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Distillation Basics

Basics

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Distillation - Introduction

What Does Distillation mean:

A process that uses heat to separate two or more substances in a liquid

mixture. This separation accomplished by vaporizing substances and
separating based on individual component vapor pressure.

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Distillation - Introduction

• Distillation is based on the fact that the vapour of a boiling mixture will be richer in the
components that have lower boiling points.So when this vapour is cooled and condensed,
the condensate will contain more volatile components. At the same time, the original
mixture will contain more of the less volatile material.

• Distillation columns are designed to achieve this separation efficiently.

Salient features of Distillation Process:

• Distillation is the most common separation technique

• It consumes enormous amounts of energy, both in terms of cooling and heating

• Requirements

• It can contribute to more than 50% of plant operating costs

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Distillation Principle

• Separation of components from a liquid mixture via distillation depends on the

differences in boiling points of the individual components.

• Also, depending on the concentrations of the components present, the liquid mixture
will have different boiling point characteristics.

• Therefore, distillation processes depends on the vapour pressure characteristics of

liquid mixtures.

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Distillation Principle

Vapour Pressure and Boiling:

The vapour pressure of a liquid at a particular temperature is the equilibrium pressure

exerted by molecules leaving and entering the liquid surface.

Some important points:

• energy input raises vapour pressure
• a liquid is said to ‘boil’ when its vapour pressure equals the surrounding pressure
• the ease with which a liquid boils depends on its volatility
• liquids with high vapour pressures (volatile liquids) will boil at lower temperatures
• the vapour pressure and hence the boiling point of a liquid mixture depends on the
relative amounts of the components in the mixture
• distillation occurs because of the differences in the volatility of the components in the
liquid mixture

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Distillation Principle

Boiling Point Diagram:

•The boiling point diagram shows how

the equilibrium compositions of the
components in a liquid mixture vary with
temperature at a fixed pressure.

•Consider an example of a liquid mixture

containing 2 components (A and B) - a
binary mixture.

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Distillation Principle

Boiling Point Diagram:

•The boiling point of A is that at which the mole

fraction of A is 1. The boiling point of B is that
at which the mole fraction of A is 0.

•In this example, A is the more volatile

component and therefore has a lower boiling
point than B.

•The upper curve in the diagram is called the

dew-point curve while the lower one is called
the bubble-point curve.

•The dew-point is the temperature at which the

saturated vapour starts to condense.

•The bubble-point is the temperature at which

the liquid starts to boil.

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Distillation Principle

Boiling Point Diagram:

•The region above the dew-point curve shows the

equilibrium composition of the superheated
vapour while the region below the bubble-point
curve shows the equilibrium composition of the
subcooled liquid.

•For example, when a subcooled liquid with mole

fraction of A=0.4 (point A) is heated, its
concentration remains constant until it reaches
the bubble-point (point B), when it starts to boil.
The vapours evolved during the boiling has the
equilibrium composition given by point C,
approximately 0.8 mole fraction A. This is
approximately 50% richer in A than the original
liquid.

•This difference between liquid and vapour

compositions is the basis for distillation
operations. 9
Distillation Principle

Relative Volatility:

•Relative volatility is a measure of the differences in volatility between 2 components, and

hence their boiling points. It indicates how easy or difficult a particular separation will be. The
relative volatility of component ‘i’ with respect to component ‘j’ is defined as

Aij = (yi/xi) / (yj/xj)

yi = mole fraction of component ‘i’ in the vapour

xi = mole fraction of component ‘i’ in the liquid

•Thus if the relative volatility between 2 components is very close to one, it is an

indication that they have very similar vapour pressure characteristics. This means that
they have very similar boiling points and therefore, it will be difficult to separate the
two components via distillation.

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Distillation Principle

Vapor Liquid Equilibria:

•Distillation columns are designed based on the

boiling point properties of the components in the
mixtures being separated. Thus the height, of
distillation columns are determined by the
vapour liquid equilibrium (VLE) data for the
mixtures.

•Vapour-Liquid-Equilibrium (VLE) Curves

•Constant pressure VLE data is obtained from

boiling point diagrams. VLE data of binary
mixtures is often presented as a plot, as shown
in the figure.
This particular VLE plot shows a binary mixture that has
a uniform vapour-liquid equilibrium that is relatively •The
VLE plot expresses the bubble-point and
easy to separate.
the dew-point of a binary mixture at constant
pressure. The curved line is called the
equilibrium line and describes the compositions
of the liquid and vapour in equilibrium at some
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fixed pressure.
Distillation Principle

The above two VLE plots shows non-ideal systems which will present more
difficult separations.
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Distillation Principle

• The most intriguing VLE curves are generated by Azeotropic systems.

• An azeotrope is a liquid mixture which when vaporized, produces the same composition as the liquid.

• The two VLE plots above, show two different azeotropic systems, one with a minimum boiling point
and one with a maximum boiling point. In both plots, the equilibrium curves cross the diagonal lines,
and this are azeotropic points where the azeotropes occur

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Equipment classification & Detail

Equipment Classification & Detail

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Distillation - Types

Based on Mode of Operation:

•Batch Distillation
•Continuous Distillation

Batch Distillation:
In batch operation, the feed to the column is introduced batch-wise. That is, the column is
charged with a 'batch' and then the distillation process is carried out. When the desired
task is achieved, a next batch of feed is introduced. (Recovery col. in R & D Pilot Plant)

Continuous Distillation:
In contrast, continuous columns process a continuous feed stream. No interruptions
occur unless there is a problem with the column or surrounding process units. They are
capable of handling high throughputs and are the most common of the two types.

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Distillation - Column Types

Continuous Columns Type:

Based on Nature of Feed-

• Binary Column - Feed contains only two components
(VGR Col.-PP Plant)
• Multi- Component Column - Feed contains more than
two components (Cracker Plant- Quench tower)

Based on Number of Product Streams-

• Multi- Product Column - Column has more than two
product streams (Cruder Refinery columns)

Based on Use of Additional Component to help with

Separation-
• Extractive Distillation - Extra feed appears in the bottom
product stream
• Azeotropic Distillation - Extra feed appears at the top
product stream

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Distillation - Column Types

Continuous Columns Type:

Based on Type of Column Internals

•Tray Column - Trays of various designs are used to hold up the liquid
to provide better contact between vapour and liquid,
hence better separation

• Packed Column - Instead of trays, ’Packings' are used to enhance

contact between vapour and liquid

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Distillation - Main Components

• Shell : A vertical shell where the separation of liquid components is

carried out

• Trays / Packing : Column internals such as trays/plates and/or packings

which are used to enhance component separations

• Reboiler : A reboiler to provide the necessary vaporisation for the

distillation process

• Condenser : A condenser to cool and condense the vapour leaving the

top of the column

• Reflux Drum : A reflux drum to hold the condensed vapour from the
top of the column so that liquid (reflux) can be recycled
back to the column

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DISTILLATION COLUMN-PLATE COLUMN

General Information:

• Distillations are governed by differences in

relative volatility.

• (The relative volatility of a species reflects its

rate of evaporation.

• A more volatile component will evaporate

before a less volatile one).

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Distillation columns: Plate Columns: Equipment Design

• After the feed mixture enters the column, it flows

down the column and across the trays in either
cross-flow or counter-current flow.

• A reboiler at the bottom separates the stream into

a vapor stream that returns to the column, and a
liquid product stream.

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Distillation - Main Components

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Distillation - Basic Operation Terminology

• The liquid mixture that is to be processed is known as the feed and this is introduced
usually somewhere near the middle of the column to a tray known as the feed tray.

• The feed tray divides the column into a top (enriching or rectification) section and a
bottom (stripping) section.

• The feed flows down the column where it is collected at the bottom in the reboiler.

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Distillation - Basic Operation Terminology

• Heat is supplied to the reboiler to

generate vapour. The source of heat
input can be any suitable fluid, although
in most chemical plants this is normally
steam. In refineries, the heating source
may be the output streams of other
columns.

• The vapour raised in the reboiler is re-

introduced into the unit at the bottom of
the column. The liquid removed from the
reboiler is known as the bottoms product
or simply, bottoms.

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Distillation - Basic Operation Terminology

• The vapour moves up the column,

and as it exits the top of the unit, it
is cooled by a condenser.

• The condensed liquid is stored in a

holding vessel known as the reflux
drum. Some of this liquid is
recycled back to the top of the
column and this is called the
reflux.

• The condensed liquid that is

removed from the system is known
as the distillate or top product.

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 DISTILLATION COLUMN-Packed Columns
Vapour

Internal Distributor
Feed
Packed Columns :
Liquid spray
Advantages:
Packings
Packing restrainer  Higher gas – liquid interaction
 Increase in column capacity
Side draw
 Lower pressure drops.
Side  For highly corrosive liquids
Stream
Disadvantage:
 Possibility of channeling higher
Packing support
tray  Multiple beds preferable
 Dead zones possible

Collection tray
Packings used during DBN to
increase capacities
Bottoms 25
DISTILLATION COLUMN – Packed column

Packings:

•Increase the interfacial area for vapour-liquid contact.

•Structured packings are easy to handle and install.
•Random packings normally dumped into column – susceptible to channeling, but
cheaper.

Types:
Structured - Random -

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 Distillation columns: Tray Columns

Vapour Condenser

Distillate Tray columns:

• Feed entry mostly through the
middle section
Cooling
Feed
Differential Liq- Vapour separation takes
Temperature place on the trays:
Trays • Distillate removed from top of
column after condensation
Heating
• Heaviers removed from bottom
• Heat required for separation
supplied by reboiler

Liquid
Reboiler
Bottoms
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Column Internals

Vapours bubble through liquid maintained on

the tray.
A weir on the tray ensures that there is always
some liquid(holdup) on the tray such that bubbling
takes place.

Downcomers are used to ensure movement of

liquid overflow to the tray below without affecting
the equilibrium on that tray.

A liquid distributor is used to uniformly distribute

the feed if the column is large

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Distillation columns: Tray Columns

Factors that affect extent of distillation:

• Column dimensions and no. of passes

• Tray type and design
• Feed entry point
• Condenser capacity and efficiency
• Reboiler capacity and efficiency

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 Distillation columns: Tray Columns

Number of passes defines the efficiency of separation as the contact area for mass
transfer is increased

Single Pass:
Liquid flows across the trays only once.
Vapours pass vertically, bubbling
Tray through the liquid

Downcomer

Vapour

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Cross flow

Counter-current flow

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Distillation columns: Plate Columns: Equipment Design

• The geometry of the trays within the column affects the extent and type of contact
between the vapor and liquid streams to achieve as complete a separation as
possible. The different tray types include sieve, valve and bubble cap.
• Down comers channel the liquid flowing from one tray down to the tray below .

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Sieve Tray

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Lift Valves

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Cap Covers

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Distillation Columns: Plate Column: Adv./Dis.

Advantages:

•Least expensive distillation column for diameters greater than 0.6 m.

•The liquid/vapor contact in the cross-flow of plate columns is more effective than the
counter current-flow in packed columns.

•Cooling coils can easily be added to the plate column.

•Can handle high liquid flow rates cost-effectively

Disadvantages:

•Higher pressure drops than packed columns

•Foaming can occur because the liquid is agitated by the vapor flowing up through it.

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Type of Reboiler

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Type of Reboiler

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Type of Reboiler

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Factors Affecting Distillation Column Operation

• Feed Conditions: The state of the feed mixture and feed composition affects the
operating lines and hence the number of stages required for
separation. It also effects the location of the feed tray.

• Vapour Flow Conditions: Adverse vapour flow conditions can cause :

• Foaming: refers to the expansion of liquid due to passage of vapour or gas, leading
to liquid buildup on trays.

• Entrainment: refers to the liquid carried by vapour up to the tray above and is again
caused by high vapour flow rates. It is detrimental because tray
efficiency is reduced: lower volatile material is carried to a plate
holding iquid of higher volatility.

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Factors Affecting Distillation Column Operation

•Weeping: caused by low vapour flow. The pressure exerted by the vapour is
insufficient to hold up the liquid on the tray. Therefore, liquid starts to
leak through perforations.

•Dumping: Excessive weeping will lead to dumping. That is the liquid on all trays
will crash (dump) through to the base of the column (via a domino
effect) and the column will have to be re-started.

•Flooding: is brought about by excessive vapour flow, causing liquid to be

entrained in the vapour up the column. The increased pressure from
excessive vapour also backs up the liquid in the downcomer, causing
an increase in liquid holdup on the plate above. Flooding is detected by
sharp increases in column differential pressure and significant decrease
in separation efficiency.

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Factors Affecting Distillation Column Operation

• Column Diameter: Vapour flow velocity is dependent on column diameter. Thus, if

the column diameter is not sized properly, the column will not perform well. Not only
will operational problems occur, the desired separation duties may not be achieved.

• State of Trays and Packing: Any factors that cause a decrease in tray efficiency will
also change the performance of the column. Tray efficiencies are affected by fouling,
wear and tear and corrosion, and the rates at which these occur depends on the
properties of the liquids being processed.

• Weather Conditions: Most distillation columns are open to the atmosphere. Although
many of the columns are insulated, changing weather conditions can still affect
column operation.

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Operation

Operation

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Distillation - Column Operation

The performance of Distillation is determined by following factors:

•Feed Condition

•Reflux Condition

•Vapour Flow Condition

•Column Diameter

•State of Trays and Packings

• Weather Conditions

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Distillation - Column Operation

Feed Condition:

•The state of the feed mixture and feed composition affects the operating lines and hence
the number of stages required for separation.

•It also affects the location of feed tray.

•During operation, if the deviations from design specifications are excessive, then the
column may no longer be able handle the separation task.

•To overcome the problems associated with the feed, some column are designed to have
multiple feed points when the feed is expected to containing varying amounts of
components.

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Distillation - Column Operation

Reflux Condition:

•As the reflux ratio is increased more and more liquid that is rich in the more volatile
components are being recycled back into the column. Separation then becomes better and
thus less trays are needed to achieve the same degree of separation. Minimum trays are
required under Total Reflux conditions, i.e. there is no withdrawal of distillate.

•On the other hand, as reflux is decreased, the ‘Pinch’ between operating and equilibrium
lines becomes more pronounced and more and more trays are required.

•The limiting condition occurs at Minimum Reflux Ratio, when an infinite number of trays
will be required to effect separation. Most columns are designed to operate between 1.2 to
1.5 times the minimum reflux ratio because this is approximately the region of minimum
operating costs (more reflux means higher reboiler duty).

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Distillation - Column Operation

Vapour Flow Condition:

Adverse vapour flow conditions can cause-

• Foaming
• Entrainment
• Weeping/dumping
• Flooding

Foaming
• Foaming refers to the expansion of liquid due to passage of vapour or gas.
Although it provides high interfacial liquid-vapour contact, excessive foaming
often leads to liquid buildup on trays. In some cases, foaming may be so bad that
the foam mixes with liquid on the tray above.
• Whether foaming will occur depends primarily on physical properties of the liquid
mixtures, but is sometimes due to tray designs and condition. Whatever the
cause, separation efficiency is always reduced.

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 Distillation - Column Operation

Vapour Flow Condition:

Entrainment
Entrainment refers to the liquid carried by vapour up to the tray above and is again
caused by high vapour flow rates. It is detrimental because tray efficiency is reduced.
lower volatile material is carried to a plate holding liquid of higher volatility. It could also
contaminate high purity distillate. Excessive entrainment can lead to flooding.

Weeping/Dumping
This phenomenon is caused by low vapour flow. The pressure exerted by the vapour is
insufficient to hold up the liquid on the tray. Therefore, liquid starts to leak through
perforations. Excessive weeping will lead to dumping. That is the liquid on all trays will
crash (dump) through to the base of the column (via a domino effect) and the column
will have to be re-started. Weeping is indicated by a sharp pressure drop in the column
and reduced separation efficiency.

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Distillation - Column Operation

Vapour Flow Condition

•Flooding:
Flooding is brought about by excessive vapour flow, causing liquid to be entrained in the
vapour up the column. The increased pressure from excessive vapour also backs up the
liquid in the downcomer, causing an increase in liquid holdup on the plate above.
Depending on the degree of flooding, the maximum capacity of the column may be severely
reduced. Flooding is detected by sharp increases in column differential pressure and
significant decrease in separation efficiency.

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 Distillation - Column Operation

Column Diameter:
•Most of the factors mentioned earlier that affect column operation is due to vapour flow
conditions: either excessive or too low.

•Vapour flow velocity is dependent on column diameter. Weeping determines the minimum
vapour flow required while flooding determines the maximum vapour flow allowed, hence
column capacity.

•Thus, if the column diameter is not sized properly, the column will not perform well. Not
only will operational problems occur, the desired separation duties may not be achieved .

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Distillation - Column Operation

State of Trays and Packing:

•The actual number of trays required for a particular separation duty is determined by the
efficiency of the plate, and the packings if packings are used.

• Thus, any factors that cause a decrease in tray efficiency will also change the
performance of the column.

•Tray efficiencies are affected by fouling, wear and tear and corrosion, and the rates at
which these occur depends on the properties of the liquids being processed.

•Thus appropriate materials should be specified for tray construction.

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 Distillation - Column Operation

Weather Condition:
•Most distillation columns are open to the atmosphere. Although many of the columns are
insulated, changing weather conditions can still affect column operation.

•Thus the reboiler must be appropriately sized to ensure that enough vapour can be
generated during cold and windy spells and that it can be turned down sufficiently during
hot seasons. The same applies to condensers.

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Controls

Controls

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Process Parameters

Input Variables:
Manipulated variables:
• External reflux, L mol/min
• Heat Input to Reboiler, Qr

Disturbances
• Feed, F mol/min
• Feed composition, Zf

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Control Configurations

There are basically three types of control configurations:

•Feed forward control configurations

•Feed back control configurations

•Inferential control configuration

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Control Configurations

Feed Forward Control Configuration:

•It uses direct measurements of disturbances to adjust the values of the manipulated variables.
•Thisparticular configuratoin takes action BEFORE the disturbances have their effect on the
process.

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Control Configurations

Feed Back control configuration:

• It uses direct measurements of disturbances to adjust the values of the manipulated
variables.
• This particular configuration takes action AFTER the disturbances have their effect on
the process.

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Inferential Control Configuration:

Inferential Control Configuration:

It makes use of Secondary Measurements to adjust the values of manipulated
variable. This is because in some cases, control variable cannot be measured directly.

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Distillation - Control System

General Control Strategies

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Troubleshooting

Troubleshooting

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Distillation - Troubleshooting

Importance:
• Stable operation to get the equilibrium

Effect of:
• Change in Feed rate
• Change in Feed composition
• Change in Feed temp.

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Distillation - Troubleshooting

Importance:
• Stable operation to get the equilibrium

Effect of:
• Change in Temperature profile
• Change in Reboiler functioning
• Change in Condenser functioning

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Distillation - Troubleshooting

Importance:
• Stable operation to get the equilibrium

Effect of:
•Malfunction of feed control valve

•Malfunction of reflux control valve

•Malfunction of steam control valve

•Malfunction of temp. sensor

•Malfunction of DP indication

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Commissioning - Decommissioning

Commissioning - Decommissioning

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Distillation - Commissioning

Steps Involved:
• Leak Test by Soap Solution at 3.5 Bar
• Hold Test
• Oxygen Removal
• Lining Up Feed to the column
• Lining Up condensate to Reboiler
• Lining Up cooling media to Condenser
• Stabilizing column on Total Reflux
• Taking forward feed after stabilization

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Distillation - Decommissioning

Steps Involved:
• Cooling of the Column

• Draining of the column and Reflux Drum

• Purging till LEL is nil.

• Blinding

• Manhole Opening

• Increasing Oxygen Concentration

• Ready for Vessel Entry

• Inspection

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Distillation - Decommissioning

Locations for Isolation

Condenser

Feed

Reflux
Reflux Drum

Heating Medium Distillate

Reboiler Bottom

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Thank You

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