should be no vertical high velocity flow vectors to
disrupt good distribution to packed beds above or below.
Some existing installations described below are recommended for similar applications.
Several ChevronTexaco heavy oil vacuum columns have grid or random packing in wash oil
sections just above the flash zones. Internals include tangential feed entries, annular shrouds, and
liquid collector trays below the packing. Deentrainment of liquid is satisfactory as long as the
internals remain in good condition. Vapor distribution in the packed section just above the flash
zone is not very good, but high mass transfer efficiency in this particular section is not needed.
The various installations operate satisfactorily. Drawing RA 800096 is typical of columns built in
recent years, but note that this subject is still in active development.
The ethylbenzene recycle column in ChevronTexaco Chemical's new styrene plant at St. James
has a 20-in. feed-entry nozzle and a two-way deflector. See Figure 300−2. The streams produced
by this deflector will travel in opposite directions, nearly tangentially to the column wall and
slightly below the horizontal. Note that
• Total exit area of the deflector is four times the inlet nozzle cross section.
• The column is 29 ft. in diameter at the feed point.
• Clearance from the feed nozzle to the packing support above is 5 ft.
• Clearance to the liquid collector tray below is 3 ft.
In this case, the feed stream is small relative to the internal streams passing the feed point.
The Richmond Light Neutral Hydrofiner Vacuum Column, 7.0 ft. in diameter, has a two-way
feed deflector similar to the above, together with an annular-shaped collector tray about 1-1/2 ft.
below the 8-in. feed nozzle centerline. (Two other RLOP vacuum columns have similar feed
entries.) As shown in Figure 300−3:
• The collector tray covers about half the column cross section, the center portion being an
uncovered chimney for vapor passage.
• The collector tray drains to a conventional pan distributor 1-1/2 ft. below.
• Vapor passes through the pan distributor in covered risers.
A variation on the two-way deflector is a tee-shaped pipe entry located just above the annular
collector. Feed is discharged horizontally in opposite directions along the column wall. One
vendor recommends that each branch (which carries half of the total flow) be sized to provide the
cross section needed for liquid velocity of 7.5 ft./sec plus the area for a vapor F factor of 25.
The Alkane Rerun Still, a 5.5-ft. diameter fractionator at Richmond, contains a shroud over the
straight in feed inlet and an annular collector tray as shown in Figure 300−4. It has following
characteristics:
• A wear plate protects the shroud from erosion by the impinging two phase feed.
• Liquid drains from the collector to a pan distributor 14 in. below.
• Clearances are tight because the hardware had to be retrofitted into an existing column.
• The radial dimension of the shroud is only 6 in., yet one third of the column cross section
is lost.
The feed entry just described replaced an earlier, unsuccessful installation. Column performance
improved, but it remained below expectations; therefore this design is not recommended. A
possible reason is that a straight in entry to the inside of a shroud does not evenly dissipate the

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energy of the incoming feed. Another disadvantage of the shroud is that it complicates the
problem of entry. A manway with removable cover is needed in the shroud. If higher cost and
pressure drop can be accepted, the distributor in Figure 300−5 is recommended for non fouling
service. It is essentially a circular manifold discharging downward and toward the column wall.
The manifold clears the column wall by at least 6 in. to allow space for flanges, supports, fitup,
etc. The gallery below provides space for vapor/liquid separation and collects the liquid for the
distributor below.
364 Line Sizes
An entry nozzle to a column may not be the same size as the external piping bringing feed to that
column. Pipe size is based on economics and flow regime criteria; nozzle size is influenced by the
need for good distribution. In the absence of other information, an estimate of the external pipe
size may be made by using the "economic line velocity":
Equation 300-8
V = 40 ρ-1/3
where V = velocity, ft./sec
ρ = single or two phase (bulk) density, lb/ft.3
Examples: "Economic velocity" for water is 10 ft./sec; for a gas stream of density 0.01 lb/ft.3 ,
186 ft./sec.
A bubble point liquid from an upstream column may be throttled, with partial vaporization,
through a control valve to feed a downstream column at lower pressure. The percent vaporization
and bulk density chosen for sizing the line downstream of the valve probably do not correspond
to the downstream column pressure but rather to some higher pressure, partway along the line,
which includes elevation head and friction loss. Thus, the line size approaching the downstream
column is not as large as "economic velocity" at the column inlet would dictate.
Crude unit vacuum column transfer lines are an exception to the above practice; they are
frequently sized for close to critical velocity, which may be in the range 250-350 ft./sec.
365 Manifolds
A manifold is a section of pipe. Fluid enters at one end and exits through several holes or fittings
along the length. The far end of the pipe is closed. A manifold may be used to bring a liquid
stream to a parting box or to distribute a two phase stream into a vapor liquid disengagement
zone. The various branches of a spray or manifold distributor are manifolds.
If the kinetic energy of the stream entering a manifold is small relative to the friction loss as the
stream passes through the manifold, the holes or branches near the entry end will have higher
flows than those near the other end. Conversely, if the kinetic energy is relatively large, the fluid
will tend to "stack up" at the far end of the manifold and the holes at that end will have the larger
flows. In either case, the problem is handled by causing the head loss through the holes to be the
controlling resistance. A more complete treatment of manifolds is found in the Chemical
Engineers' Handbook.
If a manifold feeds a parting box or a pan distributor, then absolute evenness of distribution from
the manifold is not critical; holes should be sized such that the velocity through the holes, assum-
ing equal flows, is twice the velocity entering the manifold.
On the other hand, if the manifold is the primary controller of liquid dis tribution, then
maldistribution may have to be held as low as ± 5%. The ratio of hole pressure drop to either

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velocity head of the entering stream or friction pressure drop along the manifold may have to be
as great as 10. This condition may apply to the branches of a manifold distributor. In a spray
distributor, the nozzle pressure drop must be the controlling resistance.
Caution: Discharge of a two-phase mixture from a manifold can be unpredictable, particularly if
the entering stream is intermittent, e.g., slug flow. This applies both to flowrates and to
vapor/liquid ratios at various exits.
366 Maximum Discharge Velocity
Consider the discharge of a fluid from a nozzle or manifold, directed against column internals or
a liquid surface. Design guides for single phase streams are simple. Preferred maximum velocity
for a liquid stream is 5 ft./sec; 10 ft./sec is allowable if necessary. (Spray nozzles are not
restricted in this way.)
Maximum vapor velocity up to 90% of critical is acceptable as long as
• The jet impinges on the column wall, and
• The velocit y head can be neutralized by the method discussed in Section 353.
Two-phase streams are an area of uncertainty, and the following guidance is offered.
• If erosion is a concern, use whatever protection would be appropriate for a liquid stream
of the same velocity. An example might be a wear plate.
• If turbulence and disruption of internal flow are of concern and the stream is intermittent,
e.g., slug flow, apply the liquid criterion: 5 ft./sec preferred, 10 ft./sec allowed if
necessary.
• If flow is dispersed, e.g. mist flow, assume that the unit will tolerate the same amount of
energy release, per pound of stream flow, as would occur with water at 5-10 ft./sec.
Kinetic energy is proportional to the expression ρV2. (See Section 341.) For water at 5
ft./sec, the value of this expression is 1560; water at 10 ft./sec corresponds to ρV2 of
6240. The corresponding F factors are, in round numbers, 40 and 80. Use the bulk density
and velocity of the two phase stream. Example: a homogeneous two phase stream with
bulk density of 0.1 lb/ft.3 would have a preferred maximum velocity of 126 ft./sec with
253 ft./sec allowed if necessary.

370 References
1. McMullan, B. D., Ravicz, A. E., and Wei, S. J., "Trouble shooting a Packed Vacuum Column
-- A Success Story", Chemical Engineering Progress, July 1991, pp 69-74. (Please contact
A.G. Nelson of ERTC for a copy of this reference.)
2. Albright, M. A., "Packed Tower Distributors Tested", Hydrocarbon Processing, September
1984, pp 173-7.
3. Moore, F. and Rukovena, F., "Liquid and Gas Distribution in Commercial Packed Towers",
Paper presented at 36th Canadian Chemical Engineering Conference, October 5-8, 1986.
4. Kister, H. Z., "Distillation Operation", McGraw-Hill Publishing Company, 1990, page 80.

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Figures and Drawings

Figure 300-1 Spray Head Layout

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Figure 300-2 Two-Way Feed Deflector

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Figure 300-3 Feed Deflector with Close-Coupled Annular Collector Tray

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Figure 300-4 Straight-In Entry with Shroud

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Figure 300-5 A Circular Manifold Distributor

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Figure 300-6

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Section 400 Selection, Specification, Bid Review and
Inspection

410 Introduction
This section presents material useful when carrying out a packed column project. The focus is on
packing hardware, not the broader process, control, or project engineering pic ture. Brevity is
emphasized, with material in tabular or checklist form where appropriate. If explanation is
available elsewhere in the Manual, it is omitted here.

420 Packing vs Trays


Consider trays first. Choose packing only if you have a good economic reason to do so. Some
reasons to choose packing:
• To minimize pressure, pressure drop, or pressure drop per theoretical stage. (Vacuum
columns, temperature-sensitive material, columns with bottom pressure fixed and
overhead gas being compressed.)
• To minimize quantity of liquid held up in a section of a column. (Product degradation,
coking.)
• To debottleneck a vapor-loaded, low- to medium-pressure column. (High-capacity, sheet-
metal structured packing.)
• To debottleneck a liquid-loaded, low- to medium-pressure column. (High-capacity
packing or grid in a pumparound reflux section, random packing in a sidecut stripper.)
• To simplify internals of a small-diameter column, say less than 3 ft in diameter. (An
alternative is cartridge trays.)
• To handle a very corrosive system. (Ceramic random packing.)
• To handle a foaming system, maybe. (Packing has less tendency to generate foam, but
foaming can usually be handled with trays by use of larger downcomers.)
Characteristics of various trays and packings are compared in Table 400-1.

430 Packing Selection


431 Structured Packing vs Random Packing
In general, sheet-metal structured packing is up to twice as expensive, per cubic foot, as random
packing and installation is more difficult. Therefore, select structured over random packing only
if it makes good economic sense. Some reasons for choosing structured packing:
• To achieve higher efficiency at the same capacity, e.g., to revamp an existing column to
get more theoretical stages. In new construction, structured packing might allow putting
the required number of stages into a single column rather than two, a big saving.
(Columns at pressures up to 100-150 psig, liquid rates below 20 gpm/sq ft.)
• To get higher capacity at the same efficiency; e.g., to debottleneck an existing column.
(Same restrictions as above.)

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• To get better resistance to disturbance of packed beds by flooding, severe pressure waves,
etc.
432 When to Consider Grid
• Dirty, fouling, coking service.
• When high capacity is needed and reduced mass-transfer efficiency is acceptable.
433 Which Size Packing?
In general, the sharper and more difficult the separation, the greater the number of theoretical
stages that will be required and the more likely that a smaller size packing will be chosen. The
benefit is higher efficiency; the disadvantages are lower capacity, higher pressure drop, higher
packing cost (per cubic foot), and the necessity of using a top quality distributor in order to gain
the higher efficiency expected.
• In at least 80% of refinery and chemical plant applications, the packing chosen is of the
size closest in capacity to that of a 2-inch Pall ring.
• In a very few cases, a smaller packing is chosen. Example: three stripping section beds in
the ethylbenzene recycle column at the St. James Styrene Plant have No. 25 Norton
IMTP, about equivalent in capacity to a 1-inch Pall ring. The three beds, when in good
condition, provide about 45 theoretical stages.
• In crude columns, Fluid Catalytic Cracker (FCC) fractionators, and other heavy oil
applications, somewhat larger-size packings are common.
434 Efficiency (HETP) Estimation
See Section 200 for a complete discussion of packing efficiency. Briefly:
• Where possible, use commercial plant data for a similar system and set of process
conditions.
• Use pilot-plant data for a similar system and set of process conditions and assume that
HETP of the packing in the commercial plant will be 1.25 times the HETP found in the
pilot plant.
• Use the following table for 2-inch Pall rings. For modern metal-ring packings of equal
capacity, multiply HETP values by 0.8; for structured packings, multiple HETP values by
0.6.
Application HETP, ft
Fractionators in which very high values of tray efficiency (90% - 100%) would 2.5
be expected.
Examples: deisobutanizer, ethylbenzene/styrene separation
Fractionators with 80% - 90% tray efficiency. 3.0
Fractionators with 60% - 80% tray efficiency. 4.0
Example: depropanizer.
Strippers, gasoline splitters, crude fractionators (50% tray efficiency). 5.0
Absorbers and other very low tray -efficiency applications. 8.0 - 10.0

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440 Suppliers and Brand Names of Packing


Following are the major North American suppliers of packing for industrial use. Their products
are used in ChevronTexaco plants and are considered acceptable. The omission of other suppliers
(ACS, Jaeger) does not imply that they are unsuitable.
• Glitsch, Inc., P. O. Box 226227, Dallas, Texas 75266, telephone 214-631-3841.
• Koch Engineering Company, Inc., P. O. Box 8127, Wichita, Kansas 67208, telephone
316-832-5110.
• Norton Chemical Process Products, P. O. Box 350, Akron, Ohio 44309, telephone 216-
673-5860.
• Nutter Engineering, P. O. Box 700480, Tulsa, Oklahoma 74170, telephone 918-446-
6672.
Brand names of metal-ring random packings , the most common type used in ChevronTexaco
applications, are given in Table 400-2. The older "generic" pall ring has been in use since the
1950s. "Improved" rings are of the pall ring form but are made of thinner metal, are slightly
larger than the equivalent pall ring, and have slightly higher capacity. In the "Premium" column is
each vendor's latest, most modern packing, usually the one marketed most aggressively.
The various forms of structured packings are in Table 400-3.
Each of the packings comes in a variety of sizes or capacities; these are listed in vendors'
catalogs.
An exhaustive list of packings is given in Reference 1.

450 Specifying a Packing Installation


451 New Construction and Major Revamps
In this section, assume that we have detailed knowledge of the process and that we want things
done "our way". We begin at the point where the process flow diagram is complete. The
following steps have been taken:
• Process conditions for the column have been chosen, and mass and heat balances have
been computed.
• The reflux ratio, internal traffic, and number of theoretical stages in each section of the
column are known.
• We have chosen the general type and size of packing and have determined column
diameter(s) and heights of beds.
We will ask the vendor to confirm the process parameters and to select the particular packing that
he will offer.
Preparation of the control diagram and the piping and instrumentation diagrams may be
underway, also. At this point, consider troubleshooting instrumentation. Identify all the points at
which trouble might occur. Will there be at least pressure taps available to help in diagnosis?
How about temperature points, samplers?
The next step is to present the information a vendor will need in order to bid. One way to do it is
with the following three documents:

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• A column outline drawing. In a revamp, this may be an altered "wash-off" of an earlier


drawing. This drawing shows the various items of internal hardware in correct
relationship to one another and gives key dimensions for placement. For an example, see
Drawing RC 871712- 1 in Appendix 400-A.
• A table of internal stream rates and properties. See Drawings RA 871785 and RA 871786
in Appendix 400-B.
• Written specifications giving detail on turndown, fouling resistance, pressure drop,
quality of distribution, resistance to dislodgment, etc. For an example, see RA 871715
through RA 871717- 1 Appendix 400-B. [If this material is reproduced for other use,
please remove original reference to plant, project, etc.]
452 Smaller Projects
In a smaller project, particularly a revamp, some information can be omitted that vendors can
supply. For example, the vendor may be asked to suggest the appropriate type and size of packing
to satisfy specified values of number of stages, pressure drop, column diameter, and available
height. The important point: there must be a process engineering basis for any project.
A simpler presentation of the data may be appropriate. The data sheet shown as Appendix 400-A
was developed by the Design Practices Committee of Fractionation Research, Inc. (FRI). It may
be used as-is or modified.
When asking vendors for competitive proposals, state your design basis and requirements as
specifically as possible. The more general the question asked, the more varied and superficial the
responses.
Don't expect a vendor to do extensive process engineering free of charge. Do it yourself, have
ERTC or an engineering company do it, or have a qualified vendor do it under contract.

460 Reviewing Bids and Budget Cost Estimates


A bid is basically a written offer to supply certain items of hardware as listed elsewhere in the
document. Following are the items specifically in the area of packing technology that should be
checked:
• Did Bidder omit any equipment items required by the specification? Did he propose
additional items not called for? Did he take exception to any items in the specification?
Why? Example: Company does not always call for a hold-down grid at the top of a bed
of metal rings; Bidder might question this.
• Did Bidder correctly transcribe and use the data given in the specification? Are those
derived numbers which can be checked correct? Example: given column diameter and
bed height, did Bidder quote the correct volume of packing; did he include overage to
cover the possibility that packed density in the column may be higher than in the shipping
containers?
• Did Bidder do capacity (pressure drop) calculations to confirm the column diameter or to
choose the packing size? Can you check them independently?
• Did Bidder quote an appropriate packing of the specified material? If he quoted a
premium packing in place of generic Pall rings, is the extra cost justified? Is the packing
size (capacity) appropriate? In a competitive situation, a vendor is likely to quote a
packing size larger than needed (lower cost per cubic foot), claiming that it will still have
the required efficiency.

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• At this stage, a vendor will give minimum detail on collector trays, hold-down grids, and
liquid and vapor distributors, possibly just citing catalog figure numbers. However,
Company must be assured that the distributors, when designed, will be of appropriate
quality. The vendor should state his acceptance of the design and performance criteria
given in the specification. Example : if high quality distribution is needed, a v-notch
distributor is not going to provide it. See Section 300 of this manual.
• Does the price include flow testing of distributors at the vendor's shop? This test is
recommended for high-quality distributors.
• Does the bid include installation? Probably not. In a moderate to large project involving
proprietary hardware, the cost of having a packing vendor representative on site during
installation is usually justified.

470 Reviewing Detailed Designs


Begin with those items in Section 460 that may apply. Continue with the drawings that describe
the installation in detail, following in the order below, and check each item for consistency with
the items before it. Reminder: the focus of this section is the packing installation. Piping,
structural, materials, and control aspects are not included.
471 Column (Vessel) Drawing
The main purpose is to show the column details, but major packing hardware is also shown,
usually in simplified form. You will come back to this drawing many times.
• Is diameter of each column section correct?
• Is every specified major item of internal hardware shown or indicated: manifolds, a liquid
distributor for every entering or internal stream that needs one, hold-down grids or bed
limiters, beds of packing, packing or grid support plates, liquid collectors, vapor
distributors?
• Review the nozzle (connections) list. Are they all there? Check feeds, products, reflux,
reboiler feed and return, pumparound withdrawal and return, stripping steam entry, vapor
returns from sidecut strippers, manways, thermowells, pressure taps, level gage and
controller connections, sample taps, viewing ports (very rarely). Check those items (e.g.,
pressure points, sample points) which may not be used at all unle ss trouble develops but
will be very important if it does; they tend to be overlooked or arbitrarily deleted for cost
reduction.
• Check nozzle sizes. Some are standard (thermowells) but most are sized according to
flow. In a vacuum column, there will be big vapor lines. See Section 300 for discussion
of vapor entry effects on packing performance.
• Manways: In general, you need one at the bottom of each packed bed, just above the
support plate; one at the top, just above the liquid distributor; and one to give access to
the bottoms surge volume. But note that there is a trend to eliminate manways at bottoms
of beds. If packing is to be unloaded, it will be vacuumed out, not dumped. Large
columns often have manways in pairs, on opposite sides of the column. Diameter of 20"
is tight, 24" is better, 30" is better still. The higher the operating pressure, the thicker the
column wall, the more expensive a manway is, the harder it is to justify each of them. On
the other hand, in a revamp you may find that there will be unnecessary "leftover"
manways and other nozzles covered by packed beds. These can mean trouble, particularly
in smaller columns with low liquid loading. Reason: heat loss creates additional

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(maldistributed) reflux running down the wall of the column. Such nozzles should have
plates to keep packing out of them and should be insulated to minimize heat loss.
• Now check vertical dimensions (for the first of several times). Are packed beds the right
depth? Are manways at about the right elevations? Are pressure taps in vapor spaces
between beds? Is there a reasonable clear height between beds. (Depending upon
operating pressure, column diameter, and complexity of column internals, "reasonable"
can be from 2 to 12 ft.) If redundant dimensions are given, are they consistent with
others?
• If the project is a revamp, say from trays to packing, the vessel drawing will show field
modifications to accommodate the packing. Remove unused tray rings and other inside
attachments. In particular, those which will be covered by the new beds of packing
should be cut off to within 3/8-in. of the shell. (This is about as close as a torch can cut
without affecting strength of the shell.) Debur any sharp edges.
• Read the notes. They should include required levelness of support rings. Even in a large
column, 1/4-in. from highest point to lowest is reasonable.
• Get familiar with the little drawing insert, a plan view, labeled "Nozzle Orientation" or
"Plan of Connections". It's important but easy to overlook. In a revamp, it can get
complicated. Mistakes here can result in rework and lost time during installation.
• Will there be platform access to the points you may need to get to? Working from
ladders or scaffolding can be difficult.
• Might there be the need to do gamma scanning of the column to troubleshoot problems?
What future access problems could be prevented now?
472 Installation Drawing
In a major project, the packing vendor may furnish an elevation drawing of the column looking
much like the vessel drawing. Its purpose is to show the arrangement of every item of packing
hardware. It may list drawing numbers of individual items.
• See that all dimensions are consistent with vessel drawing.
• Does the hardware match the specification and vendor's bid?
• In a large diameter column, distributors and packing support plates will involve support
beams or trusses. These are fastened to support rings and/or pedestals, which are part of
the vessel. Check all elevations.
• Take a first look for interferences. Look at depth of beams and trusses, any standpipes on
distributors, piping and manifolds connecting inlet nozzles to distributors. Any blockage
of manway access?
• Is the feed stream two-phase? How is it handled? Some recommended details are in
Section 300.
• The notes may show sequence in which items are installed. Any problems?
473 Liquid (Gravity) Distributor Drawings
Work your way down from the top of the column, but take similar items, such as distributors,
together. Look first at any piping from inlet nozzle to distribution manifold (if any), then
manifold delivering to predistributor (if any), then predistributor, then main distributor. If internal
liquid is collected and then redistributed, check placement of the downcomers from collector to
distributor. (You'll review these downcomers again when you look at collector trays.)

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• Does distributor satisfy the specification in regard to drip-point density (number per sq ft
of column cross section), minimum hole size, etc?
• Is there special provision for drip points close to the column wall, perhaps underneath the
tray-support ring?
• Check elevations shown on detailed drawings. Are they consistent with column and
installation drawings?
• Are orientations consistent with those of other internals and with nozzle orientations
shown on column drawing?
• Check flange details of any vendor-supplied piping that must mate with column-nozzle
flanges.
• Drawings should indicate design flow rate, required turndown and/or turnup from the
design point, and the pressure drop or liquid head for each. Can you confirm, using the
methods of Section 300? If distributor is a pan with chimneys (risers), check design gas
rate and pressure drop also. Liquid level on the tray will be that needed to overcome
liquid pressure drop through the holes plus the vapor-phase pressure drop through the
chimneys.
• How is distributor to be supported? With random packing, distributor will be supported
by column wall or be hung from other internals above. With structured packing,
distributor might be supported by an open grid placed on top of packing. Is there
provision for final leveling? If supported by tray ring, outer diameter of pan distributor
should overlap tray ring but allow for thermal expansion and column out-of-roundness.
(The ASME Code requires that diameter be within 1% of nominal diameter.) Fastening to
tray ring, clamps or through- bolting with slotted holes, should also allow for thermal
expansion.
• Does construction generally minimize the number of seams? Are mating pieces of
flange d connections made of plate at least 1/4-in. thick? (Section 312.)
474 Spray Distributor Drawings
A spray distributor is usually used in a service subject to coking. Some decrease in distribution
quality is accepted in return for minimizing liquid residence time and coking tendency in the
distributor.
• Check elevations, orientations, and flange details as in the case of a gravity distributor.
• See the pressure drop and layout recommendations in Section 300.
• The controlling pressure drop must be in the spray heads. Check to see that pressure drop
between the inlet nozzle at the column wall and any spray head is small (less than 10%)
relative to the spray-head pressure drop.
• It sometimes happens that spray heads attached to or on pipe stubs from the main line of
the manifold are at a slightly different elevation from those on branch lines. This is okay
as long as spray-head pressure drop controls.
• Check the spray-head catalog to see that the "minimum free-passage diameter" of the
spray nozzles is at least 3 times the maximum particle size which can pass through the
strainers on the piping to the distributor. A common specification for the strainers is 1/32-
inch particle size.
• Check spray-head pressure drop against the catalog. For each spray-head model, the
catalog lists the gallons/min flow of water (at room temperature) corresponding to each

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of several standard pressure drops (in psi). Directions are given for interpolating between
the standard values of pressure drop and for correcting for a liquid of specific gravity
different from that of water. Note: the "specific gravity" used here is the ratio of the
density of your liquid at flow conditions to the density of water at room temperature. To
find the nozzle pressure drop for your liquid and flow rate, proceed as follows:
• The water flow rate equivalent to your liquid rate is your rate per spray head at flow
conditions multiplied by the square root of the ratio (density of your liquid at flow
conditions/density of water at room temperature--8.34 lb/gal or 62.4 lb/ft 3).
• Then go to the table in the catalog, where your equivalent water rate will probably not
match one of the table entries. To adjust, use a nearby entry. Your pressure drop is
obtained by multiplying the tabular pressure drop by the square of the ratio (your
equivalent water flow rate/tabular water flow rate).
475 Hold-down Plate and Bed-limiter Drawings
A hold-down plate rests directly on (is supported by) a bed of random ceramic or carbon packing
in order to prevent it from being "fluidized" by pressure surges and to take up any slack if the bed
settles. A bed limiter or retaining plate, on the other hand, is used with plastic or metal packing
and is supported by the column wall.
If the packing must withstand severe pressure surges, the bed limiter must be solidly fixed in
place. If surges are not expected, you don't need a bed limiter. For conditions in between, many
"bed limiters" for metal packing (not plastic) rest on the packing, particularly when the liquid
distributor is only a few inches above.
A hold-down plate or bed limiter for random packing consists of a tray ring and an array of bars
to which a coarse woven or expanded metal screen is attached. For sheet-metal structured
packing, the screen is omitted.
• With random packing, check to see that the ring comes close enough to the column wall
and the screen is of sufficiently small mesh size that packing elements cannot escape.
• Check elevation and orientation of column attachments for bed limiters.
476 Packing Support Tray Drawings
The usual support tray for random packing is the "corrugated" gas injection tray with "ridges"
extending up about a foot from the lowest points or "valleys". Liquid collects in the valleys and
runs out through holes or the spaces between plate sections. Gas flows through the perforated
sides of the ridges and into the packing. Designs are pretty standard.
• Check to see that the hole and slot size is sufficiently small to retain the packing particle
size that will be used.
• Be sure that there are no gaps between sections through which packing could escape.
• In some cases, where the designer wants additional pressure drop for vapor distribution
(see Section 311), the packing support tray will be a pan with perforations for liquid flow
and chimneys for vapor.
• Check vapor pressure drop and liquid head as in Section 473, item 5. To minimize chance
of plugging, hole size should be limited only by the need to retain the packing.

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477 Collector/Drawoff Tray Drawings


These trays collect internal liquid for drawoff and/or internal redistribution. They may also
function as vapor distributors. The most common construction is a pan with chimneys for vapor
passage and a sump for collection of liquid. To minimize pressure drop in a vacuum column, the
collector may consist of branch troughs leading to a center sump with covers over the open spaces
between troughs.
• Check design flow rates and pressure drop as in Section 473.
• Check elevations and orientations for consistency with the column and installation
drawings.
• If this is a drawoff tray, one end of the collection sump must abut against the column wall
and line up with the drawoff nozzle. The lower level controller lead must be in the liquid
near the bottom of the sump, the upper lead in the vapor space. If there is to be a vortex
breaker, is the column or the packing vendor responsible for it?
• Preventing leakage will be important. If this is a pan, consider seal welding everywhere
except the support ring, where thermal expansion must be allowed. The support ring itself
should have a continuous weld at the wall. Some vendors use an "expansion ring" seal-
welded both to the tray and to the column wall. Offset above the tray allows for thermal
expansion without breaking the welds. How about liquid running down the wall?
Depending upon tray construction, a wall wiper may be needed to get liquid into the tray.
• In coking service, you want minimum liquid residence time and tall chimneys to allow
for coke buildup before it interferes with vapor flow.
478 Grid Installation Drawings
Grid is appropriate in columns subject to fouling and coking, in areas subject to upset (pressure
surges, high-liquid levels), and in cases where other internals would be overloaded. Coke buildup
on grid is minimized by good performance of liquid distributors (usually but not always spray
distributors) and provision for even vapor distribution.
When reviewing the grid installation itself, we are usually concerned with strength. Was the
requirement for strength communicated to the vendor and did he respond?
• How is the grid to be held up? Usually by a high-capacity grating, supported by beams, a
support ring, pedestals, etc.
• Perhaps more importantly, how is the grid to be held down? A badly coked grid will
restrict vapor flow and may be subject to extreme upward force. You will need high-
strength clips to hold the grid to the support ring at the column wall. The grid should be
firmly attached to any support beams; this has been a common weak point in the past. A
hold-down plate on top of the grid, secured to the column wall, may be used.
• How is the grid to be held together? The grid comes in layers 2-3 in. thick. Under some
circumstances, "J-bolts" or "hook-bolts" are used to tie adjacent layers together, but this
does not provide the strength often needed. A preferred method is support grid below,
hold-down grid on top, and threaded rods at regular intervals passing completely (top to
bottom) through the grid bed and tying it together.

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480 Process Inspection


Inspection may involve the following steps:
• Inspect fabrication at a vendor's shop for conformity with previously approved drawings.
• Witness demonstration/test of a critical liquid distributor at the vendor's test facility.
• Review test assembly of hardware outside the column.
• Inspect periodically as installation proceeds.
• Conduct process inspection of installation after completion.
This section deals primarily with the last step.
Inspection is not a routine, mechanical activity. You're looking for things out of the ordinary. If
necessary, do the inspection in several sessions, short enough to maintain mental alertness. At
each step, ask yourself, "What is going to happen here and how does the hardware make it
happen?"
As in other sections, the focus here is on packing technology only; other important subjects such
as personnel safety are not covered.
481 Recommended Equipment
• Drawings of the internals to be inspected (but study them thoroughly beforehand; you
won't do much reading in the column.)
• Two flashlights in good order.
• Notebook, pencils, pens.
• Yellow crayon.
• Tape measure.
• Carpenter's level. (For large-diameter columns, the "water balance" apparatus shown in
Figure 400-1 will allow you to measure elevation differences of 1/8-inch as much as 30 ft
apart.)
• Small pocket mirror.
• Disposable camera.
• Adjustable wrench.
• Knapsack or duffle bag.
482 In General
• Is the column shell reasonably clean and are internals scrupulously clean? No loose rust
or scale on walls, no rust at all on packing and internals, no construction debris (weld
rods, pieces of gasket material, tags, bits of tape), all dirt and dust vacuumed up?
• Are all fasteners tight? This includes flange bolts on internal piping; shackles supporting
such piping; clamps holding pans to support rings; bolted joints in distributors, hold-
downs, and support plates. If lock washers or double nuts are called for, are they in
place?
• Are gaskets installed as specified by vendor (and omitted where not called for)?

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• Has proper provision been made for thermal expansion? Check slotted holes in plate,
clamps intended to allow limited slippage at support ring, shackles, etc.
• Evidence of damage to any internals? If so, has it been properly repaired? Does
everything fit without being forced into place?
483 Gravity Distributors
• Levelness is all-important. Check it thoroughly. The usual requirement is 1/4-inch
maximum to minimum elevation.
• Are perforations the right diameter? Wrong sizes do happen.
• Follow the course of liquid flow. Are all passageways between compartments clear?
Check for blockage by gaskets or misalignment.
• Do predistributor manifold perforations line up properly with parting boxes? Do parting
box perforations line up with distributor troughs? How about elevations of the various
parts? Will there be excessive impingement by liquid streams?
484 Spray Distributors
• Is the correct spray-head model being used?
• Are spray heads properly located and at the correct elevation above the packing?
• If spray heads are already installed, is it understood that they must be removed for line
flushing before startup? Screwed-on spray heads are sometimes spot welded to stubs
during final assembly.
• Is every branch of the manifold properly supported and held in place against vibration?
• In rare cases, a spray distributor for an entering stream is used in conjunction with a
gravity distributor for an internal stream. They will be at about the same elevation and
must not interfere with one another. Check for obstruction.
485 Hold-down Plates and Bed Limiters
• Is screen mesh size correct? Screen firmly attached? If screen attached by welding, was
welding done properly and without burning holes in screen?
• If bed limiter, is it firmly attached to wall? If hold-down plate, is it free to move without
binding? Are both level?
486 Packing Support Trays
• Check for absence of gaps through which packing can escape.
• If this is the gas distributing type (pan with chimneys), are dimensions of gas risers and
liquid drainage holes correct?
487 Collector/Drawoff Trays
• Tightness is crucial. Check gasketing and seal welding for completeness and absence of
leaks. Seal welding is appropriate between various tray parts, but it should not be used
between the tray and the support ring. (Thermal expansion.) The support ring should be
continuously welded to the wall.
• Are the required weep holes (and only the required number) there? Sumps drain through
drawoff nozzles; they should not need weep holes.
• Is sump correctly aligned with drawoff nozzle? How about level-control taps?

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• If this is a trough-type collector tray (common in vacuum columns), is there provision for
catching any liquid which is running down the wall?
488 Grid Installations
• The main concern is that the grid bed be properly supported, held down, and held
together. Check all attachments.

490 References
1. Kister, H. Z. , "Distillation Design", McGraw-Hill, New York, 1992, p. 421ff.

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Tables and Figures


Table 400–1 Characteristics of Trays and Packings
Maximum Operating Pressure Resistance Ease of
Device Efficiency Capacity Range Drop Cost to Fouling Maintenance
8% Sieve High Medium Medium High Low Good Medium
14% Sieve Medium High Narrow Medium Low Good Medium
Bubble Cap High Medium Wide High Medium Medium Medium
Valve High Medium Widest High Low Medium Medium
Baffle Low Very High Wide Low Low Best Easy
Dualflow High Medium Narrow Medium Low Very Good Medium
Random High Medium Wide Low Medium Poor Difficult
Packing
Sheet Metal Very High High Wide Very Low High Poor Difficult
Structured
Packing
Grid Low Highest Wide Lowest Medium Very Good Medium

Table 400–2 Metal Ring Random Packings


Supplier Older (Generic) Improved Premium
Glitsch Ballast ring Ballast Plus Cascade Miniring (CMR)
Jaeger Tri-Packs, VSP
Koch Flexiring K-Pac, HcKp Fleximax*
Norton Pall ring Hy-Pak Intalox Metal Tower Packing
(IMTP)
Nutter -- -- Nutter ring
* Fleximax has the superficial appearance of a saddle made of expanded metal.
Koch calls it neither a ring nor a saddle.

Table 400-3 Structured Packings


Supplier Sheet Metal Grid Wire Gauze
ACS -- -- ST-100
Glitsch Gempak Glitsch C and EF-25A Goodloe
Jaeger Max-Pak -- --
Koch Flexipac Flexigrid 2 and 3 Sulzer Gauze
Norton Intalox Structured Packing -- --
Nutter Montz B1 and BSH Snap-Grid Montz A

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Figure 400-1 Water Balance Apparatus

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Appendix 400-A
Packed Tower Data Sheet

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Appendix 400-B
Process Specifications Packing and Packed Tower
Internals Fractionation Sections

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Section 500 Packed-Column Troubleshooting and Testing

510 Introduction
This section contains material on:
• Diagnosing problems in packed columns.
• Conducting test runs.
• Analyzing the data from test runs.
The focus is on packed columns, but much of this material will apply to trayed columns also.
Little coverage is given to column auxiliaries such as condensers, reboilers, pumps, etc. For
broader coverage of troubleshooting, see References 1 and 2.
Why do we need this material? Because in general, packed columns are more difficult to operate
and maintain than trayed columns.
• Packing holds up less liquid than trays do. As a result, a packed column reacts more
quickly to process changes than a trayed column does, giving an initial impression of
instability.
• Liquid distributors are susceptible to plugging. Gravity-flow distributors get out of level.
The low pressure drop in packing makes a packed column more susceptible to vapor
maldistribution than a trayed column. Poor distribution de creases separation efficiency.
• Pressure surges can disturb packed beds, releasing particles of random packings which
ultimately find their way into distributors, strainers, and pumps. Improperly supported
grid beds have fallen apart.
• Fouling, debris, and polymers plug packing. Because of the thin metal used in packing, a
corrosion rate which would take many years to weaken trays will cause packing to
crumble in a much shorter time. Plastic packings have been destroyed during column
steamout.
The above statements are not intended to be excessively negative, only realistic. However,
packing should be chosen over trays only where there are good process and economic reasons to
do so.
Most problems in packed columns are caused by out-of-level, plugged, or poorly designed liquid
distributors. (Section 300 of this manual contains criteria for good design.) There are other
causes, however, many of them outside the column. The purpose of much of this section of the
manual is to be sure that other causes are not overlooked.

520 Tools for Diagnosing Problems


One of the most effective, and often overlooked, diagnostic tools is good record keeping.
Reference to recent operating history, without extensive analysis, is often enough to solve
problems. The routinely taken operating data will include rates and analyses of feed and products
as well as key temperatures, pressures, and utility rates.
Another effective tool is pressure-drop measurements. Regularly log pressure drops across each
packed bed and across the total column. Monitor pressure drops across spray and manifold
distributors. In pan distributors and those trough-type distributors in which the troughs are

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interconnected, gage glasses or manometers can be used to measure liquid depth. If fouling or
coking of a pan-type collector tray is expected, pressure drop across that device should be
monitored.
Reference 3 describes unusual sampling methods that detected internal liquid composition
variation from place to place at the bottom of a packed bed. This variation was related to
nonuniformity of liquid distribution at the top of the bed.
Measurement of temperature variation in a horizontal plane, either above, within, or below a
packed bed, might appear to be another useful way to detect nonuniform flow. (In trayed
columns, the corresponding technique, liquid temperature measurement in the downcomers of
two- and four-pass trays, has been effective.) However, in a packed column, a thermocouple
exposed to both liquid and vapor might be subject to considerable "noise". Such temperature
surveys have so far received little notice as a diagnostic tool.

530 Organization of Troubleshooting Material


A four level approach to the investigation of problems in packed columns is presented. Levels are
the following:
• Symptoms : what is observed by the operator or technical service engineer.
• Mechanisms : what is happening in the column or the surrounding plant to cause the
observed symptoms.
• Conditions : what is wrong in the column, causing the mechanism to occur.
• Fixes: what can be done to fix the condition, prevent the mechanism, relieve the
symptoms, etc.
In such a structure, not every problem may have a corresponding entry at each level. In many
cases, once the condition is identified, the fix is obvious. Nevertheless, the structure may be
useful. Cross references are provided to help you find your way through the structure.

540 Symptoms and the Possible Mechanisms Causing


Them
The following material is worded as if the symptoms were found on initial operation of a new
column. However, if the symptoms appear after a well-documented period of good performance,
then comparison of the two operating modes might make the trouble shooting job much easier.
541 Symptom: Column Does Not Make the Expected Separation
• Analytical problem; quality of separation is really okay.
• Feed composition different from design, making separation more difficult.
• Ratio of key compositions in feed or percent vaporization of feed is different from
design, making present feed location non-optimum.
• Internal reflux or boilup ratio is different from the design or intended value. This might
be due to controller error or an unexpected degree of reflux subcooling.
• Column is, in fact, making the required separation. Product is being contaminated, e.g.,
by a feed/bottoms heat exchanger leak or by bypass of material through auxiliary or
instrument piping.

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• Column heat or material balance control is unsteady; the "cut point" is constantly
changing.
• Packing's efficiency is in fact lower than expected. (See Section 552.)
• Vapor and/or liquid distribution is poor, causing apparently poor packing efficiency. (See
Sections 553 and 554.)
• Column is close to the flooded condition, and backmixing of vapor and liquid is
decreasing packing efficiency. (See Section 551.)
542 Symptom: Column Product Rates are Unsteady
• Feed rate or composition is varying, and the control system is reacting appropriately.
• Feed enthalpy is varying, and the control system is not reacting adequately. (A
feed/bottoms exchanger without a controlle d bypass on either side is a common
contributor to this problem; unsteady bottoms flow causes unsteady exchanger duty,
which causes unsteady feed enthalpy, which further upsets the column heat balance.)
• Condenser duty is varying because of a problem on the coolant side and/or reboiler duty
is varying because of a problem on the hot side.
• Level control problem: holdup in reflux drum, on drawoff tray, or in bottom surge
volume is varying.
• Pressure control problem: a decrease of pressure causes production of additional vapor
throughout the column and increased distillate rate; an increase of pressure causes
condensation and increased bottoms rate.
• Liquid holdup in packed beds is high and unstable. Column is close to flooding. (See
Sections 551 and 555. )
543 Symptom: Column Pressure Drop is Higher Than Expected and/or Unsteady
• Column is being "bumped" by wet steam (slugs of water).
• Liquid holdup and local flooding are occurring on packing support plate(s). (See Section
555.)
• Control problem is causing high level on collector/drawoff tray or in surge volume at
bottom of column, interfering with vapor flow.
• High pressure drop is occurring in chimneys of collector tray or pan distributor. Note: if
liquid must flow by gravity through collector tray or distributor, excessive pressure drop
in chimneys will increase liquid holdup. (See Section 556.)
• Packing condition is normal, but traffic is higher than expected and is overloading the
packing.
• Vendor's pressure-drop estimate was optimistic.
• Total pressure-drop estimate did not include pressure drop through vapor distributor,
collector trays, packing support plates, or (in case of high-pressure column) of vapor
static head.
• Packing capacity is in fact lower than it should be. (See Section 551.)

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544 Symptom: Column Operating (Top) Pressure is Unsteady


If a steady pressure, at the intended value, cannot be held at the top of the column, then other
elements of the control system will not be successful either. See Reference 4 for discussion of
column pressure control.
545 Symptom: Column Condenser is Out of Heat Balance
The specific symptom referred to here is that the condenser duty computed from hot side (process
side) flow rate and process conditions is too great. By "too great" we mean greater than the
condenser duty computed from the cold side conditions (in those cases, usually water-cooled
condensers, where this calculation is possible) or greater than that computed by complete (overall
column) heat balance.
The hot process stream to the condenser is equal to the sum of the reflux plus the distillate
product(s). It is normally a dew-point vapor stream at the column top temperature. However, if
this stream to the condenser should contain a significant quantity of liquid entrained from the top
of the column, then the condenser duty computed on the basis of dew-point vapor feed will be
greater than the actual condenser duty.
Imagine a column operating in the normal manner. The column overhead stream is dew-point
vapor (only). It is condensed to bubble-point liquid, which forms liquid distillate and reflux. Now
something causes entrainment of liquid into the column overhead. This additional circulating
liquid stream is cooled somewhat in the overhead condenser but has little effect on the column
heat balance. It appears as an increased reflux rate.
In summary, the symptom may be caused by the mechanism of liquid entrainment out of the top
of the column. (Another, more commonplace possibility is error in measurement of temperature
or flowrate.)

550 Mechanisms and the Conditions Causing Them


551 Mechanism: Packing Has Lower Capacity (Higher Pressure Drop) Than it
Should
• Packing is plugged, fouled, coked, etc. If packing was recently cleaned, the cleaning was
only partially effective. This affects efficiency also. (See Section 561.)
• Packed bed is more dense than it was before, due to collapse of metal packing, softening
of plastic packing, or breakage of ceramic packing. This affects efficiency also, since
density increase is not uniform. Slow "grinding" of ceramic packing has also been
observed in beds which are highly vapor-loaded and not completely restrained by hold-
down grids; this results in "grit" collecting in the surge volume, the bottoms pump, etc.
(See Section 562.)
• The method of packin g the bed has caused it to be more dense than expected. Example:
"dry" packing gives a denser bed than "wet" packing. (Efficiency will not be affected
unless reduced capacity causes overloading.) Caution: random packings of different sizes
or shapes should not be mixed.
552 Mechanism: Packing Has Lower Efficiency Than it Should; Capacity is
Okay
• Bed is too deep. Liquid distribution to the top of the bed and vapor distribution to the
bottom of the bed are okay. Maldistribution, probably in the form of increased wall flow,
has developed "normally" in the lower portion of the bed. (See Section 563.)

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• Liquid loading is too low although quality of distribution is okay. The concern is that
liquid does not completely wet the packing surface. The lower limit on loading varies
with system properties, packing material, and vapor loading. It is probably around 0.2
gpm/sq ft.
553 Mechanism: Liquid Distribution is Poor
• Spray or manifold distributor is partially plugged (Section 561) or is leaking at gasketed
joints.
• Pan or trough distributor is partially plugged (Section 561), is out of level, has leaking
seams, or is operating outside of its design range (either too low a rate, causing uneven
distribution, or too high a rate, causing uneven overflowing).
• Collector tray is allowing liquid to leak at wall; this liquid bypasses distributor tray
below.
• Hats covering chimneys (vapor risers) of collector/redistributor tray are missing, allowing
liquid from bed above to fall directly and unevenly onto bed below.
• A two-phase feed is handled poorly, allowing the liquid portion to land unevenly on the
packing.
• Liquid distributor was not designed properly. See Section 300, Liquid and Vapor
Distributors.
• Significant heat loss through uninsulated flanges, manway covers, etc. is generating
additional reflux in the column. This liquid flows down the column wall.
554 Mechanism: Vapor Distribution is Poor
• Chimneys in collector tray immediately below packing are partially blocked, creating
high-velocity currents.
• A high-velocity vapor stream from the reboiler or stripping steam entry impinges on the
bottom of the bed. Note: vapor distribution is an important factor in efficiency, mainly in
packings such as structured packings, which have very low pressure drop per foot of
height. See Section 300 for discussion on how increased pressure drop through a vapor
distributor or packing-support plate can be used to even out vapor flow.
555 Mechanism: Liquid is Held Up on Packing Support Plate
• Design is improper. Modern packings require a high-capacity, "gas-injection" type of
support plate.
• Debris or polymerized material is partially plugging liquid channels of support plate.
556 Mechanism: High Pressure Drop in Chimneys
• Chimneys are partially plugged.
• Chimneys are undersized. Chimney area is normally 10-25% of column cross section;
15% is average.
557 Mechanism: Liquid is Entrained Out of the Top of the Column
• Column (packing) is overloaded.
• Liquid on a pan-type distributor is being held up to the point that vapor chimneys are
partially blocked.

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560 Fixes for the Most Common Conditions


561 Condition: Plugging of Liquid Distributors and Packing
The following material is condensed from Reference 3, Section 300 of this Manual.
• Keep rust and debris out of the column. Use parallel strainers, without bypasses, on feed,
reflux, and any pumpback streams to the column. Strainers should have 1/32-inch
perforation size and be located as close as possible to the column. Use stainless piping
between strainers and column.
• On startup, use line-washing procedures which flush debris away from column. Flush
lines and manifolds before installing spray heads. Beware of debris collected in tank
bottoms.
• Minimize use of gasketing. Where possible, mating surfaces of distributors should be
constructed of heavy plate without gaskets.
• Prevent rusting of carbon steel packing. Dry such packing thoroughly before startup and
prevent water entering column thereafter. Rust may be removed from packing by
chemical cleaning in place, but the procedure does not clean completely.
562 Condition: Co llapse, Softening, Breakage of Random Packing
Collapse of metal packing is caused by corrosion and extremely rough handling. A load of
stainless packing was ruined by being washed with hot, chloride-containing water. Some of the
newer ring-type packings are made of much thinner metal than earlier Pall and Raschig rings
(1/16-in. wall).
Plastic packings are susceptible to high temperatures. Column steamout on shutdown has ruined
many loads of plastic packing.
Ceramic packings must be handled carefully during shipment and column loading. Screening for
removal of fragments is not usually successful; additional packing is broken during the screening
operation. "Wet packing" is used for ceramic packings: a water level is maintained in the column
several feet above the packing surface; individual boxes of packing are emptied just above the
water surface.
Restrain plastic packing by a bed limiter, which is supported by being attached to the column
wall, not by resting on the packing. Retain ceramic packing by a hold-down grid, which rests on
the packing. Metal packing is not always restrained, but should be if highly vapor-loaded. Either a
bed limiter or a hold-down may be used; a bed limiter is preferred.
563 Condition: Excessive Bed Depth
(This clearly is a design problem, not a condition which may develop during operation.) The
usual rule for maximum bed depth is 30 ft or the height equivalent to 10 theoretical stages,
whichever is less.

570 Conducting a Test Run


In the present context, test runs are conducted for the purpose of investigating problems. Other
purposes include:
• To define a base point for subsequent debottlenecking.
• To compare present performance with what might reasonably be expected from the
present packing or from more modern internals.

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Reference 5, attached to this section of the Manual as Appendix 500-A, contains guidance for
conducting a test run. See also References 1 and 2 and (for extensive detail) Reference 6.
Note the recommendation that all readily available data be taken, including redundant data and
data around column auxiliaries. Redundant data can be very useful in resolving problems in heat
and material balances and in supporting chosen values of primary variables. You can seldom
predict which redundant data will turn out to be important; take it all.

580 Analyzing Test Data


The usual procedure is:
1. Make a general inspection for "reasonableness".
2. Adjust the raw data to bring it into heat and material balance.
3. Make a computer model or simulation of the column for the purpose of determining internal
loadings and plate efficiency.
References 1, 2, 5, and 6 deal with this subject also.
581 Material Balance
If all stream rates have been measured, sum the product streams and compare to the feed stream
(or sum of feed streams). If the streams are mixtures of identifiable components, as contrasted
with heavier mixtures defined by analytical distillations (ASTM D 86, ASTM D 1160, etc.), make
this comparison for individual components also. In the author's experience (5), closure within 5%
is excellent; 3% is ideal (6).
582 Heat Balance
A variety of "envelopes" for heat balance are possible. See Figure 1 of Appendix 500-A. Closure
within 5% is ideal (6). Depending on the type of reboiler used, 10% may be more realistic. In
decreasing order of likely accuracy, here are the items which may need to be measured:
• Enthalpy of a single -phase process stream, including feed(s), products, reflux, stripping
steam, water drawoff, etc.
• Steam-heated reboiler duty.
• Water-cooled condenser or product-cooler duty.
• Fired reboiler or feed-preheater duty.
• Air-cooled exchange duty (yes, it has been done, using pitot tubes, temperature probes,
etc.)
Deriving the feed enthalpy from measurements, rather than overall column heat balance, is
recommended. It may affect estimation of optimum feed location, composition pinch zones, and
packing efficiency. If the feed is partially vaporized at the column entry, then its enthalpy will
preferably be determined at an upstream point where it is single phase, followed by adjustment
for any heating or cooling done in between. Measuring temperature and pressure at the feed entry
and then picking enthalpy off a vaporization curve is less accurate, particularly if the feed mixture
is narrow-boiling.

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583 Making the Computer Model


The usual procedure is as follows:
1. Fix pressures at reflux drum, column top, etc. according to measured values.
2. Convert any hydrocarbon mixture streams to pseudocomponents.
3. Sum the observed products to get the feed. This is usually done when it is judged that
measured rates and compositions of feed and products are equally reliable. In
multicomponent systems, it preserves product compositions; this facilitates estimation of
separation efficiency based on light key to heavy key ratio.
4. Fix (n-1) product rates (e.g., one product rate in a two-product column).
5. Fix reflux rate and temperature, reboiler duty, or whatever heat-balance variable is judged to
be most reliable. Fix thermal condition of the feed.
6. Assume an HETP (height of packing equivalent to a theoretical plate) and fix the number of
theoretical stages in each packed bed of the column.
7. Compute the remaining variables.
8. Compare the computed separation with the observed separation, revise HETP appropriately,
and repeat the previous two steps until a satisfactory match is found. See Appendix 500-A for
details of comparing computed to observed separation.
584 An Alternative Computer Model
The following alternative procedure may be useful in a case where the engineer has more
confidence in the feed stream description than in the products. Product key ratios (see Section
585) must be reliable, however.
1. As in step 1 of Section 583, fix pressures at reflux drum, column top, etc. according to
measured values.
2. As in step 2 of Section 583, convert any hydrocarbon mixture streams to pseudocomponents.
3. Fix the feed rate, composition, and enthalpy at the observed feed stream values.
4. Fix the reflux rate or one of its alternative variables.
5. Fix the condenser temperature if there are vapor and liquid distillate products or if reflux is
subcooled.
6. Assume values of total distillate and HETP. Fix the number of theoretical stages in each bed.
7. Compute the remaining variables.
8. Compare light key/heavy key ratios at top and bottom, revise both total distillate and HETP,
and repeat the previous two steps until satisfactory matches are found. Again, see Appendix
500-A for more details.
Once the column is modeled according to Section 583, it is little additional trouble to run the
alternative model. Unexpected insight may result.
585 Comparing Computed Separation With Test Data
Ideally, there will be only two distributing components in a simple two-product fractionator:
• The light key, which goes primarily to the distillate.
• The heavy key, which goes primarily to the bottoms.

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In that case, the procedure of Section 583 can result in computed product compositions very close
to the observed ones, limited only by needing to use whole numbers of theoretical stages.
More often, there are other distributing components; some lighter than the light key, some heavier
than the heavy key, some intermediate in volatility to the keys. (The chosen keys should be major
components of product streams and/or components whose concentrations must be controlled.) In
general, non-keys will not actually distribute in the same manner as the ideal stage calculation
predicts. This is the reason we compare on the basis of key ratios rather than product
compositions.
Comparison of computed temperatures with observed ones is helpful in assessing quality of data
or explaining anomalies, but temperature comparison should not be used, in preference to key
component separations, to determine packing efficie ncy. Temperature disagreements of 5-10F are
common.
Deriving packing efficiency for columns processing heavy hydrocarbon mixtures has so far met
with limited success. Reference 7 (Appendix 500-B) details a recent effort, including:
• The various analytical distillations that may be encountered.
• The problems of converting from one to another.
• The traditional measures of degree of separation. The conclusion, unfortunately, is that it
is very difficult to estimate separation efficiency of a heavy oil colu mn.
The simulated or gas chromatographic distillation, ASTM Test Method D 2887, is a very useful
procedure. For many purposes, it may be considered equivalent to a TBP (true boiling point)
distillation, the usual basis for generating pseudocomponents. However, the simulated distillation
(SD) of a given petroleum fraction usually has longer "tails" than the TBP, i.e., the SD
temperatures for 0%, 5%, and 10% distilled are lower than the corresponding TBP temperatures
and the SD temperatures for 90%, 95%, and 100% are higher. The length and shape of tails are
the indicators of separation efficiency.
In 1986, Pascagoula Refinery installed an improved liquid distributor above the wash-oil packed
bed of the Vacuum Distillation Unit. Quality and percent recovery of heavy gas oil improved, but
the increase of packing efficiency could not be quantified. This is the more typical experience.
586 Computing Packing Loading
If the purpose of the test run is simply to check column capacity, then a single computer
simulation run, using a reasonable value of HETP, will probably suffice. Simulation produces
internal stream rates and physical properties; these are used in standard packing capacity and
pressure-drop correlations. If vapor and liquid rates change as they pass through a design point
(stage), the higher pair of rates is usually used.
Remember that, in the ideal stage model used by the computer, internal traffic is computed by
heat and material balance on the basis of "passing" streams which are one theoretical stage apart.
As mentioned in Reference 5 (Appendix 500-A), the passing streams in a trayed column come
from points one actual tray apart. Where tray efficiency is particularly low and/or the column
temperature changes greatly from one theoretical stage to the next, it may be necessary to
recompute internal rates with temperatures adjusted to reflect actual stages.
A similar concern exists in packed columns. Internal streams approach temperature equilibrium
more rapidly than they approach mass-transfer equilibrium. Rather than coming from points one
theoretical stage apart, passing streams come from points which are, in the limit, only a
"differential" vertical distance apart. In areas of steep temperature gradient, the conservative
approach is to recompute internal liquid and vapor rates at critical loading points using the same

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temperature for the passing streams. For example: When modeled with an ideal stage computer
program, the stages numbered from the top down, conditions in the upper portion of a certain
fractionator are as shown in the following table. Stage 1 is the condenser; the internal liquid
stream from that stage, L1, is the reflux. The packed bed is represented by stages 2 and 3. V 2
leaves the top of the bed; V 4 enters at the bottom.

Stage Temperature, F Vapor Liquid Vapor Rate Liquid Rate


* Enthalpy Btu/Lb * Enthalpy Btu/Lb Lb/Hr Lb/Hr
1 118 --- 29 --- 330,400
2 270 245 112 519,100 403,100
3 342 275 153 591,800 454,300
4 379 291 177 643,000 ---
* The enthalpy datum is liquid at 60°F.

Let Vi = vapor rate from stage i, lb/hr.


Li = liquid rate from stage i, lb/hr.
hi = enthalpy of liquid stream from stage i, Btu/lb.
Hi = enthalpy of vapor stream from stage i, Btu/lb.
D = "delta mass", the net flow of material up the column, the difference between the mass
flow rates of passing streams in lb/hr. In this case, D is also the net distillate rate.
Q = "delta heat", the net flow of heat up the column, the difference between the total
enthalpies of passing streams in Btu/hr.
Two simple formulas are used:
For mass balance, D = Vi - Li-1.
For heat balance, Q = V iHi - Li-1 h i-1.
Combining and rearranging, Vi = (Q - D•hi-1)/(Hi - h i-1).
Passing streams in the above table are in mass and heat balance. D is 188,700 lb/hr. For example,
V2 - L1 = 519,100 - 330,400 = 188,700. Q is 117.6 MMBH. For example, V2H2 - L1h1 =
(519,100)(245) - (330,400)(29) = 117.6x106.
We now recompute traffic within the packed bed, assuming that each passing liquid stream is at
the same temperature as that of the vapor it passes. In this system, liquid enthalpy has little
composition dependence; therefore, we simply substitute hi for hi-1. For example, stream L2 is
now assumed to be at the same temperature as stream V 3, 342°F instead of 270°; h2 becomes
153 Btu/lb instead of 112 Btu/lb. V3 and L2 are recomputed.
V3 = (Q - D•h2)/(H3 - h2)

= [117.6x106 - (188,700)(153)]/[275 - 153]


= 727,300
L2 = V3 - D = 727,300 - 188,700 = 538,600

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Stage Temperature, F Vapor Enthalpy Liquid Enthalpy Vapor Rate Liquid Rate
Btu/Lb Btu/Lb Lb/Hr Lb/Hr
1 118 --- 29 --- 330,400
2 270 245 153 519,100 538,600
3 342 275 177 727,300 549,900
4 379 291 --- 738,600 ---

V2, remaining in balance with the reflux stream, does not change. L2 and V3, representing
loading at the top of the bed, increase markedly. At the bottom, the point of highest loading, the
vapor rate increases by about 15%. The bed is sized using L3 and V4.

590 References
1. Lieberman, N. P., "Troubleshooting Process Operations", 3d Ed., PennWell Books, Tulsa,
Oklahoma, 1991.
2. Kister, H. Z., "Distillation Operation", McGraw-Hill, New York, 1990.
3. McMullan, B. D., Ravicz, A. E., and Wei, S. J., "Trouble shooting a Packed Vacuum Column
-- A Success Story", Chemical Engineering Progress, July 1991, pp 69-74. (Please contact
A.G. Nelson of ERTC for a copy of this reference.)
4. Sorensen, R. C., "Pressure Control Methods for Distillation Columns", CRTC Internal
Report, January 10, 1990.
5. Ravicz, A. E., "Testing of Plant Scale Distillation Columns", CRC Internal Report, October
14, 1970.
6. "AICHE Equipment Testing Procedure, Packed Columns", 2d Ed., AIChE, New York, 1990.
7. Ravicz, A. E., "Performance Evaluation, RLOP HNC Vacuum Column C-1550", CRC
Internal Report, September 30, 1986.

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Appendix 500-A
Testing of Plant Scale Distillation Columns

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Appendix 500-B
Performance Evaluation RLOP HNC Vacuum Column

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Section 600 Packed Liquid/Liquid Extraction Guide
(by R.A. Wuopio and Gabriel Li)

610 Introduction
Liquid/liquid extraction provides one of the best methods to remove impurities from product
streams and to recover valuable products from process streams. ChevronTexaco uses packed
liquid/liquid extraction columns in amine treating of FCC C3 cuts as well as in MTBE and
TAME plants for recovery of methanol. The primary advantage of the packed column is that it
provides large mass-transfer area per unit volume.
Liquid/liquid extraction takes advantage of:
• the different solubility of the solute in both phases
• the density difference between the liquid phases to remove impurities from process
streams.
The two liquid phases are immiscible or partially miscible in this process while the solute is
soluble in both phases. Mass-transfer takes place either due to differences in solubility or due to a
concentration driving force arising from a chemical reaction in the solvent phase.
This process design guide is a tool for both evaluating the capacity of existing packed
liquid/liquid extraction columns as well as designing new columns.
The Norton correlations, the recently developed Seibert and Fair correlation, and two other
historical correlations are discussed in this report. Data from literature were used to evaluate each
model. The more commonly used Norton correlations were found to oversize many while
occasionally undersizing others. Because of the failure of the Norton correlations to accurately
predict flooding velocities, they should not be used for the design of new extraction columns. The
Siebert and Fair model, developed with a theoretical basis, was found to be superior and should
be used in designing new extractors. A Lotus 123 spreadsheet, LLFLOOD, containing the
Seibert and Fair model, has been created for your use in designing or rating a packed liquid/liquid
extraction column. This Packed Liquid Extraction Program is now available in the Engineering
Tool Kit section of Simsuite.
One of the key process parameters which affect the capacity of an extractor is the interfacial
tension. Because this property is difficult to measure in many cases, a model has been provided to
estimate it from stream composition and surface tension data.
A brief overview of the required column internals, such as packing support plates,
distributors/redistributors, bed limiters, and packing types, is also included to aid the engineer in
designing a new extractor.

620 Comparison of Flooding Models


The capacity of an extractor column is governed by a variety of parameters which include the
density difference between the liquid phases, the liquid viscosities, the interfacial tension, the
solvent wetting characteristics, the size and type of the packing, the solute transfer direction, and
the diameter of the column. The capacity of a column is exceeded when flooding or phase
inversion occurs, as follows:

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• Flooding results when the continuous phase flow is increased to the point where its
velocity meets or exceeds that of the dispersed phase. Under these conditions, the
dispersed phase holdup increases rapidly, and eventually the dispersed phase is forced out
the other end of the column.
• Phase inversion results when the dispersed phase flow is increased and the number of
droplets increases until this phase begins to fill the interstitial voids in the packing. This
usually takes place when the dispersed phase holdup becomes greater than 50% of the
void volume.
The Norton Models (9), the Seibert and Fair Model (13,14), the Dell and Pratt Model (8), and the
Hoffing and Lockhart Model (10) are presented here in this design guide. The latter two models
are comparable to the Norton Models, but have not been traditionally used by ChevronTexaco.
More information on these two models can be found in Appendix 600-A.
The Norton models were developed based on data in the absence of mass-transfer while the
Seibert and Fair Model takes into account mass-transfer effects, and therefore, is more reliable in
predicting flooding velocities for industrial systems.
In evaluating each of the models, flooding data from Ballard and Piret (4), Dell and Pratt,
Breckenfeld and Wilke (6), and Seibert and Fair were tested against each of the correlations. The
only flooding data for extractor systems with mass-transfer were obtained from Seibert and Fair
and from a single flooding data point for the Richmond FCC amine treater. Data from the other
three sources were acquired from experiments performed in the absence of mass -transfer. Tables
600-1 and 600-2 summarize the predicted flooding velocities and percentages for the four models
considered.
621 Norton Correlations (9, 11, 15)
The Norton Correlations, which have historically been used by ChevronTexaco to design
extractors, are modifications of the original Crawford and Wilke Correlation, displayed in Figure
600-1. The Crawford and Wilke model was based entirely on empirical findings and did not
account for solute transfer effects. When extractors based on this model failed to meet design
capacities, Norton realized that the lower interfacial tension resulting from mass-transfer caused
flooding at lower rates than anticipated. A large contingency for mass-transfer effects on flooding
was built into the Norton model. In their first model, Norton used different flooding limit curves
for different continuous phase flow (Vc) to dispersed phase flow (Vd) ratios to account for mass-
transfer effects. Figure 600-2 shows the flooding curves for this model.
This model was not successful in solving the problem because it now oversized many extractors,
but still occasionally undersized others. Figure 600-3 illustrates the failure of this model. As one
can see, the model grossly underpredicts the flooding velocities for all systems without mass-
transfer. This large discrepancy is attributed to the allowance that Norton adopted for mass-
transfer effects. This plot further reveals that even with this huge allowance the model still over
predicts flooding velocities for many of the systems with mass-transfer. In some cases, extractors
flooded at 50% of the Norton flooding limit. There are also other serious problems associated
with this model in predicting the proper trends. For example, this model erroneously predicts a
lower percentage of flooding with increasing Vc at constant V d.
At this point, Norton reverted to using the Crawford-Wilke correlation, but recommended that
extractors now be designed at 12% to 20% of flooding. A parity plot for this model (at 12% of
flooding) is shown in Figure 600-4. As one can see, this model seriously underpredicts the
flooding velocity for all systems. Using this model would result in the oversizing of extractors
and therefore a waste of capital.

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Both Norton models have significant drawbacks, and therefore, should not be used to design
extractors.
622 Seibert and Fair Correlation (13,14)
The Seibert and Fair Correlation was developed from a theoretical basis and is superior in many
ways to the Norton models. The authors built their model from first principles and included the
different effects of packing, mass-transfer direction, and drop-to-drop interactions in a stepwise
manner in arriving at a model for predicting flooding velocities. The results of their sequential
approach are several "intermediate" correlations for predicting drop diameters and dispersed
phase holdups. These "intermediate" models were tested and validated with experimental data to
lend credibility to the final flooding correlation. More information on this model can be found in
Section 1 of Appendix 600-B.
A parity plot for this model is shown in Figure 600-5. The model is more accurate in predicting
flooding for mass-transfer systems than the other three models. This model also correctly predicts
higher flooding percentages for systems with lower interfacial tension whereas the other
correlations incorrectly predict the opposite dependence on interfacial tension. The one weakness
in this model is that it tends to overpredict the flooding velocity at high continuous phase flow
with low dispersed phase velocities. An example of a flooding calculation using this model is
provided in Section 2 of Appendix 600-B.
623 Results and Discussion
The Seibert and Fair model is clearly the best of the models considered and we recommend it for
designing extractors. Extractors should generally be designed at 60% of flooding. This 60%
covers the scatter in the data and provides an allowance for impurities which may lower the
interfacial tension. The successful application of the model requires accurate data on the system
properties, such as the densities of the two phases and interfacial tension. For design purposes, the
density differences and the interfacial tensions should be determined for the system at the top and
bottom of the extractor. Use the lower of the two extreme values for calculating flooding
velocities. Be sure to include effects of the solute on the system properties, if they are known.
Pay special attention to systems with low interfacial tensions, such as butanol-water mixtures.
The flooding velocities for these systems are extremely sensitive to the interfacial tension. For
example, a decrease of 1 dyne/cm (which may be caused by impurities or even by the solute) for
a 4 dyne/cm system could increase the flooding percentage in a given column by as much as 30%.
Therefore, for such systems, accurate values for interfacial tension must be obtained for reliable
results. See Section 650 for more information on predicting interfacial tension.

630 Phase Separation Considerations


The above models only take into account flooding in the packed sections of the column. They do
not predict the required diameter for phase separation. This value is determined by the Stokes'
Law settling velocity; more information can be found on this subject in the Process Design
Guide for Liquid-Liquid Phase Separator Systems by R. A. Wuopio. In most cases, the
required diameter for flooding is greater than that for phase separation. However, it is always
better to check both to be sure, and to use the larger of the two values.

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640 Packed Liquid/Liquid Extraction Flooding Design and


Rating Program, "LLFLOOD"
As you can see by the example calculation in Appendix 600-A, the Seibert and Fair model
calculation is somewhat involved. To make it easier to use, we've incorporated it in a Lotus 123
spreadsheet, LLFLOOD (See Fig ure 600-6). The program can be used for design or rating of a
packed liquid/liquid extraction column.
The required inputs for this program are:
Vessel Diameter
Continuous and dispersed phase flow rates
Continuous phase viscosity
Continuous and dispersed phase densities
Interfacial tension
Packing unit surface area
Packing void fraction
Direction of mass-transfer
See Appendix C for information on estimating interfacial tension.
Packing parameters for some of the more common packings are provided in Table 600-3. Packing
types not included in the table may be obtained from the vendor.
The program will calculate the predicted continuous phase flooding velocity and the percent of
flooding. Note that the droplet sizes separated according to Stokes' Law for both phases are also
calculated. These values should be less than 100 microns for good phase separation.
Note: Contact Al Nelson ([email protected], 510 242-2562) for information
on the LLFLOOD program.

650 Interfacial Tension


One of the key parameters in determining the flooding velocity for a liquid/liquid extractor is the
interfacial tension between the two liquid phases. It is also one of the least understood. Although
it is related to the relative surface tensions of the two phases against air, interfacial tension is
largely determined by the molecular interaction between the two liquids. In particular, the
presence of oxygenated compounds in the two phases has a profound effect on the interfacial
tension. For example, the n-butanol/water system has an interfacial tension of 2 dynes/cm, even
though the surface tensions of the two liquids are 24 and 74 dynes/cm respectively.
The systems of immediate interest in ChevronTexaco refineries are:
• Caustic scrubbing of various hydrocarbon streams for removal of H2S and mercaptans;
• Water washing of hydrocarbon streams;
• Amine treating of FCC C3 cuts;
• Water scrubbing to remove methanol from MTBE and TAME.
Most of these systems have a total pressure higher than one atmosphere at room temperature,
making direct measurement of the interfacial tension difficult. Therefore, we have estimated their

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interfacial tensions based on laboratory data for similar systems whose interfacial tension can be
measured at atmospheric pressure. Based on these data, we have prepared Figure 600- 7 for
estimating interfacial tensions for evaluating the capacity of packed liquid/liquid extractors
running at 90-125°F.
For the methanol extraction column in MTBE and TAME plants, the experimental data showed
quite a bit of scatter. It was clear, however, that the presence of a significant amount of methanol
in the system reduced the interfacial tension by 30 to 40 dynes/cm compared to a hydrocarbon-
water system. For these columns, as well as for any other application, we recommend using the
general interfacial tension correlation which is included in Appendix 600-C. A sample calculation
for the methanol extraction column in the El Segundo TAME Plant is also included in Appendix
600-C.

660 Mass-Transfer Considerations


The mass-transfer rates of a system will determine the height of the column. These extractors are
usually overdesigned to ensure that the product specifications are met. The penalty for
undersizing the extractor usually far exceeds the capital cost of the extra packing. In cases where
no data exists, pilot plant studies should be performed to determine the equilibrium relationship
of the solute and the overall mass-transfer coefficient.

670 Extraction Column Internals


671 Packing Size
The packing size plays an important role in determining the average drop size within the column.
It would seem advantageous to use the smallest packing size available to obtain the smallest
droplets; however, there is a certain "critical size" of packing below which the packing voids are
so small that the droplets are locked in the interstices. Under these conditions, the droplets tend to
coalesce and have larger average diameters than ones formed in larger packings, The relationship
for determining this critical packing size diameter was originally developed (3) for Raschig rings
and Berl saddles but is commonly used for other packings as well. This minimum packing size,
calculated from Equation 1, is about 1/2 inch for most systems.
dcrit = 2.42 * {γ/(∆ρ*g)]
where γ is the surface tension, dynes/cm
∆ρ is the density difference between the two phases, g/cc
g is the gravitational constant, cm/s2
There is also a maximum packing size that should not be exceeded for a particular system. If too
large a packing size is used, channeling of the dispersed phase will occur, decreasing the mass-
transfer efficiency. To avoid this phenomenon, make the packing size less than 1/8 of the column
diameter.
The optimal packing size is a balance between capacity and efficiency. Smaller packing has a
higher efficiency but less capacity than larger packing. Commercial extractors typically use 1-
1/2" to 2" packing. Many plants have debottlenecked their columns by increasing the size of the
packing, provided the larger packing has the required mass-transfer efficiency.

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672 Packing Material and Wetting Characteristics


The selection of ceramic, plastic, or metal packing may affect the performance of the extractor.
The extractor is most efficient when the continuous phase preferentially wets the packing. In
situations where the dispersed phase wets the packing, thin films of this phase cover the surface
of the packing, resulting in a reduction of the interfacial area available for mass-transfer.
The wetting characteristics of materials differ greatly. Ceramic packings are wetted by aqueous
solvents, while plastics packings are wetted usually by organic solvents, although their wetting
characteristics can change over time, Metal packings are wetted by either aqueous or organic
solvents depending on the initial exposure of the metal surface.
Metal packings are most commonly used because of their ease of fabrication, light weight, and
high void fraction. Ceramic materials have high densities and may cause mechanical failures in
support plates. They also are brittle and tend to break into smaller pieces that plug the bed and/or
the heavy-phase pump suction. However, they are especially useful in corrosive systems.
673 Packing Shapes
The packing shape affects the droplet flow path and the resistance to flow. The development of
packing shapes remains an empirical art in which the pressure drop and the mass-transfer
efficiency of the bed must be determined experimentally. Both structured and random packings
can be used in liquid/liquid contractors. Structured packing is more effective in providing even
liquid distribution in large columns (I.D. >3 ft), but is more expensive than random packing.
Random packing with redistributors, spaced 9 to 12 ft apart, is commonly used in industrial
extractors.
Various packing shapes have been developed over the years. A partial list of the available types
and sizes are provided along with the associated surface area and void fraction data in Table 600-
3. When making a selection on the type of packin g to be used, refer to vendors for advice on the
most appropriate one for your system.
674 Vessel Outline Drawings
Typical vessel outline drawings for both the light-phase-dispersed and heavy-phase-dispersed
cases are provided in Figure 600-8 and 600-9 for your information. (In general, it is advantageous
to have the process stream as the dispersed phase to maximize the interfacial mass-transfer area.)
The discussion of column internals below uses Norton internals as examples. Equivalent internals
are also available from other vendors, such as Glitsch and Koch.
675 Packing Support Plates
The most common manner of operating an extractor is to have the light phase dispersed with the
interface maintained above the packed bed. Under these conditions, the packing support plate and
the disperser plate are usually designed as a single plate. The reason for this is that a separate
support plate tends to adversely disrupt the light-phase dispersion rising through it. In the single
plate design, the light phase enters below this plate and flows through the orifices on the top
surface of the plate into the packed bed. The heavy phase flows through the downcomers of the
plate, past the entering pool of light-phase liquid, and finally out of the column. A sample
drawing and description of a dispersion/support plate taken from the Norton Standard Internals
Catalogue is shown in Figure v10.
The specifications of a disperser/support plate include the number, location, and size of the
orifices as well as other mechanical considerations. Limit the velocity of the dispersed phase
through these orifices to 70 ft/min to avoid forming emulsions. The most common orifice sizes

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are 0.19 and 0.25 inches in diameter, although 0.14 and 0.31 inch orifices have also been utilized.
This plate is available from Norton (Model 834) for towers with diameters greater than 1 foot.
In the case where the heavy phase is dispersed, the design of column internals will differ slightly
from that of the light-phase-dispersed case. Conventional support plates shown in Figure 600-11
are used to support the packing with a separate disperser plate now located at the top of the
column. The design of this disperser plate is much like that shown in Figure 600-10 with some
minor modifications. This plate, however, is installed in an inverted position situated 10 to 12
inches above the top of the packed bed.
676 Distributors
The distributor of the continuous phase is similar to the one shown in Figure 600- 12. Norton
offers both plastic (Model 1944) and metal (Model 844) distributors. We recommend sizing the
orifices to provide a low entrance velocity of less than 170 ft/min to minimize the disturbance of
the dispersed phase rising through it. The dispersed phase distributor is similar, but has risers
extending almost to the disperser/support plate, which prevent the dispersed phase fluid from
interfering with the continuous phase exiting through the plate downcomers.
677 Redistributors

Redistributors are very important for columns with random packing. Space them 9 to 12 ft. apart
for best results. if no redistributors are used, maldistribution of liquid will occur, causing a loss in
mass-transfer efficiency. For light-phase-dispersed flow, the disperser/support plate design can
also be used for redistribution plates within the column. For heavy-phase-dispersed flow, an
individual redistribution plate is placed between the bed limiter and the support plate. This plate
is similar to the disperser/support plate except that it is installed in an inverted position.
678 Bed Limiters
A bed limiter is placed above each packed section to prevent expansion of the bed and to
maintain an even top level. The bed limiter, usually made from plastic or lightweight metal, is
held down either by the column internal located immediately above it or by clips which fasten it
to the column wall. A drawing of a bed limiter is provided in Figure 600-13. Norton supplies two
models of metal limiters (Model 824 and 823) with different size limitations and one model of
plastic bed limiter (Model 1868).
679 Coalescing Pads
Coalescing pads are sometimes needed to obtain good phase separation for systems with low
interfacial tension and/or high viscosity. These pads should consist of fibers which are
preferentially wetted by the phase to be separated to help coalesce the droplets. They can help
reduce carryover to the other phase, but use them with caution if there is a potential plugging
problem.

680 References
1. AICHE Data Prediction Manual, Surface Tensions, Chapter 7, 1986
2. API Data Book, Surface and Interfacial Tension, Chapter 10, 3rd Edition, 1976
3. Bailes, P.J.; Hanson, C.; Slater, M.J., The Design of Randomly-Packed Columns with
Uniform Packing for Liquid-Liquid Extraction, University of Bradford, School of
Chemical Engineering, 1977
4. Ballard, J.H.; Piret, E.L., Ind. & Eng. Chem., 42(6), 1088 (1950)

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5. Blanding, F.H.; Elgin, J.C., Trans. Am. Inst. Chem. Eng., 38, 305 (1942)
6. Breckenfeld, R.R.; Wilke, C.R., Chem Eng. Prog., 46, 187 (1950)
7. Crawford, J.W.; Wilke, C.R., Chem Eng. Prog., 47(8), 423 (1951)
8. Dell, F.R.; Pratt, H.R.C., Trans. Inst. Chem. Eng., 29, 89 (1951)
9. Eckert, J.S., Hydrocarbon Proc., 117, March 1976
10. Hoffing, E.H.; Lockhart, F.J. Chem Eng Prog, 50 , 94 (1954)
11. Neumanitis, R.R; Eckert, J.S.; Foote, E.H.; Rollison, L.R., Chem. Eng. Prog., 67 (11), 60
(1971)
12. Norton Chemical Process Products, Standard Tower Internals Catalogue
13. Seibert, A.F.; Fair, J.R. Ind. Eng. Chem. Res., 27, 470 (1988)
14. Seibert, A.F.; Reeves, B. E,; Fair, J.R., Ind. Eng. Chem. Res., 29, 1901 (1990)
15. Strigle, R.E., Random Packing and Packed Towers , Gulf Publishing Company, Houston,,
p. 240 (1987)
16. Wuopio, R.A.; Process Design Guide for Liquid-Liquid Phase Separator Systems

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Tables and Figures

Figure 600-1 Crawford – Wilke Correlation

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[
Figure 600-2 Norton Correlation with Vc/Vd Flooding Curves

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Figure 600-3 Parity Plot for the Norton Correlation with Vc/Vd Curves

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Figure 600-4 Parity Plot for the Norton (12% of Flood) Correlation

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Figure 600-5 Parity Plot for the Seibert and Fair Correlation

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Figure 600-6 Sample Output from LLFLOOD

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Figure 600-7 Interfacial Tension of Hydrocarbon – Water Systems

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Figure 600-8 Vessel Outline Drawing for Light Phase Dispersed

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Figure 600-9 Vessel Outline Drawing for Heavy Phase Dispersed

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Figure 600-10 Disperser Support Plate

Figure 600-11 Conventional Support Plate

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Figure 600-12 Distributor

Figure 600-13 Bed Limiter

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Appendix 600-A Other Flooding Models


1 ) Dell and Pratt Correlation (8)
The form of the Dell and Pratt Model, shown in Figure 600-A1, is based on Bernoulli balances of the
solvent and aqueous phases. This model was developed based on systems without mass-transfer, and
therefore possesses some of the same drawbacks as the Norton model. Figure 600-A2 shows the parity
plot for this model and reveals that this model overpredicts flooding limits for nearly all systems with mass-
transfer.
2) Hoffing and Lockhart Correlation (10)
The Hoffing and Lockhart Correlation is represented by the curve in Figure 600-A3. This correlation is
based totally on empirical observations of systems without mass-transfer. The parity plot on Figure A4
indicates the severe limitations of this model in systems with mass-transfer.

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Figure 600-A1 Dell and Pratt Correlation

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Figure 600-A2 Parity Plot for the Dell and Pratt Correlation

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Figure 600-A3 Hoffing and Lockhart Correlation

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Figure 600-A4 Parity Plot for the Hoffing and Lockhart Correlation

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Appendix 600-B More Information on the Seibert and Fair Model


1) Development of the Seibert and Fair Model
The first step in the development of the Seibert and Fair model was to determine the average drop size for
mixtures and process conditions within the extractor. The authors discovered that the drop diameters were
markedly affected by the mass-transfer direction. They observed that drop diameters were larger for
systems with mass-transfer from the dispersed phase to the continuous phase (d->c) than for systems with
mass-transfer in the reverse direction (c-> d) or with no mass-transfer at all. This effect may be attributed
to the differences in interfacial tensions arising from solute transfer. The drop-size correlation, shown in
Equation A1, includes a correction factor, η, which accounted for this mass-transfer direction dependence.
Predicted values compared favorably with data with a standard deviation of less than 10%.
(A1)
dvs = 1.15*η*[γ/(∆ρ*g)]
where dvs is the Sauter drop diameter, cm

η is the drop correction factor


= 1 for (c->d) or no mass transfer
= 1.4 for (d->c)
The next step in developing the model is to account for drop hydraulics. The authors began by performing
a force balance on the drop, and proceeded to build in the drop interaction function, the tortuosity factor,
and the packing correction function to the basic force equation. The result is Equation A2, a correlation for
the dispersed phase holdup. Note that this must be solved iteratively.
(A2)

φ d = [Vd*cos -2(πξ/4)]/{ε*Uso*exp(-1.92*φ d)-[Vc/(1-φ d)]}

where ξ is the tortuosity factor


φ d is the dispersed phase holdup
Uso is the characteristic slip velocity, cm/s
NOTE: Equation A2 is reproduced as shown in the original reference. The notation is unusual. In
-2 -2
general, “cos (x)” means “(cos x) .”
Equation A2 was tested against experimental data and fared well with a standard deviation of 12%. From
this equation, the authors finally arrived at a correlation for flooding by assuming that at flooding the
dispersed-phase holdup fraction is equal to the value of π/6. This is the theoretical maximum holdup for a
cubic arrangement of spherical droplets. Based on this assumption, Equation A3 was developed to predict
continuous-phase flooding velocities. The percentage of flooding is found by dividing the actual continuous-
phase velocity by the predicted continuous-phase flooding velocity.
(A3)

1/Vcf = 5.63/(ε*Uso)*{1+0.925(Vdf/Vcf)*[cos -2(πξ/4)]}

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where Vdf is the dispersed-phase velocity at flooding, cm/s


Vcf is the continuous-phase velocity at flooding, cm/s

2) Example Flooding Calculation


A methanol-rich C4 hydrocarbon stream in the MTBE plant is to be extracted with water. The dispersed
phase will be the hydrocarbon stream and the continuous phase will be the water phase. The column has a
diameter of 6 feet and uses 1.5 inch Hy-pak packing from Norton. The example will calculate the
operating flooding percentage of the column with the Seibert and Fair model.
The following data are provided for this problem.

C4 Feed rate: 2561 ft3/hr

Water Rate: 205 ft3/hr


Mass-transfer direction: dispersed to continuous

Packing void fraction: 0.972 ft3/ft3

Packing superficial area: 36 ft2/ft3


Continuous-phase viscosity 0.62 cp
Dispersed phase viscosity: 0.14 cp

Continuous phase density 61.7 lb/ft3

Dispersed phase density 35.1 lb/ft3


Continuous phase surface tension: 71.4 dynes/cm
Interfacial tension: 15 dynes/cm
1) Find the Sauter Drop Diameter, dvs, in cm.

dvs = 1.15*η*[γ/(∆ρ*g)]0.5

where η is the drop correction factor


= 1 for (c->d) or no mass transfer
= 1.4 for (d->c)

dvs = 1.15*1.4*{15/[(61.7-35.1)/62.43*980]}0.5
dvs = 0.305 cm
2) Determine the characteristic slip velocity, Uso, in cm/s

P = (ρc2*γ3)/(µc4*g*∆ρ)

H = [(4*dvs2*g*∆ρ)/(3*γ)]*[µw/µc]0.14*P 0.149

Re/P 0.149 = 0.94*H 0.757 - 0.857, H≤59.3

Re/P 0.149 = 3.42*H 0.441 - 0.857, H>59.3

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Uso = (Re*µc)/(dvs*ρ c)
where Re is the drop Reynolds number

µw is the liquid viscosity of water, cp

µc is the liquid viscosity of the continuous phase, cp


P, H are dummy variables used to break the calculations into several equations

P = {(61.7/62.43) 2*153}/{(0.62/100) 4*980*(61.7-35.1)/62.43} = 5.34 e+ 9

H = [{4*0.4982*980(61.7-35.1)/62.43}

/(3*15)]*[0.009/(0.62/100)]0.14

*(1.013 e + 11) 0.149 = 272.5 > 59.3

Re = (3.42*272.50.441 - 0.857)*(5.34 e+9) 0.149 = 1093


Uso = {1093*(0.62/100)}/{0.498*(61.7/62.43)} = 13.8 cm/s

3) Calculate the tortuosity factor, ξ.


ξ = a*dvs/2

ξ = 36*0.498/(2*30.58) = 0.293
4) Calculate the continuous phase flooding velocity, Vcf in cm/s

1/Vcf = 5.63/(ε∗Uso)*{1+0.925(Vdf/Vcf)*[cos-2(πξ/4]}
where Vdf/Vcf is the ratio of dispersed flow to continuous flow
Vcf = 1/{5.63/(0.972*13.8)*{1+0.925*(2561/205)

*[cos -2(3.14*0.293/4)]}}
Vcf = 0.181 cm/s
5) Calculate the flooding percentage, Flood %.
Flood% = (Vc operating /Vcf)* 100%
Flood% = (205*30.58/(3.14*3*3*3600)/0.181}*100% = 34%

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Appendix 600-C Prediction of Interfacial Tension


1) Hydrocarbon-Water Systems
A simple correlation for predicting interfacial tension of paraffin-water systems is presented in the API
Technical Data Book:
0.5
γHW = σH +σW -1.10 (σH σW)
where γHW = Interfacial tension, dynes/cm
σH = Surface tension of hydrocarbon, dynes/cm

σW = Surface tension of water, dynes/cm


This correlation is limited to saturated hydrocarbons containing 5 or more carbon atoms. It doesn't work
well for aromatics. Do not use this equation for non-hydrocarbon systems, particularly those in which the
organic phase contains oxygenated compounds. The oxygen in the organic phase in contact with an
aqueous phase has a strong effect on the interfacial tension. For such systems, use the more general
correlation below.
2) General Correlation
To develop a general correlation to predict interfacial tension when no data exists, we collected all the data
we could find in the literature plus some data generated at ERTC and analyzed it using multiple regression.
The correlation is based on the surface tension relationship used in the API correlation, plus factors to
account for the difference in chemical structure between the two liquid phases. This relationship should be
used only if labratory data are not available for the system in question.
The correlation is as follows:
0.5
ln γ = 7.202 + 0.040 {σA + σB-1.10( σA σB} - 6.35Cwat - 13.66Calc
-6.77Cald - 10.72Cket - 3.99Cest - 8.23Cacid - 5.21Ceth
-17.22Camin - 5.590CNoth + 0.29CC - 0.34Colef - 8.97CNa

where γ = Interfacial tension, dynes/cm

σA and σB = Surface tension of the two phases, dynes/cm and the following terms are the absolute
difference between concentrations of the chemical constituents in the two phases, wt%
Cwat = Oxygen in H-OH (water)
Calc = Oxygen in R-OH (alcohol)
Cald = Oxygen in H-C=O (aldehyde)
Cket = Oxygen in R-C=O (ketone)
Cest = Oxygen in R-COOR (ester)
Cacid = Oxygen in R-COOH (acid)

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Ceth = Oxygen in R-O-R (ether)


Camin = Nitrogen in NH or NH2 (amine)
CNoth = Nitrogen in any other form
CC = Carbon
Colef = Ratio of olefinic bonds to total carbon-carbon bonds
CNa = Sodium or other cation
If the compound being extracted is present in concentrations of more than 1% of the total system, it should
be included in the composition of one of the phases.
Example: Calculate the interfacial tension of the nitrobenzene (C6H5NO2)-water system at 20°C.
MWA = 123.1

σΑ = 43.8 dynes/cm
σΒ = 72.9 dynes/cm
Cwat = 16/18.0 - 0 = 0.889
CNoth = 14/123.1 - 0 = 0.114
Colef = 3/5 - 0 = 0.600
CC = 6*12.0/123.1 - 0 = 0.585
(Oxygen in organic NO2 form is not a significant contributor to interfacial tension)

ln γ = 7.202 + 0.040 {43.8 + 72.9 - 1.10((43.8)(72.9))0.5


- (6.35)(0.889)-(5.59)(0.114)-(0.34)(0.600) + (0.29)(0.585)}
γ = 21.6 dynes/cm (actual = 24.0 dynes/cm)
Example: Calculate the interfacial tension of the n-pentane-20% DEA ((HOCH2CH2)2NH) systen at
23°C.
MWnC5 = 72.1
MWDEA = 105.1

σΑ = 15.7 dynes/cm
σB = 62.1 dynes/cm
Cwat = 0.8(16/18.0) - 0 = 0.711
Calc = (0.2)(2)(16)/105.1 - 0 = 0.0609
Camin = (0.2)(14)/105.1 - 0 = 0.0266
CC = (5)(12.0)/72.1 - (0.2)(4)(12.0)/105.1 = 0.741

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ln γ = 7.202 + 0.040 {15.7 + 62.1 - 1.10((15.7)(62.1))0.5


- (6.35)(0.711) - (13.66)(0.0609) - (17.22)(0.0266)
+ (0.29)(0.741)}
γ = 28.6 dynes/cm (actual = 26.5 dynes/cm)
Example: Calculate the interfacial tension for the methanol extraction column in the El Segundo TAME
Plant. The column uses water to extract methanol from the following hydrocarbon feed at 100°F.
σ, dynes/cm

Wt% Mol% (Figure 600-C2)


Butanes 1.5 1.6 9.5
2-Methyl 1-butene 1.6 1.8 14.5
2-Methyl 2-butene 2.9 3.1 15.8
Pentanes 81.4 69.3 14.0
Methanol 12.6 24.2 21.1
100.0 100.0 15.7 (molar avg)

MWA = 61.4

σA = 15.7 dynes/cm
σB = 70.2 dynes/cm
Cwat = 16/18.0 - 0 = 0.889
Calc = (0.126)(16/32.0) - 0 = 0.0630
CC = (0.015)(4)(12.0)/58.1 + (0.016 + 0.029)(5)(12.0)/70.1 + (0.814)(5)(12.0)/72.1 +
(0.126)(1)(12.0)/32.0 - 0 = 0.776
Colef = (0.016 + 0.029)(1)/4 = 0.011

ln γ = 7.202 + 0.040 {15.7 + 70.2 - 1.10((15.7)(70.2))0.5


- (6.35)(0.889) - (13.66)(0.0630) + (0.29(0.776)}

γ = 18.1 dynes/cm

The data included in the interfacial tension correlation are shown in Table 600-C1. The multiple regression
coefficient , R2, is 0.95 for this correlation. The standard error of the interfacial tension predicted by the
correlation for the data used in its development is 1.2 dynes/cm, corresponding to an average error of 16%
(See Figure 600-C1).
Figures 600-C2 – 600-C5 contain data on surface tensions of hydrocarbons and aqueous solutions which
can be used with this correlation. Surface tensions of mixtures can be estimated by blending the surface
tensions of the components on a molar basis.

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Figure 600-C1 Parity Plot for the General Interfacial Tension Correlation

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Packed Column Technology 600 Packed Liquid/Liquid Extraction Guide

Figure 600 C2

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Packed Column Technology 600 Packed Liquid/Liquid Extraction Guide

Figure 600 C3

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Packed Column Technology 600 Packed Liquid/Liquid Extraction Guide

Figure 600 C4

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Packed Column Technology 600 Packed Liquid/Liquid Extraction Guide

Figure 600 C5 Surface Tension of Water and Aqueous Solutions

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