PROCESS

DISTILLATION

TRAINING MANUAL
COURSE EXP-PR-PR180
Revision 0.1
 Exploration and Production
Process
Distillation

PROCESSING

DISTILLATION

CONTENTS

1. OBJECTIVES ..................................................................................................................5
2. INTRODUCTION TO DISTILLATION PRINCIPLES ........................................................6
2.1. ...................................................................................................................................6
3. DISTILLATION PROCESS ..............................................................................................7
3.1. VOLATILITY..............................................................................................................7
3.2. HEAT TRANSFER AND MATERIAL TRANSFER.....................................................8
3.2.1. Material Balance (Bilan matière).........................................................................8
3.2.2. Heat Balance ......................................................................................................8
3.3. REBOILING.............................................................................................................10
3.4. INTERNAL REFLUX & EXTERNAL REFLUX .........................................................10
3.5. DESCRIPTION OF THE DISTILLATION PROCESS ..............................................11
4. TYPES DE DISTILLATIONS..........................................................................................14
4.1. UNSTEADY STATE DISTILLATION .......................................................................14
4.2. STEADY STATE DISTILLATION ............................................................................15
4.3. MULTIPLE STILLS DISTILLATION.........................................................................16
5. STRIPPING ...................................................................................................................19
5.1. DETAILED DESCRIPTION OF A STILL SECTION.................................................20
6. FRACTIONATION..........................................................................................................24
6.1. EXERCICES ...........................................................................................................27
7. DISTILLATION TECHNOLOGIES .................................................................................29
7.1. TRAYED COLUMNS...............................................................................................29
7.1.1. Bubble Cap Tray)..............................................................................................29
7.1.2. Down-comers....................................................................................................30
7.1.3. Weirs ................................................................................................................31
7.1.4. Tray Types........................................................................................................32
7.1.5. Sieve Deck........................................................................................................32
7.1.6. S-Section ..........................................................................................................32
7.1.7. Glitsch (Ballast) Tray ........................................................................................33
7.1.8. Side-to-Side Pan...............................................................................................33
7.2. PACKED TOWERS.................................................................................................34
7.2.1. Berl Saddle .......................................................................................................34
7.2.2. Raschig Ring ....................................................................................................34
7.2.3. Limits of satisfactory packing operation for a specific set of packing fluid
properties....................................................................................................................35
7.2.3.1. Liquid entrainment – flooding .....................................................................35
7.2.3.2. Liquid distribution .......................................................................................35
7.3. COMPARISON BETWEEN TRAYED AND PACKED COLUMNS...........................36
7.3.1. Advantages and drawbacks of trays and packing.............................................36
7.3.2. Choice criterions for trayed and packed columns .............................................37
7.4. EXERCISES............................................................................................................38
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8. AUXILIARY EQUIPMENT..............................................................................................39
8.1. REBOILERS............................................................................................................39
8.2. CONDENSERS .......................................................................................................40
8.3. STRAINERS............................................................................................................42
8.4. REFLUX DISTRIBUTORS ......................................................................................42
8.5. DEMISTERS ...........................................................................................................43
8.6. EXERCISES............................................................................................................44
9. OPERATING PARAMETERS ........................................................................................45
9.1. DÉFINITIONS OF OTHER GENERAL BASIC PARAMETERS...............................45
9.1.1. Temperature Gradient: .....................................................................................45
9.1.2. Initial Boiling Point ............................................................................................46
9.1.3. Distillation End Point.........................................................................................46
9.1.4. Interpretation of a Dew point and Bubble Point curve.......................................46
9.2. MAIN PARAMETER CONTROL LOOPS ................................................................48
9.2.1. Tower-bottom temperature control loop............................................................48
9.2.2. Pressure control in a distillation column............................................................49
9.2.3. Bottom liquid level control in a distillation column .............................................50
9.2.4. Differential Pressure .........................................................................................51
9.2.5. Flow control loop at the inlet of a distillation column .........................................51
9.2.6. Process Safety on a Distillation Column ...........................................................52
9.2.7. Control system for the main parameters of a standard column.........................53
10. OPERATING A DISTILLATION COLUMN...................................................................54
10.1. OPERATING A STANDARD COLUMN.................................................................54
10.1.1. Pressure .........................................................................................................54
10.1.2. Temperature ...................................................................................................54
10.1.3. Flowrates ........................................................................................................56
10.1.4. Levels .............................................................................................................56
10.1.5. The lateral cut-extraction levels ......................................................................57
10.1.6. Analysers ........................................................................................................57
11. PERFORMING DISTILLATION ...................................................................................58
11.1. STARTING UP A DISTILLATION COLUMN .........................................................58
11.1.1. Preparing the utilities ready for column start-up..............................................58
11.1.1.1. Circuits Preparation..................................................................................58
11.1.1.2. Filling........................................................................................................59
11.1.1.3. Verification - Activation.............................................................................59
11.1.1.4. Temperature stage...................................................................................60
11.1.2. Following step:................................................................................................60
11.1.2.1. Process Conditions ..................................................................................60
11.1.2.2. Raising Temperature................................................................................61
11.1.2.3. Production Conditions ..............................................................................61
11.2. STOPPING A DISTILLATION TOWER .................................................................62
11.3. PREPARING A COLUMN FOR INTERVENTIONS...............................................64
12. TROUBLESHOOTING.................................................................................................66
12.1. REFLUX TEMPERATURE DECREASE. ..............................................................66
12.2. INTERACTION OF OTHER PROCESS VARIABLES ...........................................66
12.3. LOSS OF HEAT ....................................................................................................67
12.4. LOW LOW LEVEL (LSLL) AT REFLUX DRUM.....................................................67
12.5. LOSS OF COOLING WATER ...............................................................................68

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13. GLOSSARY .................................................................................................................69

14. SUMMARY OF FIGURES............................................................................................72
15. CORRECTIONS FOR EXERCICES ............................................................................73

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1. OBJECTIVES
At the end of this module, the training participant must be able to:

Identify the structure and describe the function of the distillation column.

Understand the process of fractionation

Describe the operation of multiple still distillations.

Know the operating parameters

Identify the process of unsteady and steady state distillation

Know the main troubles that can occur in operating a distillation column

NB:
Before starting reading this module it is advised to review one’s knowledge
concerning another module called: Hydrocarbons behaviour

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2. INTRODUCTION TO DISTILLATION PRINCIPLES

2.1.
To obtain cuts of different types of components for use in different applications (e.g. Cuts
of Gas-Oil) or of individual components (e.g. separate cuts of Propane and Butane) the Oil
& Gas industry had develop, very early on, a process altogether different from separation,
which separates only the different liquid and gas phases from each other, at set P,T
conditions.

This process is called DISTILLATION, and its derived form, FRACTIONATION. The first,
the DISTILLATION, separates fluids by type called ‘cuts’ (e.g. cuts of Gas-Oils are first
distilled, then cuts of Kerosenes, then cuts of Gasolines) whereas the second,
FRACTIONATION, separates them by component which are the bases of end products
(e.g. Heavy Gas-Oils are fractionated from Light Gas-Oils, Heavy Gasolines are
fractionated from light Gasolines).

Obviously, the two operations are conducted in different columns in a series, starting with
a first column that performs Atmospheric Distillation (because it usually distils at pressures
of less than 3 Barg). The term most often used for this is the word “Topping”.

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3. DISTILLATION PROCESS
Prior to study the distillation Process within a column, it would be useful to introduce some
general parameters and/or terms used in the drive of a distillation tower. It will be the
‘Volatility’, the ‘Material Balance’ and the ‘Heat Balance’.

3.1. VOLATILITY

Volatility is one of the particular properties of fluids allowing the existence au Distillation
Process
How it works? A simple demonstration reveals it hereafter:

In one hand, have few drops of water and in the over hand get some droplets of alcohol. In
this situation, the two fluids are at same pressure (P0) and at skin temperature (about
36°C°. Skin, being the heating source, what is going on?
After a short time, the alcohol droplets have disappeared, evaporated while in the other
hand, water is still there.

The difference comes from the ‘manifestation’ of a physical property during this
vaporisation; it is the “Volatility of fluids” which appears between different fluids at different
temperatures for a given pressure.

The more the substance is volatile, the lower the temperature of vaporisation is. In the
given example, the alcohol vaporise at 78°c at atmospheric pressure when water does it at
100°C.

Temperature of vaporisation depends only upon pressure; consequently, there is a

vaporisation temperature different for each pressure different.

An other parameter, closed to volatility, being in fact the consequence, is the Vapour
Pressure (VP), term seen in thermodynamic course. VP is a characteristic for a fluid in
equilibrium Liquid/Vapour at a given temperature, at a well defined pressure. This VP
increases with temperature; it is (naturally) the more volatile substance which has the
higher VP.

In the "Oil & Gas" industry the crude oil and other distillation feeds are actually a mixture of
several different compounds, thus with a different volatility & therefore. They have different
boiling points.
So, the mixture does not have a single boiling point, but rather a boiling range.

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3.2. HEAT TRANSFER AND MATERIAL TRANSFER

Roughly speaking, knowing what enters the column and what we want out, how to proceed
to finalise the expected result? It is the function of the thermal account: the energy to bring
into the system/process to obtain the desired components in quality and quantity.

3.2.1. Material Balance (Bilan matière)

When the tower is functioning normally, all material that enters the tower leaves the tower.
In other words, all the material that enters as feed leaves as product.

This means the input of material to the tower equals the output of material from the tower.
This balance of material is an application of the principle of conservation where input
always equals output.

If the amount of feed is increased, the total amount of product increases;

Any component in the feed is also subject to the principle of conservation of material.

For example, a feed containing 25 pounds of pentane must separate into products that
also contain a total of 25 pounds of pentane.

This means that for each 1,000 pounds of feed with a weight ratio of 25% pentane, 250
pounds of pentane enter the tower and 250 pounds of pentane must leave the tower.

If a feed contains a given amount of pentane and 80% of it is removed as overhead

product, then 20%.must be removed in the bottom product.

This by heating the mixture of different components to the boiling point of the lightest
compound in the mixture, but not quite to the boiling point of the heavier compounds.

3.2.2. Heat Balance

Energy put into the tower is also subject to the principle of conservation.

Energy is put into the tower in the form of heat. So, energy balance is heat balance, and
heat into a tower must equal heat out of the tower.

There are two different forms of heat:

Sensible Heat: is the heat added to raise the temperature of a substance.

o So, the heat added to raise the temperature of water from 150º F (66°C)to
160º F ( 71°C ) is sensible heat.

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Latent Heat: is the heat added to change the phase of a substance, without
increasing the temperature. 30 (Eg: 100°C for H20 valid for a pure component
only )

Another source of heat to the column is the feed which is preheated through a battery of
exchangers and heated through a furnace to reach the calculated temperature at the
column inlet.

There are also sources of heat loss:

One way to remove heat from the column is by transferring heat to the cooling
water in the condenser.

Another source of heat loss is through the removal of top and bottom product.

Controlling the amount of heat entering and leaving the column is known as controlling the
heat balance of the column.
If the temperature of the feed to a column increases from 550º F (288°C) to 600º F
(315°C), the amount of heat brought into the column increases

Because more of the heavier compounds vaporize and begin moving up the column, the
portion of heavier components leaving the column as overhead product increases.

If more of the heavier components leave in the overhead product, the overhead product
becomes heavier.

These heavier components are the lightest components in the bottom liquid.
If the lightest components in the bottom liquid leave, the bottom product becomes heavier
and both products can go off-specification.

To keep producing products that are on-specification, the extra heat coming into the
column must be removed.

On the multiple compound extractions columns there is a very useful way to remove
excess heat off a column it is to withdraw one part of liquid at a determined level of the
column, pump it out towards an exchanger for heating a fluid circulating through the other
part of the exchanger and then return this liquid back to the column at a higher level,
because the liquid has lost heat in the heated exchanger thus its temperature has
decreased.

This option is called "Pump-Around"

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Figure 1 : Sketch of thermal account principle

3.3. REBOILING

Heat must be applied to the material that has entered the distillation column to vaporise
the lighter components in the feed. Otherwise there will not have the dynamic of the
distillation process i.e. the raising stream of vaporized components & the down flow stream
of the condensing components

Some of these vapours make it to the top of the column and are piped into the condenser
where heat is removed.
One way how heat is added to the column is by increasing steam flow to the reboiler.
That maintains the necessary temperature in the column bottom, to keep the system
working

3.4. INTERNAL REFLUX & EXTERNAL REFLUX

The vapours leaving the column at the top are partially condensed through an Air cooler
exchanger or a water cooled Exchanger the double phase Liquid / Vapor is recovered in a
drum called Reflux Drum, one part of the liquid is pumped back to the column top tray as
External Reflux
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This cooled liquid removes heat from the rising vapours. The reflux condenses the heavier
fractions on the top tray, so they flow through the down-comer onto the tray below. At each
tray, the reflux is provided by the cooler liquid from the tray above.

The operation carried on in the column is a two-way process.

A stream of vapours rises upward and a stream of liquid flows downward.

The liquid flowing down to lower trays is called Internal Reflux.

The Reflux flowing down and vapour rising up to each tray controls the temperature of the
liquid on that tray.

At the temperature on each tray, some of the liquid vaporises and some of the vapours
condense. The working of a fractionating tower depends on the constant process of
vaporizing and condensing.

This necessary vaporizing and condensing is constantly maintained throughout the

fractionating tower by the difference in temperature between the reflux that is flowing
downward and the rising vapours.

3.5. DESCRIPTION OF THE DISTILLATION PROCESS

As already stated, the temperature in a distillation column gradually decreases from

bottom to top.

The diagram Distillation unit for crudes (Topping), in this paragraph illustrates this
description. It represents a conventional Topping column with different cuts extraction
stages A, B, C, D & E from bottom to top, during the distillation process.

The Raw crude usually passes through this type of column for initial processing at the
refinery.

Heat for the crude oil feed is furnished by a series of heat exchangers and a furnace.

The heated crude is fed into the flash zone. The crude oil enters the column in a vigorously
boiling and evaporating state.

To handle this turbulence, the space between the feed tray and the next higher tray must
be larger than the space between the other trays in the tower.
Any remaining light components are removed by steam that is fed into the bottom of the
tower.

The temperature of the crude as it enters the tower is usually sufficient to vaporize or flash
out most of the light components

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The part of the column where light components are stripped out of the liquid is called the
"stripping section".

The liquid that works its way to the bottom of the tower is removed as reduced crude.
In most distillation columns, trays are numbered from the bottom up to the Top.

The vapours generated at the bottom of the tower contact the liquid on the first tray of
section B, then, the vapours are cooled, and some of the heavier hydrocarbons in the
vapours condense.

Figure 2: Distillation unit for crudes (Topping)

At the same time, the liquid absorbs heat from the vapours so some of the light fractions in
the liquid vaporize.

The vapours developed on the first tray of section B pass up through the risers and bubble
caps into the liquid on the second tray of section B.

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The liquid on the second tray is at a slightly lower temperature than liquid on the first tray.

When the vapours bubble up through the liquid on the second tray, the heavier
hydrocarbons in the vapour tend to condense.

The lighter fractions in the liquid absorb heat and vaporize

The highest temperature is at the bottom of the column, and the lowest temperature is at
the top of the tower.

The operation of a distillation column depends on the constant process of vaporizing and
condensing.

As this vaporization-condensation cycle repeats itself, a different fraction is gradually

isolated on each tray.

The tray temperature determines the composition of each fraction at fixed pressure.

The lightest fraction is developed on the Top tray & the heaviest fraction is developed on
the bottom tray;

As moving up the distillation tower, the products become lighter & lighter, consequently
temperature decreases towards the last tray & column top

The condensed vapours flow down to the tray below while the vapours that have not
condensed rise into the next tray of section B.

The liquid and vapours at the top of section B are essentially free of the heaviest fraction,
reduced crude.

Part of the liquid on the tray at the top of section B is drawn off into a separate still, called
a stripping column which is described hereunder in following paragraphs.

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4. TYPES DE DISTILLATIONS
Two types of distillation exist:

¾ Unsteady Distillation (Distillation par batch)

¾ Steady Distillation (Distillation continue)

4.1. UNSTEADY STATE DISTILLATION

Operation of the still (Column) by putting in a batch of mixture, vaporizing part of the
mixture, and draining off the part that is left, is called "batch distillation" or "unsteady
state distillation."

For example in Schematic diagram of a two-component unsteady state distillation,

hereunder, the mixture to be separated is 50% hexane and 50% pentane.

If all the mixture is vaporized, the

condensed liquid collected at Point E
contains 50% pentane and 50% hexane.

To separate the mixture, it must be

partially vaporized, because pentane is
more volatile than hexane, it tends to
vaporize more rapidly than hexane.

When heat is applied to the mixture to

partially vaporize it, the vapours pass
from the liquid mixture, at Point B, to the
tubing, at Point C. At this point the liquid
has changed to a vapour, or gas.

The vapours pass from the tubing to a

condenser at Point D.

Figure 3: Schematic diagram of a two-

component unsteady state distillation

The condenser produces a liquid product by removing heat from the vapours.

The condenser converts the vapours to a liquid, at the point when the liquid is half-
vaporized, pentane, the lighter component, is concentrated in the condensed vapour.

At the time when the liquid is partially vaporized, hexane is concentrated in the liquid.

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4.2. STEADY STATE DISTILLATION

Steady state distillation is much more efficient than unsteady state distillation.
In unsteady state distillation the liquid is introduced into the still one batch at a time.
In steady state distillation, the liquid is introduced continuously.

The liquid feed enters the still continuously at Point A. Part of the liquid is withdrawn from
the still continuously at Point B. The liquid withdrawn from the still at Point B is enriched in
hexane.

Just as in unsteady state distillation, the vapours are condensed in the condenser.

The liquid collected in the condenser is enriched in pentane.

Because the liquid is fed to the still continuously and the liquid is removed from the still
continuously, the composition of the liquid in the still remains the same.

Because the composition of the liquid in the still remains the same, vaporization is
maintained in the still without a change in temperature.

Both steady state and unsteady state distillation involve the application of heat to a mixture
to partially vaporize the mixture, and the use of a condenser to remove heat from the
vapours.

But in steady state distillation, the conditions in the still remain the same.

Figure 4: Schematic diagram of a two-component Steady State distillation

Although steady state operation of a simple still is much more efficient than unsteady state
operation, it is not very practical in the oil industry.

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The condensed vapours are not pure enough in the percentage of pentane to be useful,
nor is the liquid in the still pure enough in the percentage of hexane to be useful, nor is the
liquid in the still pure enough in the percentage of hexane to be useful.

4.3. MULTIPLE STILLS DISTILLATION

The first still in Figure Diagram of the configuration of a three-phase three-condenser

distillation hereunder is the same as the single still in Figure Schematic diagram of a two-
component Steady State distillation (Paragraph 4.2), but the distillation apparatus shown in
Figure of this paragraph was created by joining two additional stills to the still shown in
Figure of previous paragraph.

Using multiple stills can increase the purity of one of the products.

The feed is introduced continuously to Still One. Instead of being withdrawn continuously
from the first still, this liquid becomes the feed to Still Two.

The liquid feed to Still Two is richer in hexane than the feed to Still One.

Because the feed to Still Two is richer in hexane, the boiling temperature in
Still two must be higher than the boiling temperature in Still One.

1 2 3

Figure 5: Diagram of the configuration of a three-phase three-condenser distillation

The boiling point in Still Three is higher than the boiling temperature in Still Two.

The liquid that is withdrawn from Still Three is even further enriched in hexane.
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The vapours are condensed in condensers at each still. The vapours from each still
contain a higher percentage of pentane, and a lower percentage of hexane than the liquid
in the still.

The vapours condensed at Still Two and Still Three are less concentrated in pentane than
the original liquid feed to Still One. The liquid stream from the total multiple still is
relatively pure in hexane.

The precision of multiple-still operation can be improved by equipment changes, as shown

in Figure Configuration diagram of a three-phase distillation with one condenser
hereunder. In this operation, the vapours are condensed only at Still One.

Figure 6: Configuration diagram of a three-phase distillation with one condenser

Figures also differ in that heat is applied only to Still Three in last schematic.

Operation efficiency of the still in last Figure (with one condenser) is improved over
operation efficiency of the still in previous Figure because only one condenser and only
one source of heat are needed

The vapours from Still Three are cycled back into Still Two. The vapours from Still Two are
cycled back into Still One and are finally condensed at Still One.

Because the vapours are allowed to cycle back through the previous stills, the vapour
stream is richer in pentane than the vapours condensed at Still Three in Figure 5.

Because heat is added only to Still Three, the heat required to vaporize the liquid in Still
One and Still Two is provided by the recycled hot vapours.

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Operation of the stills as shown in Figure with three condensers separates a 50-50 mixture
of pentane and hexane into a 63% pentane - 37% hexane vapour stream and a relatively
pure 15% pentane - 85% hexane liquid stream.

Multiple-still operation produces one stream of relatively pure product.

Adding more stills in the series improves the purity of the liquid stream, but does not
improve the purity of the vapor stream.

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Light component vapors

back to main Column
5. STRIPPING
Aim
To extract the light phases which remain in the heavy cuts
through re-vaporisation either by increasing temperature
or by decreasing partially the pressure of the mixture.
(e.g. to remove the remaining gasoline’s, commonly
called Naphtas, from a Kerosene cut) using a Stripping
inert fluid that is not a hydrocarbon. This function is often
performed by steam in so called lateral stripping columns
connected to the distillation column.

Figure 7: Schematic diagram of a Stripping column

By construction the stripping column also has trays, bubble caps, and down-comers like
a miniature distillation tower.

As the liquid flows through the stripping column, it contacts steam. The steam lowers the
hydrocarbon partial pressure and the lightest components in the liquid are vaporized.
Again, refer to figure of first figure in paragraph 3.2.2, these vapours are returned to the
distillation column several trays above where the liquid was withdrawn.

The liquid that leaves the bottom of this first stripping column is a product called Gas Oil.
The vapours from section B along with vapours from the gas oil stripping column rise into
section C.

Then, the same vaporization-condensation cycle that occurred in section B repeats itself
on the trays in section C. At the top of section C, a portion of the liquid is withdrawn to
another stripping column where the lighter vapours are stripped from kerosene.

At section D, another stripping column withdraws part of the liquid as Naphta, and so on
the vapours continue to rise, and the liquid continues to flow down.

The vapours that are fed back into the tower combine with vapours from section E and
rise toward the top of the tower, where gasoline is drawn off as overhead vapour.

The overhead vapour passes to a condenser where gasoline is condensed. Vapours that
will not condense (called non-condensable gases) are sent to the plant fuel system or are
removed for further processing. These gases are also used to control pressure in the
tower and are stored in the reflux accumulator drum before leaving the system. A part of
the liquid that does condense from overhead vapours is returned to the tower as a
controlled flow of reflux.

The liquid that flows down from one tray to the next one is called (as already stated above)
internal reflux because it does the actual cooling inside the tower. At each tray the reflux
is provided by the cooler liquid from the tray above.
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5.1. DETAILED DESCRIPTION OF A STILL SECTION

Stripping can be accomplished more efficiently in a standard column of Distillation

The section of the column shown in Figure Diagram of the distillation of a Pentane /
Hexane mixture hereunder is used to Strip pentane from hexane.

The section of the column shown in this figure performs with one piece of equipment the
same stripping operation that required multiple stills in the process shown in figure
Configuration diagram of a three-phase distillation with one condenser in paragraph 4.3

Each deck in the stripping section of

the distillation column illustrated here
corresponds to one still in figures of
paragraph 4.3.

Because the whole operation is

carried out in one unit, certain
devices are necessary to separate
the decks from each other.

Figure 8: Diagram of the distillation of

a Pentane / Hexane mixture

In the distillation column the feed

enters near the top of the stripping
section, and passes down through
the down-comers on all the trays into
the reboiler where heat is applied to
the mixture

The heat that is applied to the mixture

in the reboiler vaporizes the liquid,
and the vapours are returned to the
distillation column

Vapours leaving the lowest tray pass upward in the same way through the next tray, and
the vapours leaving that tray pass through to the next tray above, causing the liquid to boil.
As these vapours give up heat to the liquid, some of the heavier vapours condense.

The vapours that condense and become part of the liquid are primarily hexane.

The heat supplied from the hot vapours to the liquid on the tray causes some of the lighter
liquid to vaporize and pass upward.

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As in the series of multiple stills in figures of paragraph 4.3, the vapour that leaves the
stripping section of the distillation column is not as pure in pentane as the bottom product
is in hexane.

Like the multiple stills in figures of paragraph 4.3, the distillation column separates the
mixture into two product streams.

The liquid stream is relatively pure; the liquid stream can be made more pure by adding
more trays to the stripping section of the distillation column.

To be most useful, the separated mixture should be relatively pure in both streams.

Figure Operating diagram of a column section hereafter, shows a simplified close-up

drawing of the separating devices.

Each separation stage consists of a metal shelf

called a plate, deck, or tray.

Vertical chimneys that let the vapours through the

tray are called risers.

A bubble cap covers each riser.

The bubble caps allow the hot vapours from one

tray to bubble through the boiling liquid in the next
tray.

The down-comer (or boot) allows the liquid to flow

from one tray of the column downward to the next
tray.

Figure 9: Operating diagram of a column section

One complete tray assembly consists of the tray

itself, the vertical chimneys, called risers that
protrude and are covered by bubble caps, and the
down-comer, which allows liquid to flow from one
tray to another.

Each tray assembly compares to one still in figures of paragraph 4.3.

Two relatively pure product streams can be obtained by modifying the distillation column.
Another section is added to the distillation column above the stripping section.

The parts of the column above and below the feed entrance have different functions.

The stripping section produces a bottom product pure in hexane.

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The rectifying section above the feed produces an overhead product pure in pentane.

The section above the feed is the rectifying section.

After the feed enters the column, the liquid drains down nearly to the bottom and enters
the reboiler, where it is partially vaporized.

The vapours from the reboiler re-enter the still and proceed upward in the distillation
column.

At each tray some portion of the heavier component condenses and flows down to the
next lower tray.

Figure 10: Diagram of two-component (C5 & C6) distillation

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The vapours formed and not condensed continue up through the column, heating the liquid
in the trays and becomes more and more concentrated in pentane.

At the top of the column, parts of the vapours are condensed, and parts of the vapours
are removed as overhead product.

To obtain a separation on any stage, hot vapours must bubble through the liquid on the
stage, causing it to boil.

To maintain a liquid level on the top stage, part of the condensed vapour is fed back into
the column as reflux.

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6. FRACTIONATION
Most mixtures that are separated in the oil industry are multi-component mixtures and
need to be divided into more than two product streams.

The components of these mixtures are called fractions, and the process by which they are
separated is called fractionation.

If a multi-component mixture is partially

vaporized, the lighter fractions tend to
concentrate in the vapor and the heavier
fractions tend to concentrate in the
liquid.

Figure 11: Fractionation of crude oil

A typical crude oil contains many fractions. If the crude oil shown opposite right is
fractionated, reduced crude is the bottom product. The overhead products are gas and
gasoline.
To separate a multi-component
mixture, the distillation column
shown in Diagram of two-
component (C5 & C6)
distillation in previous
paragraph must be modified. It
allows for the removal of only
two fractions of products.

Figure 12: Diagram assembly

for distillating crude oil &
fractionating cuts

To separate a typical crude oil,

the tower must be modified and
allow for the removal of several
fractions.

All fractions between the

lightest and the heaviest
fractions are removed from the
tower into separate stripping
columns. Each of the stripping
columns strips the lightest
fractions from the liquid. The
liquid (consisting of the heaviest
fraction) is removed from each
stripping column as product.
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As stated before all the vapours from the stripping columns are returned to the
fractionating tower.

The fractionating tower consists of a stripping section below the feed and a rectifying
section above the feed. The feed is heated by a preheat furnace.

Vaporization in the tower below the feed point is provided by steam fed into the bottom of
the tower.

Figure 13: Photo showing what

happens on a tray

Heat for vaporization above the feed

is provided by hot feed entering the
tower from the preheat furnace.

Each tray in the fractionating tower

contains liquid that is boiling at a
specific temperature.
Boiling liquid maintains the
temperature on each tray.

The bottom product drawn off is reduced crude.

The rising vapours mingle with the boiling liquid on the first tray of Section B, and the
heavier hydrocarbons tend to condense.

The vapours developed on the first tray of Section B rise through the risers and the bubble
caps into the liquid on the second tray of Section B.

The liquid on the second tray is also boiling at a specific temperature, slightly lower than
the temperature on the first tray.

When the vapours bubble through the boiling liquid on the second tray, the heavier
hydrocarbons tend to condense.

The condensed vapours flow down to the tray below; the vapours that have not condensed
rise into the next tray of Section B.

The liquid and vapours at the top of Section B are essentially free of the heaviest fraction,
the reduced crude. Part of the liquid on the tray at the top of Section B is drawn off into a
separate still, called a stripping column.

The stripping column strips the light vapours from the mixture and gives gas oil as a
product.

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Vapours from the liquid drawn off from Section B are re-introduced into the fractionating
tower at Section C and are fed back into the tower at a point higher than the point where
the liquid was drawn off.
The mixture entering a stripping column is liquid. Vapours from Section B rise directly into
Section C. At the top of Section C, a portion of the liquid is withdrawn to another stripping
column, where the lighter vapours are stripped from kerosene.

The vapours continue to rise, and the condensed vapours continue to flow down.

At Section D, another stripping column withdraws part of the liquid and provides naphtha
as a product.

The vapours that are fed back into the tower combine with vapours from Section E and
rise toward the top of the tower, where gas and gasoline are drawn off as overhead.
The overhead vapours pass to the condenser, where the gasoline is condensed.

A part of the liquid condensed from these vapours is returned to the tower as a controlled
flow of reflux. The reflux is pumped into the top tray of the tower. This cooled liquid
removes heat from the rising vapours. The reflux condenses the heavier fractions on the
top tray, so they flow through the down-comer onto the tray below. At each tray, the reflux
is provided by the cooler liquid from the tray above.

The operation carried on in the fractionating tower is a two-way process. A stream of

vapours rises upward and a stream of liquid flows downward.

The condensed overhead returned to the top of the tower is called reflux.

The liquid flowing down to lower trays is also called reflux. Reflux flowing down and
vapour rising up to each tray controls the temperature of the liquid on that tray.

At the temperature on each tray, some of the liquid vaporizes and some of the vapours
condense. The working of a fractionating tower depends on the constant process of
vaporizing and condensing.

This necessary vaporizing and condensing is constantly maintained throughout the

fractionating tower by the difference in temperature between the reflux that is flowing
downward and the rising vapours.

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6.1. EXERCICES

1. Consider two liquids: Liquid A is composed of Light molecules and Liquid B is

composed of Heavy molecules. Which liquid has a lower volatility?

‰ Liquid A

‰ Liquid B

2. To separate the components, only a portion of the mixture is vaporized. Then the
remaining liquid is drained off, and a new batch of mixture is put into the still. In which
component the liquid that is drained off is enriched?

‰ The lightest component

‰ The heaviest component

3. As more pentane passes into the vapors, the remaining liquid is enriched in hexane.
Hexane has a higher boiling point than pentane, so the boiling point of the liquid must
rise to maintain vaporization. How are the conditions Temperatures & composition in
the Still constantly changing or always the same?

‰ Constantly changing

‰ Always the same

4. The heat that is applied to the mixture in the reboiler vaporizes the liquid, and the
vapors are returned to the distillation column. Where do the hot vapors enter, at the top
or at the bottom?

‰ At the top

‰ At the bottom

5. The heat supplied from the hot vapors to the liquid on the tray causes some of the
lighter liquid to vaporize and pass upward. Which is the component with the higher
percentage contained in vapors than in the remaining liquid?

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6. The stripping section, which strips the lighter component from the heavier, leaving the
heavier component relatively pure, is above the feed or below the feed?

‰ Above the feed

‰ Bellow the feed:

7. If the temperature on a tray at the bottom of Section B is 640° F, the temperature on a

tray at the top of Section C is:

‰ 240°F

‰ 700° F.

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7. DISTILLATION TECHNOLOGIES

7.1. TRAYED COLUMNS

7.1.1. Bubble Cap Tray)

The bubble cap tray, shown, is not

a part of the tower structure, but is
supported in the tower.

It can be lifted or knocked loose.

Because the tray is light and not

designed to resist much pressure,
rapid changes in pressure or vapour
velocity can cause the tray to lift.

Figure 14: Bubble cap tray

Because metal expands when it is heated, the tray design and installation must allow for
expansion. If too little allowance is made for expansion, a tray pressing against the shell
may bend or warp.

The primary function of the bubble cap tray is to bring

liquid and vapour into close contact.

Bubble cap trays are designed to permit the vapour to

bubble through the liquid with maximum efficiency and
contact.

Figure 15: Bubble caps

The riser (chimney) allows vapour to come up from the tray below. Risers also support the
bubble caps. The bubble cap is mounted on top of the riser.

Most bubble caps are round, allowing for good vapour-liquid contact. The lower edge of
the bubble cap contains teeth or slots. The vapour is forced out through the teeth at the
lower edge of the bubble cap into the boiling liquid on the
tray.

The bubbles formed should be small so that there is a

greater area for vapour-liquid contact. For example, if
Bubble A is separated into smaller bubbles, there is
greater chance for vapour-liquid contact.

Figure 16: Bubbles

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The vapour’s speed (velocity) through the bubble cap's teeth and slots must be at a set
rate. If the vapour velocity is too slow, the bubbles formed are large and fractionation on
the tray is poor. On the other hand, if the velocity is too fast, the vapour "blows" through
the liquid with no contact.

The sketch represents what happens when

vapours pass through a bubble cap tray.

The vapour is broken into small bubbles,

which increase the surface area for vapour-
liquid contact.

Figure 17: Vapour passing through a bubble

cap tray

The bubble cap sits on top of the riser and the riser channels down from one tray to the
next through down-comers

7.1.2. Down-comers

The down-comer is a passageway through which the liquid flows down from one tray to the
next lower tray. Reflux is carried down the tower by the down-comers.

The chimney provides an upward passageway for vapour and the down-comer provides a
downward passageway for liquid.

Down-comers are sometimes referred to as "inlet" or "outlet" down-comers:

The down-comer that brings liquid down into a tray from above is the inlet down-
comer. The inlet down-comer on one tray is the lower end of the outlet down-
comer on the tray above.

The down-comer that allows liquid to run down out of a tray is called the outlet
down-comer.

The down-comers on all trays must be free of obstruction or the liquid flow will be
impaired.

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7.1.3. Weirs

Weirs are dams that rise from the trays.

Weirs, like down-comers, are either inlet or outlet. Liquid leaving the tray must flow over
the outlet weir before it enters the down-comer.

The overflow weir keeps a proper liquid depth on the

tray, keeping the bubble cap teeth submerged. The
distributor weir is placed on the inlet side of the tray in
front of the liquid down-comer.

The liquid coming down from the tray above flows over
the distributor weir before it crosses the tray. The
distributor weir helps to spread the liquid across the
tray.

Figure 18: Overflow weir

Weirs are natural places for blockage, because they

retain coke, scale, bolts, or other foreign material.

Trays have small drains or "weepholes" drilled into them. The drains are about 1/4 - 1/2
inch. When the tower is shut down, the weepholes let out any liquid trapped on the trays
so that the tower may be cleaned.

Most trays in the tower are level, but trays where a side stream is being drawn off have a
low place at the end or middle of the tray. A low place in certain trays is called a "trapout
pan." This depression collects a pool of liquid on a tray where a side stream is being
removed.

The trapout pans gather a pool of liquid to be drawn off from the tray without affecting
efficient fractionation.

To provide proper side stream flow, trapout pans must be clean.

"Tray gradient" refers to the difference in liquid depth on the

inlet and outlet sides of the tray. Normally, the liquid on the inlet
side of the tray is higher. In this drawing, bubble formation on
the outlet side of the tray is poor, because the teeth or slots of
the bubble cap are above the liquid level.

Figure 19: Tray gradient

If the liquid level is too shallow, the efficiency of that tray decreases. Also, tray efficiency
is decreased if coke, scale, or other deposits foul it.

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7.1.4. Tray Types

Each tray in a fractioning tower must provide contact between vapour and liquid. Trays
differ from each other in the way they bring about this contact. The most common tray is
the bubble cap tray, which lets vapour bubble up through liquid held on the tray by the
overflow weir.

Bubble caps are scattered about the tray in a pattern that creates an even distribution of
vapour bubbling through the liquid.

Bubble cap trays are efficient for most feeds, but with
some materials, vapour-liquid contact can be maintained
at lower costs with other types of trays, including:

Sieve deck.

S-section.

Glitsch or ballast tray.

Side-to-side pan.

Figure 20: Overflow weir

7.1.5. Sieve Deck

The sieve deck is used for a large quantity of materials, but its capacity is inflexible. A
tower equipped with sieve decks must handle a relatively fixed quantity of material.

For example, this sieve deck is equipped with down-comers and weirs like the bubble cap
tray. This tray is a sheet of light metal with a large number of holes drilled through
it. Vapour rising in the holes keeps the liquid on the tray and bubbles up through it. The
overflow weir keeps a constant depth of liquid on the tray.

7.1.6. S-Section

The S-section tray is also inexpensive

and easy to construct. It is made of
overlapping
S-shaped sections which form long
continuous bubble caps and troughs for
the liquid and the vapour.

Figure 21: S-section

Each long "cap" has slots cut in its lower edge that act like bubble-cap teeth, releasing
vapour into the liquid in the troughs.
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7.1.7. Glitsch (Ballast) Tray

The ballast tray works much like the
bubble cap tray. The ballast tray
changes its openings to handle flow
rates varying from low to high.

Figure 22: Ballast tray

A typical
ballast tray has large holes like the bubble cap tray, but these
holes do not have risers. Each hole has a cover consisting of
two or three nested caps held in place over the hole by guides
that go down through the plate and hook beneath it.

When there is no vapour, the lowest cap sits over the hole and
closes it. The second cap stands above it on short legs.
Under low pressure, the lowest cap rises only until it meets the
second cap.

As the flow of vapour increases, both the bottom cap and the
second cap may rise until the top cap stops them. So, the hole
opens in stages to allow a variation of the vapour flow from a low
to a high rate.

Figure 23: Nested caps

7.1.8. Side-to-Side Pan

The side-to-side pan (shown

here below) is often used when
coke or other fouling material is
present.

These materials can block

bubble cap risers and interfere
with vapour-liquid contact.

Figure 24: Side-to-side pan

The side-to-side pan drops a curtain of liquid for the vapour to pass through.

While this pan is not efficient in vapour-to-liquid contact, it can process foul liquid without
reducing liquid-vapour contact

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7.2. PACKED TOWERS

Most oil industry towers are tray towers, but packing instead of trays is used in some
towers to provide contact between vapour and liquid.

Packing material used in towers may be ceramic, non-corrosive metal alloy, or other
substances that resist corrosion by impurities in the feed.

The most common types of packing are:

Raschig ring.

Berl saddle

Figure 25: Packings

7.2.1. Berl Saddle

The Berl saddle is usually made of non-corrosive stamped

metal alloy.

Figure 26: Berl saddle

7.2.2. Raschig Ring

The Raschig ring is a hollow cylinder with a diameter equal to

its height. There are three common types of Raschig rings.

Towers using Raschig rings and Berl saddles are packed

randomly. Ceramic rings are dropped into water to prevent
breakage during packing. The towers are packed with
material the way a pail is filled with ice cubes.

Figure 27: Raschig rings

Other towers are packed in layers. These towers may be

packed with material placed in layers between sheets of
mesh.

Packed towers provide large surface areas over which the descending liquid may contact
the rising vapour.

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7.2.3. Limits of satisfactory packing operation for a specific set of packing

fluid properties

7.2.3.1. Liquid entrainment – flooding

Generally, packed columns should be operated somewhere between 25 and 85 % of flood.

Tight designs run the risk of having excessive liquid entrainment or even flooding.

On the other hand, operation at very small percents of flood is unwise, both economically
and because of reduced efficiency due to insufficient vapour/liquid contacting.

7.2.3.2. Liquid distribution

The importance of good liquid distribution cannot be overemphasized, since the potential
efficiency of any packing can only be attained when the packing is evenly wetted.

The actual type of distributor which should be used depends on column size, packing type
and intended column service.
Liquid distributors should generally be located 15 to 45 cm (6 to 18 inches) above the
packing in order to provide sufficient free vapour space in the column for gas disengaging.
Liquid re-distributors are used to correct mal-distribution of liquid in a column by collecting
liquid from an upper bed and distributing it uniformly to a lower bed.

A re-distributor should be used between beds of Rashing rings and Berl saddles, but is not
generally necessary between beds of Pall rings or Intalox saddles. 26
The maximum bed depth (without redistribution of liquid) should be 6 m (20 ft) regardless
of packing type. More frequent liquid redistribution should be considered for any packing
where the liquid rate is less than 5 m3/(h.m2).

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7.3. COMPARISON BETWEEN TRAYED AND PACKED COLUMNS

7.3.1. Advantages and drawbacks of trays and packing

Pressure drop

Packed columns usually yield a lower pressure drop per equilibrium stage.

This can be important for low pressure operations.

At the elevated pressures encountered in natural gas processing, column pressure drop is
usually not a major issue.

Liquid loading

For a given diameter a packed column has more capacity than trayed columns when liquid
to vapour ratio is high.

Corrosion

Random packing can be fabricated from ceramics and plastics instead of trays fabricated
from expensive alloy materials.

Flexibility

Packed columns usually have limited turndown capabilities. Whereas trays can be
operated as low as 10-15 % of full load, packings are limited to about 50 % of fuel load.

Liquid distribution

In trayed columns, the liquid phase is forced to flow across a tray surface.
With gas bubbling through the liquid, contact is assured. In packed towers, the liquid and
vapour are free to seek their own flow paths and channeling can occur.

In packed columns the control of the vapour and liquid phase’s distribution is a critical
problem.

Liquid phase must be properly distributed at the top of the column and must be
redistributed at 6 meters intervals or every 10 column diameters, whichever is smaller.

Packed towers are more susceptible to plug with dirt and other foreign materials than
trayed columns.

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In production operations where salt water is present, salt plugging is a problem if the
temperature is high enough to vaporise the water.

7.3.2. Choice criterions for trayed and packed columns

There are some general guidelines for the first choice between trayed or packed columns.
These are not absolute because in some services they are both suitable, the choice being
economic or operational (e.g. floating support in offshore production).

Generally, a packed column is suitable when:

The column diameter is small (less than 600 mm),

Corrosive fluids require special metallurgy,

A low pressure drop is needed (e.g. vacuum columns),

The liquid rate is high enough to minimise distribution problems,

The depth of packing required does not exceed about 8 meters.

The depth of random packing is limited by the crushing or deformation

characteristics of the packing (some plastics are limited to bed depths of 3 to 4
meters),

The liquid foaming is not pronounced. When foam is present, it tends to fill the
interstices of the packing and enhance flooding.

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7.4. EXERCISES

8. Which one has a distributor?

‰ Weir A

‰ Weir B

9. For good fractionation, the vapor velocity must be:

‰ Fast

‰ Moderate

‰ Slow

10. Which tray is designed to work with variable flow S-section?

‰ Sieve deck

‰ Ballast

11. In which cases the packed towers are very efficient: when vapor and liquid are
distributed throughout the tower evenly or unevenly?

‰ Evenly

‰ Unevenly

12. If a tower does not use trays, it is called a:

‰ Carbon tower

‰ Demister

‰ Packed tower

‰ Tray tower

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8. AUXILIARY EQUIPMENT
8.1. REBOILERS

Heat for fractionation is normally

supplied by a pre-heater, a reboiler,
or by a combination of a pre-heater
and reboiler.

The type of heater depends on the

operation being performed.
Heavy oils are usually fractionated
with a pre-heater supplying all the
heat.

Figure 28: Example of a reboiler

For example, a tower producing asphalt usually employs only a pre-heater.

For operations involving light hydrocarbons, reboilers are usually used in combination with
the preheated feed.

For example, separating hexane and pentane is usually accomplished using preheated
feed and a reboiler.

In a reboiler tower, the preheated feed entering the tower contacts vapor rising from the
bottom of the tower. The vapors rising from the bottom of the tower are generated in the
reboiler. These vapors strip the lighter components from the liquid on each tray. At the
bottom of the tower, only the heavier fractions remain. The overhead vapor is then
removed from the tower and condensed, and part of this condensate is returned to the
tower as reflux.

The bottom product can be drawn off from the

bottom of the tower, and it is basically free of
the lightest fractions.

The reboiler is usually a separate unit located

beside the tower. It is a heat exchanger that
provides heat to the bottom of the tower.

Figure 29: Composition of a reboiler

The reboiler consists of a metal shell with tube

bundles inside. The liquid flows through the
shell around the bundle, and is heated by the
hotter metal in the tube bundle.

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On this tower are shown the two main equipments which

allow operating the distillation:

The equipment at Point A is the reboiler.

At Point B, vapors rising from the reboiler enter the tower.

Then, at Point C, liquid from the tower is drawn off the
reboiler.

The liquid and vapor lines must be kept clean or the flow of
the liquid and vapor passing between the reboiler and the
tower will be interrupted.

Figure 30: Distillation equipment

At the top outlet is shown the condensing assembly made of

one condenser & the Reflux Drum

Baffles direct the flow of liquid through the

reboiler and must be installed in the tube
bundle. The baffles ensure that all the liquid is
heated by forcing it to contact the hot tube
bundles.

Figure 31: Baffles

NB: Please report to the appropriate module concerning the different ways of Heating a
fluid: EXP PR EQ 110 to get more details for this topic

8.2. CONDENSERS

Tubes must be kept clean inside and

outside to provide good heat exchange.

A condensing process is the reverse of a

reboiling process. While reboilers are used
to add heat to a liquid, condensers are
used to remove heat from a vapor.

Figure 32: Condenser

In fact, condensers are used to liquefy the

overhead product. A condenser usually
consists of a metal shell containing a tube
bundle.

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The overhead product passes around the tube bundle. The overhead vapor continually
passes into the shell. Cooling water circulating through the tubes removes heat from the
vapor and comes out warmed.

The condensate (condensed vapors) passes from the condenser into an

accumulator. From the accumulator, some of the condensate is removed as product and
some is pumped back into the tower as reflux. Reflux enters the tower at the top.

Diagrams of this process usually show condensers at the top of the tower. In a small unit,
the condenser may be located at the top, but in a large unit, the condenser is usually too
large to be mounted at the top of the tower.

In this tower:

The condenser is located at Point A.

The accumulator is located at Point B.

The overhead product is removed at Point C.

Overhead vapor is removed at Point D.

Reflux enters the tower at Point E.

Figure 33: Distillation equipment

In condensers, the shell side of the tube is often damaged by

corrosion. Resulting leakage may allow oil and water to mix.

Water sent to the tower with reflux can cause violent pressure surges or poor operation. If
condenser leakage is not prevented or repaired, water may re-enter the tower with the
reflux.

Gas escaping from the condenser with the water can be a financial loss and a fire
hazard. If there is leakage in the tube bundles, dangerous gases may get out of the
condenser into the cooling tower or sewer, with the warmed water.

The reboiler is shown at the bottom part, as previously stated.

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8.3. STRAINERS

During the operation of a tower, bubble caps, bolts, coke, and other foreign bodies may be
dislodged and carried along with the reflux. If these objects pass out of the tower with the
bottoms product, they can damage the pumps.

Strainers in the bottom of the tower can prevent damage to pumps. The bottoms product
passes through the strainers as it is pumped off for storage. The strainers trap loose
objects as the bottoms product is pumped off.

Strainers must have small enough openings to catch even small objects, but large enough
openings so that the flow of oil out of the tower is not hindered. The holes must be kept
open so that the flow of liquid through the strainer is not blocked.

8.4. REFLUX DISTRIBUTORS

Overhead reflux is normally returned to the tower on the top tray.

If there is nothing to spread the reflux evenly across the tray, all of the reflux will pour into
the tower at the same spot. Then, it may not spread itself evenly across the whole tray.

Figure 34: Reflux distributors

Some towers can spread the reflux evenly over the

whole top tray.

For example, tower B has a reflux distributor that spreads the reflux across the tower
which is a better solution.

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8.5. DEMISTERS

Entrainment occurs when drops of liquid

suspended in vapor are carried up into the next
tray, or into the overhead.

Entrainment can be serious when the overhead

product must be a dry gas.

It can usually be cut down by controlling vapor

velocity and by proper tray spacing.

Figure 35: Demister

It can also be cut down by "demisters" that are

fitted in the tower where entrainment is most
likely to have serious consequences.

Demisters (entrainment eliminators) are usually located at the top of a tower.

Entrainment occurs when drops of liquid suspended in vapor are carried up into the next
tray, or into the overhead.

Demisters are constructed of fine gauge wire knitted into mesh.

Vapors can pass easily through the mesh, but drops of liquid cannot.

Demisters must be kept clean of dirt or foreign matter.

Plugged demisters hamper the flow of vapor.

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8.6. EXERCISES

13. The reboiler vapors returning to the tower contain the heaviest or the lightest fractions?

‰ The heaviest fractions

‰ The lightest fractions

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9. OPERATING PARAMETERS

9.1. DÉFINITIONS OF OTHER GENERAL BASIC PARAMETERS

The three main criterions characterising a distillation are :

Temperature Gradient

Initial Boiling Point

Distillation End Point

9.1.1. Temperature Gradient:

The range of temperatures from the top of the column to the bottom is called the
"temperature gradient."

The temperature gradient can reveal a great deal about how well the column is performing.

The temperature on each tray in a distillation column is different.

So, the composition of the fraction on each tray in a column is different. Heat is added to
a tray by hot vapors rising up the column.

Heat is removed from a tray by reflux flowing across it and down the column.

If some of the reflux is drawn off as side product, the amount of heat removed by the reflux
from the trays below the draw-off decreases.

As already stated along this module, in a distillation column, there is a countercurrent flow
of fluids. A stream of hot vapors rises up in the column and a stream of cooler liquid flows
downward. The vapors bubble up through the liquid on each tray inside the tower. As a
result of this contact, light materials in the liquid tend to vaporize and heavy materials in
the vapor tend to condense

The highest temperatures occur at the bottom of a column, where hot vapors are
generated.

The high temperatures vaporize most of the light material out of the liquid, so a heavy
fraction is formed at the bottom of the column.

The lowest temperature occurs at the top of a column where reflux is added to the system.

The cooler reflux condenses most of the heavy material out of the rising vapors, so a light
fraction is isolated at the top of the column
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9.1.2. Initial Boiling Point

The initial Boiling Point of a product is determined by a laboratory distillation test.

To conduct the test, the sample is placed in a container and heated. The vapors rising
from the sample pass through a condenser and are collected.

The temperature at which the first drop of condensate is collected is the Initial Boiling
point.

9.1.3. Distillation End Point

The end boiling point (EP) of a petroleum product is the highest temperature reached
during a laboratory distillation test, or the temperature at which the last drop of liquid
vaporizes during the test.

Because heavy hydrocarbons are the last to vaporize, the end boiling point (or end point)
test is used to check for heavy hydrocarbons present in a product.

9.1.4. Interpretation of a Dew point and Bubble Point curve

Figure 36: Dew point and bubble point

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There are two curved lines on this graph. One represents the dew point; the other
represents the bubble point. A temperature scale is on the left side of the graph.

The bottom scale shows the composition of the mixture of compounds ‘A’ (Light one) and
‘B’ (Heavy one). This graph tells us how much of ‘A’ and how much of ‘B’ is in the vapor
and how much of each is in the liquid at any given temperature.

For example, to find the composition of the vapor at a tray whose temperature is 250º F,
first find 250º F on the temperature scale at Point ‘a’. Then, follow the line over to the dew
point curve at Point ‘b’. Now, drop straight down to the composition scale at Point. ‘c’ The
composition scale reads that the vapor at 250º F consists of approximately 60% ‘A’ and
40%. ‘B’. To find the composition of the liquid on the same tray, start at 250º F on the
temperature scale at Point ‘a’. Then, move over to Point ‘d’ on the bubble point curve.

Finally, drop straight down to Point ‘e’ on the composition scale. The composition of the
liquid on that tray is 25% ‘A’ and 75% ‘B’. There will be a higher percentage of lighter
components ‘A’ in the vapor above a liquid than in the liquid itself.

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9.2. MAIN PARAMETER CONTROL LOOPS

9.2.1. Tower-bottom temperature control loop

The variable being controlled is the tower bottom temperature.

A filled thermal bulb and an attached transmitter act as the sensing or measuring means in
this control loop.

The control valve regulates the flow of steam through the reboiler.

This raises the reboiler temperature, and in turn, more hot vapors are introduced into the
bottom of the tower.

A more precise regulation consists of arranging a cascade between the TIC & the FIC on
the steam, the TIC being the " Master "

Figure 37: Functional diagram of the reboiler loop

(temperature control at tower bottom)

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9.2.2. Pressure control in a distillation column

Recall The pressure should be maintained as steady as possible to prevent the change of
% of mixture on the trays; if ever the pressure is increased thus the temperature has to be
increased as well to recover the correct %!

The figure shows the tower operating pressure. Tower operating pressure is sensed or
measured by a primary element located inside the transmitter.

Measurement information is sent to a controller that records the data on the chart. The
final control element is a valve located on the off-gas line from the accumulator.

Figure 38: Pressure control diagram

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9.2.3. Bottom liquid level control in a distillation column

The figure below shows a liquid level control in the bottom of a distillation column. The
sensing / measuring means is the displacer attached to a liquid level transmitter.
The control valve regulates the flow of bottom product.

Figure 39: Bottom liquid level control diagram

The most standard regulation loop for the bottom level is the cascade between the LIC &
FIC installed on the bottom product outlet line towards the next column ( if any ) in such
way to obtain a steady flow feeding the next column ( in this case the FIC being the
master )

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9.2.4. Differential Pressure

The pressure at the top of the column is slightly lower than the pressure at the bottom of
the column. This slight difference in pressure is called the differential pressure of the
column.

By observing the pressure indicators mounted on the column, and finding the difference in
pressure, this ∆P is easily calculated.

This parameter is not regulated but as an indicator it is very precious to give the behaviour
of the column: foaming, destruction of the distillation process, surge etc…

9.2.5. Flow control loop at the inlet of a distillation column

The control loop in the figure below regulates the flow of feed into a distillation column.
The primary element is an orifice plate located in the flow line. The orifice plate creates a
pressure difference that is measured by a differential pressure cell. The flow transmitter
translates this difference into a flow measurement.

Figure 40: Diagram of a flow control loop at the inlet of a distillation column

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The diagram above gives only an overall view of a crude oil distillation column with a feed
pump located in the Storage (off-site) several hundred metres from the column. The crude
is pre-heated through a series of exchangers in which the heating fluids are the different
fluids that must be cooled when leaving the main column.

The temperature of the crude pre-heated this way is lowered to 90% of its feed
temperature by passing through a furnace with several burner units. The last few degrees
are supplied by a feed / bottom product exchanger.

9.2.6. Process Safety on a Distillation Column

The reality of Process Safety equipment’s on a column is not a well defined specificity; it
depends the type of column and its construction date. At least the common safety devices
found would be for temperature control: they are:

TSHH on bottom temperature, which trips the Reboiler Heater to avoid

vaporisation of too much bottom product.

TSLL on head temperature, which trips the Reflux towards the column to avoid
the ‘re-drop’ of vaporised phase.

Then, according to the type of equipment installed upstream of bottom products

outlet, there could be a LSLL closing totally the outlet LCV. This results in
stopping the supply of the following column (if existing), event which should be
avoided. This LSLL could also trip the Reboiler Heater.

In Packing Column, is found as well a ∆PSHH tripping column supply by closing

the loading FCV.

Concerning the Pressure, there is no PSHH (except in cryogenic distillation) but

two PSV’s (one in service, the second in stand-by).

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9.2.7. Control system for the main parameters of a standard column

This schema illustrates the flow of the material in and out of a distillation column and
shows the location of valves, pumps, and instruments. This is called a "Process Flow
Diagram."

∆P

Figure 41: Diagram of the main control parameters of a standard column

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10. OPERATING A DISTILLATION COLUMN

10.1. OPERATING A STANDARD COLUMN

NB: This paragraph must be taken as nothing other than a general distillation operating
guideline; it is not intended to be an operating handbook for a panel operator in training.

All the operating parameters of a tower are closely related to one another; a modification in
one parameter leads to changes in the others, making operating any given tower a
delicate process, not to mention the effects on the columns downstream.

It is therefore important to act on any one of the four main variables in "Moderate tempo",
as we say in music.

This implies excellent knowledge of the Distillation process, logical thinking and patience.

10.1.1. Pressure

As regards the tower Pressure, it normally does not need to be changed for any given
qualitative load (e.g. for a Crude from a given source). Moreover, a tower cannot distil any
type of Crude, as it is designed for a limited range of crudes.

However, any pressure increase in the column entails the need to act on the reboiling and
reflux temperatures (a good example is water: at atmospheric pressure, P0, water boils at
100°C whereas at a pressure of 2.4 Barg it boils at 166°C and at 12 Barg it boils at
188°C).

However, if for any reason the tower pressure must be reset, by a doing a restart for
example, just proceed as below:

Either directly reset the column’s PIC (Pressure Indicator Controller) setpoint if the
current pressure is within 0.1 to 0.5 Barg of the desired pressure.

Or put the PIC in manual mode and increase the pressure by steps of 0.1 Bar
once the pressure is stabilised at the step.

10.1.2. Temperature

Three temperatures must be scrupulously maintained to obtain the required temperature

gradient from the bottom to the top of the tower:

The feed temperature at the inlet of the column: to change it, act gently on the
inlet TIC and remember that this will not change the temperature at the bottom of
the column, but only that of the bottom product leaving the column, downstream of
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the Feed / Bottom product exchanger. This temperature can vary from 240°C to
380°C depending on the category of Crude being distilled

The column bottom temperature: act on the TIC located on the line returning to
the column, from the sampled bottom Product (reboiling loop).

But, if the temperature is controlled as per described in paragraph 9.2.1 here

above, then it has to be controlled at its initial setpoint.

NB: just to remember that all column temperatures interpret the mixture
composition all along its processing from bottom to top and can be seen on
trays equipped with a TI.

Column head temperature: act on the TIC located at the head of the column, or
on the FIC located on the discharge line of the reflux pump.

Most large-capacity distillation columns also have pump-around return temperatures. As

seen in the descriptive part of this course, these are flow-controlled effluent circulation
loops going from the column trays to exchangers. They are involved in heating accessory
fluids and return to a higher tray with a precise TI; the temperature adjusts itself as a
function of the pump rate going to the relevant exchanger.

Knowing that temperature reactions are slow, always apply small variations in
increments/decrements of + / ─ 1°C and, most important, wait until the variation affects the
other temperatures in the column, generally five to ten minutes.

Any variation that is too strong will change the ratio of components all along the trays or
packing and result in a composition which is out of specification (OOS).

When in doubt, always gradually return to design values, wait until the column stabilises
(this may take ½ to 1 hour) and start over – gradually.

Do not forget that each tray acts as a separator, i.e. for that given temperature and
pressure (which is presumed constant over a small height) there is a very precise
equilibrium between Liquid: vapour ratio, which is why it is so important to respect the
temperature gradient all along the column.

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10.1.3. Flowrates

There are three different types of flowrate:

The feed flowrate rate of the column is controlled by an FIC generally located at
the outlet of the pre-heating exchangers. This parameter is usually adjusted only
during start-up or shut-down phases or as instructed by the plant’s Programme
Section. In this case too, proceed gradually to allow time for the temperature
controllers to react and stabilise at the normal values.

The reflux rate at the head of the column: in theory, we act on the unit flowrate,
i.e. 1 tonne / hour or 1 m3 / hour (but the increments are usually a fraction of
that!).

The reboiling rate for large-capacity columns: when provided by a circulation

pump (doubled or tripled) and a reboiling furnace. In general we act on the
Reboiling TIC, except during start-up phases.

10.1.4. Levels

The two main levels are:

The liquid level at the bottom of the column: this is very important as it
required for reboiling (no level, no distillation – this is the first operation that is
performed at start-up).

An operating tower maintains a constant amount of liquid in the bottom of the

tower.

During operations, the bottom product is drawn from the bottom.

The height that this bottom liquid reaches is the liquid level of the tower.

A normally operating tower maintains a constant liquid level.

Towers are equipped with LIC. These controllers show the height of the liquid level
and by adjusting the LIC in connection with a FIC set in mode "cascade» ensures
the bottom product controls of the liquid level.

The level in the Reflux drum: this is also fundamental because if there is no
level in the drum, there is no temperature control at the head of the column. Make
sure the head condenser is started (usually composed of an air cooler followed by
a water-cooled heat exchanger).

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10.1.5. The lateral cut-extraction levels

There are also LICs on the relevant trays:

Heavy Gas Oil (HGO)

Middle Gas Oil (MGO)

Light Gas Oil (LGO)

Kerosene

Heavy Naphta

Light Naphta

Gas ( LPG & C1 / C2 )

10.1.6. Analysers

On a standard column, there is at least one analyser for composition of distillate (at head)
and an other one for composition of bottom product.

They are in line analysers giving permanent indications / information’s on products

composition (head and bottom). They are of great importance for control of the process.

Viewing the trend graph on DCS screen allow anticipation of correction of operation
parameters following a (abnormal) deviation of the expected values.

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11. PERFORMING DISTILLATION

11.1. STARTING UP A DISTILLATION COLUMN

Preamble

To give an accurate idea of what is starting up a distillation column entails, this section
gives a chronological description of the different stages in starting up a crude oil distillation
column, from the gas in a sub-atmospheric state (FG at a pressure of 1 Barg) up to the
production of components at required specifications.

All “Process” circuits have been drained of steam condensates following the inerting of
circuits with steam).

All the circuits in the column are checked.

11.1.1. Preparing the utilities ready for column start-up

Considering how complex it is to operate a distillation column, it is obvious that all utilities
required for the ensuring the sequence of the different phases must be prepared and
ready before the column is started-up.

Instrument air

Cooling water

Fuel-Gas

LP and MP steam

Electrical power supply (at this stage all electrical motors for the pumps and air
coolers are plugged into the power supply).

Service air

11.1.1.1. Circuits Preparation

The following circuits are then prepared for column start-up:

Line-up of exchanger circuits (usually there are two series of pre-heating

exchangers connected in parallel)

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Filling of exchanger cooling water circuits for the feed and desalter circuits

Line-up of feed circuit for filling

Line-up of bottom product circuit for filling

Line-up of the feed tank and feed pumps (transfer of Crude from Storage to
Distillation)

Gradual start-up of feed pumps at low flowrate to fill up the unit

11.1.1.2. Filling

Then the distillation unit is filled up:

Filling of the Feed circuit up to the Desalter

Filling of the distillation column (bottom liquid level = 75%)

Circulation of crude through the feed heating furnaces (usually the crude passes
through 4 times under the control of the FIC)

When the checked circuits are filled and the level of the crude in the column reaches 75%,
then the feed pump is stopped.

A so-called “Long” closed circulation process is established, in which the crude is pumped
through a closed circuit by the pump at the column bottom. The fluid passes through the
product circuit all the way up to the by-pass valve, and back to the feed circuit upstream of
the series of pre-heating exchangers; it then passes through all the exchangers (feed
side), through the furnace, enters the column where it settles to the bottom, ending its
journey through the closed circulation loop.

The extraction circuits for the Gas-Oil & Kerosene cuts are opened.

At this stage the crude is flowing cold in closed circulation in the unit. The following stage
consists in establishing closed circulation with the heater on to start raising the feed
temperature

11.1.1.3. Verification - Activation

The following circuits are checked and enabled:

Air circuits for furnace combustion

Fuel-Gas for pilot burners

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Fuel-Gas for main burners

The pilot burners and several main burners in the furnace are then lit.

The steam is open to circulate in the convective part of the furnace (production of
overheated steam)

The furnace temperature is increased to 280°C, with a gradient of +40°C / hour to

obtain a crude oil temperature of 110-120°C in the desalter

11.1.1.4. Temperature stage

When the desalter temperature reaches 110 / 120°C:

A so-called “Short” closed circulation process is started, in which the circuit is

shorter because it by-passes the Desalter.

The air-cooler at the top of the column is started.

11.1.2. Following step:

When the short circulation and the circulating crude temperature are stabilised, so-called
“Open (or production) circulation” is established, i.e. from the feed storage tank, using a
transfer pump on stream (used before to fill the unit) and the pump of the unit crude, up to
the product storage tank.

11.1.2.1. Process Conditions

The Product circuit to its storage tank is lined-up

The normal Crude feed circuit is checked and lined-up

The two pumps mentioned above are started

Short circulation is stopped

All of the flow controls (feed flow through the two series of pre-heaters, furnace
pass flows, bottom product outflow) are in “Automatic” mode

The stripping steam circuit at the bottom of the column is opened

Adjustment of the level in the Desalter

Start-up of desalter water circulation pump

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The feed rate is increased to an intermediate value of 50-60%

At this stage, circulation is opened with a column bottom temperature at 280°C, and
distillation, strictly speaking, has now started.

The following stage consists in raising the feed temperature to 320°C and increasing its
flowrate:

11.1.2.2. Raising Temperature

The reflux circulation to the column is started

The temperature is increased to 320°C at a rate of 35°C / hour

The feed rate is increased to 80% in gradual increments

The process safety alarms (TSHH, LSHH, FSHH & their values for LL) are
enabled

11.1.2.3. Production Conditions

When the distillation parameters are stabilised, we move on to production conditions:

The feed rate is increased to 100%,

The tower’s operation settings are fine-tuned,

The furnace temperature is increased to 380°C,

The injection of chemical products is started,

Lateral extractions of the Gas-Oil, Kerosene & Naphtha cuts are opened,

The upper, middle and lower Pump-Arounds are started,

The air coolers are started “on demand”.

The Distillation Section is now in normal production and all products are either in Stock
(Product) or in the Stripping columns (Gas-Oil, Kerosene), or in the downstream processes
(e.g. Desulphuration of Naphtha, etc…).

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11.2. STOPPING A DISTILLATION TOWER

As when starting-up a Crude oil distillation section, the paragraph below lists the
chronological order of the different shut-down phases required to stop it. The starting point
here is when the section is in normal production.

First stage: targeted preliminary operations which would be too long to describe here, but
which are briefly listed:

Reprocessing of slop (products outside specifications) is suspended,

Fuel-Oil burners are stopped

Heavy Gas Oil extraction is stopped

Fluidisation of the above Heavy GO with Light GO (to avoid congealing at lower
temperatures)

First feed flowrate decrease

First feed flowrate decrease

Second feed flowrate decrease

The unit is then in a stable situation at 80% load and 320°C. The following stage consists
in switching to short closed circulation (same setting as the equivalent phase during start-
up).

Temperature decrease from 320°C to 280°C,

Closing of lateral extraction of Gas-Oil, Kerosene & Naphtha cuts,

Shut down of "Pump-Around" system,

Furnaces off,

Turn off circulation of LPG to downstream installations, but keep in mind that
reflux to the column will be at its highest,

Switch to short closed circulation (set the relevant circuit),

Stop the Desalter pumps,

Stop injection of chemicals.

The unit is now cooling down and in closed short circulation. In the following stage, cooling
continues until the temperature reaches 150°C and circulation is switched to the Long
circuit.
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A Product Outlet exchanger on a second column / Crude Feed is bypassed,

The products leaving the tower are directed to the Heavy Slop and Light Slop
tanks,

“Long” circulation is established,

Cooling continues until temperature reaches 100°C,

At 100°C Long circulation is stopped (column bottom pump stopped),

The levels are drained if the section is stopped for a maintenance operation.

The Distillation unit is now in normal shut down and either ready for re-start or ready for
isolation and inerting, in view of maintenance intervention.

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11.3. PREPARING A COLUMN FOR INTERVENTIONS

Preparing a distillation unit for a maintenance intervention is a long operation that requires
two to three days, depending on the importance, size and quantity of the relevant
equipment. The paragraphs below give the chronological order of the different stages
performed when preparing a unit for handover.

At the end of shutdown, there are two possible outcomes at this stage:

Either re-start,

Or continuation for maintenance intervention.

In the second case, we shall proceed with the following actions:

First stage:

Drain all of the liquid hydrocarbons in the unit, from the Battery Limits (the entry
point)

Start the circuit that by-passes the Desalter,

Drain and isolate the pumps using blind flanges,

Prepare a stock tank to store washing effluents,

Blow-down the unit to the flare circuit pressure,

Turn-around the Reversible Joints with the open side towards the Blow-Down
circuit.

Second stage:

Wash all circuits with water.

Third stage:

Drain wash water out of all circuits and equipment (starting with vents to
atmosphere)

Close drains as soon as hydrocarbons appear

Slightly re-pressurise the column

Drain circuits and equipment to Blow-Down circuit through distillation column

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Fourth stage:

Inert all circuits with LP steam to the Blow-Down circuit

Fire up the furnace to prevent condensation of the steam in the lines

Fifth stage:

Inert the LP steam in all circuits to the atmosphere

Sixth stage:

Stop steam insertion

Insert blind flanges to isolate the unit

Re-inert with steam after installing blind flanges

Turn off the furnace

Inert the furnace’s Fuel-Gas circuits with nitrogen

Electrically isolate all rotating machines.

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12. TROUBLESHOOTING

12.1. REFLUX TEMPERATURE DECREASE.

If by any reason (for instance malfunction of the overhead air-cooler) the reflux
temperature decreases then it is cooler, the cooling capacity of the external reflux is
greater.

As the cooler external reflux enters the column, it cools the top of the column.

More than usual this increased cooling condenses more vapours in this section, so the
amount of internal reflux increases & the composition at the top of the column has
changed and the overhead product has become lighter.

There will be an increase in the amount of internal reflux on every tray in the column.

This changes the composition and temperature of each tray.

If the reflux flow is not cut back to counteract the increased internal reflux, and the column
temperature is controlled by steam input to a reboiler, thus the Steam to the reboiler will
increase

To maintain the temperature profile in the column without increasing the steam;

A less expensive way to keep the products on-specification is to reduce the flow of
external reflux.

But the reflux temperature has to be monitored so that when it begins to rise again, the
flow can be increased as needed.

12.2. INTERACTION OF OTHER PROCESS VARIABLES

As already stated; change in one process variable affects changes in other variables.

For example, supposing the feed temperature drops, as the feed enters the column, the
proportion of light components in the feed that will flash immediately decreases.
With fewer components flashing, the proportion of lights components falling to the bottom
of the column increases.

This will cause the bottom level to increase.

And with more lights in the bottom product, the composition of the bottom product will
change.

If there are now more lights in the bottom product, and considering light components boil
at lower temperatures the bottom temperature will decrease, and the flow of overhead

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vapours decreases. And because there are fewer overhead vapours entering the
condenser, the liquid level in the accumulator or reflux drum drops.

When the accumulator liquid gets low enough, there will be insufficient liquid available for
overhead product and for reflux.

12.3. LOSS OF HEAT

Heat entering the tower may be sharply reduced or cut off. When heat entering the tower
is reduced, heat leaving the tower must also be reduced. When heat entering the tower is
totally cut off, the tower must be brought promptly and steadily to a standby condition and
held there until the heat supply is available again.

Heat may be reduced or cut off by failure of the steam pressure supplying heat to the feed.
In a tower with a reboiler, failure in the steam supply may reduce or cut off heat to the
reboiler. Failure in the hot oil to heat exchangers or reboilers may reduce or cut off heat to
the tower.

When the feed or the reboiler no longer provides heat, the reflux flow rate should be
promptly, but gradually decreased. A constant balance between heat into the tower and
heat out of the tower must be maintained, as much as possible, when the heat supply
decreases. Tower temperatures should be kept as normal as possible to provide a quick
return to normal operations. Whatever heat there is should be conserved carefully, to keep
the operation as normal as possible.

A constant balance between heat into the tower and heat of out of the tower must be
maintained as the heat supply is returned to normal conditions. Abrupt swings in tower
temperatures may damage the equipment.

12.4. LOW LOW LEVEL (LSLL) AT REFLUX DRUM

Two possibilities:

The Head Condenser is cooled par water (ER type).

Verify the positions of inlet and outlet valves of the ER. Most of the time, they are
butterfly valves with manual lock. Due to vibrations, this lock can be ‘gone’, the valve
being closed. Reopen the valve in that case – and readjust / repair the lock!

The Head Condenser is cooled by air (Overhead Air Cooler)

Start immediately an other Air Cooler (Several Air Cooler, including Stand-by ones
equip generally a unit). Then make enquiring about the (initial) fault.
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If condensers are not involved, it is probably a fault in temperature control loops of the
column.

First, then, verify the control loop of reflux drum done by a TIC fitted on the drum inlet (or
on the drum itself). And controlling two TCV. One controlling the distillate flow in the
condenser, the second bypassing the same condenser. If the bypass TCV is blocked
open, there is no possibility for condensation; take it in ‘manual control’ and close it
completely for the distillate to pass (in totality) through the other

In opposite, if it is the inlet TCV which is blocked (closed), take it in ‘manual control’ and
open it (full open) for the distillate to go inside the Condenser. Once the level is back to
normal, call instrumentation maintenance.

Other source of trouble: Head of Column Temperature too high and Condenser is not
powerful enough to condense even partially the distillate. Verify and decrease the reboiler
heating to avoid accumulation of heavy components in Column Head.

12.5. LOSS OF COOLING WATER

This is a different cause than the one pointed out here above, indeed this is loss of Cooling
Water to the overhead condenser by Mechanical breakdowns of pumps or losses of power
may result in loss of cooling water.

Cooling water removes heat from the system. The liquid that leaves the condenser is
divided into two streams. One stream is drawn off as overhead product and the other is
returned as reflux. If cooling water is lost and nothing is done to remedy the problem, then
equipment becomes damaged.

Loss of cooling water causes overheating in the condenser, and overheating can damage
the cooling coils.

Immediately Cut Off the heating medium on the reboiller

Then if present, by-pass the Feed / bottom product exchanger & the heating of the
Furnace

Wait for the restore of Cooling Water

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13. GLOSSARY
API Gravity
Unit used to measure density, given in °API.

Batch Distillation
The operation of a still by putting in a batch of mixture, vaporizing part of the mixture, and
draining off the part that is left. Also called unsteady state distillation.

Condensation
When more molecules are entering the liquid from the vapour phase than are escaping the
liquid.

Centigrade
Unit used to measure temperature, in °C. in the International System SI

Cracking
Breaking large, complex hydrocarbon molecules into smaller molecules; a chemical
reaction.

Cut
Fraction of oil that contains similar types of hydrocarbons.

Density
Mass of a substance per unit of volume, or, the heaviness of a substance. Often
measured in pounds per cubic foot.

Distillation
The process by which the components of a liquid mixture are separated by partially
vaporizing the mixture, and collecting and condensing the vapours. Also called
fractionation.

Down-comer
Tray component that allows the liquid to flow from one tray of the column downward to the
next tray.

Enrichment
The process by which a mixture becomes richer in one of its components.

Equilibrium
The point at which equal numbers of molecules pass between the liquid and the gas
phase.

Evaporation
When more molecules are escaping a liquid than returning to it.
The opposite of condensation.

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Fahrenheit
Unit used to measure temperature, °F in the British system

Fractionation
Separation of mixtures of hydrocarbons without affecting their structure; a physical
process. Also called distillation.

Gas
State of matter in which molecules are in random and chaotic motion. Also called vapour.

Heat
Form of energy, specifically thermal energy.

Hydrocarbons
Molecules composed solely of hydrogen and carbon atoms.

Immiscible
Liquids that do not mix, like gasoline and water. Kelvin
Unit used to measure temperature; an absolute scale in °K.

Latent Heat
Heat added to a material that does not change its temperature.

Miscible
Liquids that readily mix.

Multiple Stills
Any combination of two or more stills (Columns) operating together with continuous feed.

Partial Pressure
When two or more gases are mixed, the separate pressures of the gases are called partial
pressures. The total pressure of a gaseous mixture is equal to the sum of the partial
pressures.

Rankin
Unit used to measure temperature; an absolute scale in °R.

Rectifying Section
The section of a distillation column above the feed.

Reflux
The cooled and condensed vapours that are re-introduced as liquid, and allowed to run
back down the columns. Used to establish a level of liquid on the top tray and to help
control the temperature of the trays.

Reforming
Atoms or groups of atoms that are added, removed, or rearranged to result in different

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hydrocarbon molecules with higher octane ratings; the restructuring of hydrocarbon

molecules.

Risers
The vertical chimneys that let vapours rise through the trays in the distillation column.

Sensible Heat
Heat that raises the temperature of a substance.

Specific Gravity
The heaviness of one substance in relation to another substance.

Stripping
The process of removing the lighter component from a mixture, leaving the heavier
component relatively pure.

Stripping Column
A separate still that strips the light vapours from a mixture.

Stripping Section
The section of a distillation column below the feed.

Vaporize
To convert into vapour by the application of heat.

Vapour Pressure
A measure of a liquid's tendency to vaporize at a given temperature.

Viscosity
A measure of thickness or ability of fluidity, or, ability of a liquid to flow.

Volatility
Refers to the ease at which a liquid vaporizes. Liquids with high volatility vaporize easily
and are in the Carbon Number scale from C6 up to C8
Liquids with low volatility do not vaporize easily; they begin with C9+ in the Carbon
Number scale

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14. SUMMARY OF FIGURES

Figure 1 : Sketch of thermal account principle ...................................................................10
Figure 2: Distillation unit for crudes (Topping) ...................................................................12
Figure 3: Schematic diagram of a two-component unsteady state distillation....................14
Figure 4: Schematic diagram of a two-component Steady State distillation.......................15
Figure 5: Diagram of the configuration of a three-phase three-condenser distillation ........16
Figure 6: Configuration diagram of a three-phase distillation with one condenser.............17
Figure 7: Schematic diagram of a Stripping column ..........................................................19
Figure 8: Diagram of the distillation of a Pentane / Hexane mixture ..................................20
Figure 9: Operating diagram of a column section ..............................................................21
Figure 10: Diagram of two-component (C5 & C6) distillation .............................................22
Figure 11: Fractionation of crude oil ..................................................................................24
Figure 12: Diagram assembly for distillating crude oil & fractionating cuts ........................24
Figure 13: Photo showing what happens on a tray ............................................................25
Figure 14: Bubble cap tray.................................................................................................29
Figure 15: Bubble caps ......................................................................................................29
Figure 16: Bubbles.............................................................................................................29
Figure 17: Vapour passing through a bubble cap tray .......................................................30
Figure 18: Overflow weir ....................................................................................................31
Figure 19: Tray gradient.....................................................................................................31
Figure 20: Overflow weir ....................................................................................................32
Figure 21: S-section...........................................................................................................32
Figure 22: Ballast tray ........................................................................................................33
Figure 23: Nested caps......................................................................................................33
Figure 24: Side-to-side pan................................................................................................33
Figure 25: Packings ...........................................................................................................34
Figure 26: Berl saddle........................................................................................................34
Figure 27: Raschig rings ....................................................................................................34
Figure 28: Example of a reboiler........................................................................................39
Figure 29: Composition of a reboiler ..................................................................................39
Figure 30: Distillation equipment........................................................................................40
Figure 31: Baffles...............................................................................................................40
Figure 32: Condenser ........................................................................................................40
Figure 33: Distillation equipment........................................................................................41
Figure 34: Reflux distributors .............................................................................................42
Figure 35: Demister ...........................................................................................................43
Figure 36: Dew point and bubble point ..............................................................................46
Figure 37: Functional diagram of the reboiler loop (temperature control at tower bottom) 48
Figure 38: Pressure control diagram..................................................................................49
Figure 39: Bottom liquid level control diagram ...................................................................50
Figure 40: Diagram of a flow control loop at the inlet of a distillation column.....................51
Figure 41: Diagram of the main control parameters of a standard column ........................53

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15. CORRECTIONS FOR EXERCICES

1. Consider two liquids: Liquid A is composed of small molecules and Liquid B is
composed of large molecules. Which liquid has a lower volatility?

; Liquid B

Liquid B has a lower volatility than Liquid A.

B has lower vapor pressure than Liquid A. is heavier than Liquid A. & has a higher
boiling point than Liquid A.

2. To separate the components, only a portion of the mixture is vaporized. Then the
remaining liquid is drained off, and a new batch of mixture is put into the still. In which
component the liquid that is drained off is enriched?

; The heaviest component

During unsteady state distillation, as more pentane, the component with the lower
boiling point, is vaporized, the boiling point of the liquid must rise to maintain
vaporization. As the liquid mixture vaporizes, more pentane than hexane passes
into the vapors and can be partially vaporized later to achieve further separation of
the components.

3. As more pentane passes into the vapors, the remaining liquid is enriched in hexane.
Hexane has a higher boiling point than pentane, so the boiling point of the liquid must
rise to maintain vaporization. How are the conditions in the Still constantly changing or
always the same?

; Constantly changing

When the mixture is introduced into the still in one batch, the composition of the
liquid and the temperature of the liquid are constantly changing.
Because conditions in the still are constantly changing, the process is called
"unsteady state distillation".

4. The heat that is applied to the mixture in the reboiler vaporizes the liquid, and the
vapors are returned to the distillation column. Where do the hot vapors enter, at the
Top or at the Bottom?

; At the bottom

Vapors leaving the lowest tray pass upward in the same way through the next tray,
and the vapors leaving that tray pass through to the next tray above, causing the
liquid to boil. As these vapors give up heat to the liquid, some of the heavier
vapors condense. The vapors that condense and become part of the liquid are
primarily hexane.

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5. The heat supplied from the hot vapors to the liquid on the tray causes some of the
lighter liquid to vaporize and pass upward. Which is the component with the higher
percentage contained in vapors than in the remaining liquid?

Pentane

The liquid removed from the bottom (the liquid stream) is relatively pure in hexane.

6. The stripping section, which strips the lighter component from the heavier, leaving the
heavier component relatively pure, is above the feed or below the feed ?

; Bellow the feed

Adding separation stages above the feed can produce an overhead product
relatively pure in the lighter component.

7. If the temperature on a tray at the bottom of Section B is 640° F, the temperature on a

tray at the top of Section C is:

; 240°F

Because due to the nature of components which become more & more lighter as
rising in the column their boiling point is lower & lower thus their temperature

8. Which one has a distributor?

; Weir B

While the distributor weir helps to distribute liquid on the tray, the overflow weir
helps maintain the level of liquid on the tray.

9. For good fractionation, the vapor velocity must be:

; Moderate

If the rate is too slow, the bubbles will be too large. If the rate is too fast, there is
too little contact. Also, if the teeth or slots are dirty, fractionation will be poor
because the vapor flow is obstructed.

10. Which tray is designed to work with variable flow S-section?

; Ballast?

The ballast tray is similar to a bubble cap tray, but is more adaptable to variation in
throughput.

11. In which cases the packed towers are very efficient: when vapor and liquid are
distributed throughout the tower evenly or unevenly?

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; Evenly

Efficiency is impaired when areas or channels open up where liquid or vapor is

able to travel through the tower without making contact.

12. If a tower does not use trays, it is called a:

; Packed tower

In all towers, the purpose of trays or packing is to provide efficient vapor-liquid

contact.

13. The reboiler vapors returning to the tower contain the heaviest or the lightest fractions?

; The lightest fractions

Part of this heavy liquid is drawn off to a reboiler where the lightest fractions are
vaporized and fed back to the tower.

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