CDB3044 Process Plant Design Semester May 2019: Synthesis of Separation Systems (Homogeneous)

CDB3044 Process Plant Design
Semester May 2019

By Dr. Oh Pei Ching
➢ Synthesis of
Separation Systems
(Homogeneous)
1
Lecture Learning Outcome
▪ By the end of this lecture, you are expected to:
• Design distillation column for multicomponent
mixture
• Design the optimal sequencing of distillation

columns for separation of multicomponent mixture
• Make judgment and provide appropriate

specification for the operating parameter of
separation process
CDB3044 Process Plant Design 2

Separator for Homogeneous Fluid Mixtures
• The separation of a homogeneous fluid mixture requires the creation of
another phase or the addition of a mass separation agent.
• If homogeneous liquid mixture is partially vaporized, then another phase
is created, and the vapor becomes richer in the more volatile components
(i.e. those with the lower boiling points) than the liquid phase.
• The liquid becomes richer in the less volatile components.
• If the system is allowed to come to equilibrium conditions, then the
distribution of the components between the vapor and liquid phases is
dictated by vapor-liquid equilibrium considerations.
• A single equilibrium stage can only achieve a
limited amount of separation.
• Greater degree of separation will be achieved by
taking the vapor from the single-stage separation to
another separation stage and partially condensing
it and taking the liquid to another separation stage
and partially vaporizing it, and so on with repeated
condensation and vaporization. Vapor-liquid equilibrium

Figure 9.1 A cascade of equilibrium stages

with refluxing and reboiling
• It is assumed in the cascade that liquid and vapor
streams leaving each stage are in equilibrium.
• The more volatile components are transferred to the
vapor phase and the less volatile components are
transferred to the liquid phase.
• At the top of the cascade, liquid is needed to feed the
cascade. This is produced by condensing vapor that
leaves the top stage and returning this liquid to the first
stage of the cascade as reflux. This can be done by a
total condenser or a partial condenser.
• Vapor is also needed to feed the cascade at the bottom
of the column. This is produced by vaporizing some of
the liquid leaving the bottom stage and returning the
vapor to the bottom stage of the cascade in a reboiler.
• The feed is introduced at an intermediate stage, and
products are removed from the condenser and reboiler.
The methods by which vapor and liquid are contacted in each stage of
the cascade in distillation fall into two broad categories:
(a) Plate or tray column
(b) Packed column • Liquid enters the first plate at the
top of the column and flows across a
perforated plate.
• Liquid is prevented from weeping
through the holes in the plate by the
up-flowing vapor. In this way, the
vapor and liquid are contacted.
• The liquid from each
plate flows over a weir
and down a downcomer
to the next plate.
• Disadvantage of conventional tray
is the downcomer arrangement
(a) Conventional tray (b) High capacity tray makes a large area not available
Figure 9.2 Distillation trays for contacting liquid and vapor.

The methods by which vapor and liquid are contacted in each stage of
the cascade in distillation fall into two broad categories:
(a) Plate or tray column
(b) Packed column • The column is filled with a solid
material that has a high voidage.
• Liquid trickles across the surfaces of
the packing, and vapor flows upward
through the voids in the packing,
contacting the liquid on its way up
the column.
• Many different designs of packing
are available.
• The random packing is pieces of
preformed ceramic, metal or plastic.
• Structured packing is manufactured
(a) Random or dumped packing (b) Structured packing by sheets of metal being preformed
with corrugations and holes and
Figure 9.3 Distillation packing joined together in slabs and layers.
When trays are preferred
• Liquid flowrate is high relative to vapor flowrate

(occurs when the separation is difficult).
• Diameter of the column is large (packings can
suffer from poor distribution of the liquid over
the packing).
• There is variation in feed composition (trays can
be more flexible to variations in operating
conditions).
• The column requires multiple feeds or multiple
products (tray columns are simpler to design for
multiple feeds or products). (a) Conventional tray
Figure 9.2 Distillation trays

When packing is preferred
• Column diameter is small (relative cost for

fabrication of small-diameter trays is high).
• Vacuum conditions are used (packings offer lower
pressure drop and reduced entrainment tendencies).
• Low pressure drop is required (packings have a lower
pressure drop than trays).
• The system is corrosive (a greater variety of corrosion
resistant materials is available for packings).
• The system is prone to foaming (packings have a
lower tendency to promote foaming).
• Low liquid hold-up in the column is required (liquid (a) Random packing
holdup in packings is lower than that for trays). Figure 9.3 Distillation packing

General equilibrium stage for distillation
• Feed, vapor and liquid can enter

the stage.
• Additional product can be
withdrawn at intermediate stage
as liquid or vapor sidestream.
• Heat can be
transferred to or
from the stage.
Figure 9.4
1) Material balance for Component i and

Stage j (NC equations for each stage)
2) Equilibrium relation for each

Component i (NC equations for
each stage)
3) Summation equations (one for each stage)
Figure 9.4 General equilibrium stage

for distillation

4) Energy balance (one for each Stage j )
Figure 9.4 General equilibrium stage

for distillation
These equations require physical property data for
vapor-liquid equilibrium and enthalpies, and the set of
equations must be solved simultaneously 11
CDB3044 Process Plant Design
Binary Distillation
Overall material balance
Material balance for Component i
To simplify the analysis, it can be

assumed that the molar vapor and liquid
flow rates are constant in each column
section, which is termed constant molar
overflow. This is strictly only true if the
component molar latent heats of
vaporization are the same, there is no
Figure 9.5 Mass balance on a simple heat of mixing between the components,
distillation column heat capacities are constant and there is
no external addition or removal of heat.

Binary Distillation – Rectifying Section
Consider the part of the column above the feed
Figure 9.6 Mass balance for the rectifying section

Overall balance for the rectifying section
Material balance for Component i
Reflux ratio, R, is defined to be
Given the reflux ratio, the vapor flow can be

expressed in terms of R
These expressions can be combined to give an

Figure 9.6 Rectifying section of a
equation that relates the vapor entering and
column and the flows and compositions
liquid flows leaving Stage n
of the liquid and vapor

On an x–y diagram for Component i this is a straight

line starting at the distillate composition with slope
R/(R + 1) and which intersects the diagonal line at xi,D.
Starting at the distillate composition,

xi,D, a horizontal line across the
equilibrium line gives the
composition of the vapor in
equilibrium with the distillate (y1).
A vertical step down gives the liquid composition
leaving Stage 1 (x1).
Figure 9.6 x-y diagram
Another horizontal line across gives the composition
of vapor leaving Stage 2 (y2), etc.

Binary Distillation – Stripping Section
Consider the part of the column below the feed
Figure 9.7 Mass balance for the stripping section

Overall mass balance for the stripping section

around stage m + 1
Component balance
Equation relating the liquid entering and the

vapor leaving Stage m + 1
Figure 9.7 Vapor and liquid flows and

compositions through the stripping
section of a column

On an x–y diagram, this is a straight line with

slope L’/V’, which intersects the diagonal line at
xi,B.
Starting from the bottom composition, xi,,B, a

vertical line up to the equilibrium line gives the
composition of the vapor leaving the reboiler (yB).
A horizontal line across to the operating line gives
the composition of the liquid leaving Stage N (xN).
A vertical line up to the equilibrium line gives the
vapor leaving Stage N (yN), etc.
Figure 9.7 x-y diagram

Binary Distillation
The rectifying and stripping sections can be brought together at the feed stage.
Consider the point of intersection of the operating lines for rectifying and stripping sections.
From previous equations
Where yi and xi are the
intersection of the operating lines.
Subtracting gives
What happens at the feed stage depends on the condition of the feed (subcooled liquid,
saturated liquid, saturated liquid-vapor mixture, saturated vapor or superheated vapor).
To define the condition of the feed, the variable q is introduced:
q = 1 for saturated liquid;

q = 0 for saturated vapor

Binary Distillation
The flowrate of feed entering the column as liquid is
The flowrate of feed entering the column as vapor is
An overall mass balance on the feed stage for vapor gives
An overall mass balance on the feed stage for liquid gives
Relationship between compositions of feed and the

vapor and liquid leaving the feed tray:
This equation is known as the q-line.

On the x-y plot, it is a straight line with slope q/(q−1) and
Figure 9.8 Mass balance for the
intersects the diagonal line at xi,F
feed stage
Binary Distillation
• The material balances for the rectifying and
stripping sections can be brought together.
• The construction of Figure 9.9a is started by plotting
the operating lines for the rectifying and stripping
sections.
• The q-line intercepts the operating lines at their
intersection.
• The construction steps off between the operating
lines and the equilibrium lines.
• The intersection of the operating lines is the correct
feed stage, that is, the feed stage necessary to
minimize the overall number of theoretical stages. Figure 9.9(a) Combining the
• This method of design is known as the McCabe– rectifying and stripping sections
Thiele Method. – for optimum feed location
The McCabe–Thiele Method is restricted in its application because it only applies to binary
systems and involves the simplifying assumption of constant molar overflow. However, it gives
important conceptual insights into distillation that cannot be obtained in any other way.
Binary Distillation
(a) The optimum feed (b) Feed location below the (c) Feed location above the
location optimum stage optimum stage
Figure 9.9 Combining the rectifying and stripping sections
Figure 9.9b and c shows alternative stepping procedures which leads to a feed stage
location below or above the optimum feed stage. This results in an increase in the number
of theoretical stages.
Multicomponent Distillation
▪ In multicomponent distillation, decision must be made between the two key

components.
▪ The light key component is the one to be kept out of the bottom product
according to some specification.
▪ The heavy key component is the one to be kept out of the top product
according to some specification.
▪ The separation of the nonkey components cannot be specified.
▪ Lighter than light key components will tend to go predominantly with the
overhead product.
▪ Heavier than heavy key components will tend to go predominantly with the
bottoms product.
▪ Intermediate boiling components between the keys will distribute between the
products.
Fenske Equation
Consider total reflux conditions For total reflux
A component mass balance gives
Combining equations
Figure 9.13
Stripping If a binary separation (only A and B)
section of a
column under
total reflux
conditions
R refers to reboiler and B refers bottoms

As reflux conditions are total, the liquid composition in the reboiler is the same
as the bottom composition.
Combining equations
and gives
Similarly, the composition at Stage N–1 can be related to Stage N
Combining the above two equations

Figure 9.13 Stripping
section of a column under
total reflux conditions

Continuing up the column to the distillate
Assuming a total condenser and the relative

volatility to be constant gives
Fenske Equation
Predicts the number of
theoretical stages for binary
separation at total reflux
where
Nmin = minimum number of theoretical stages
Figure 9.13 Stripping
αAB = relative volatility between A and B
section of a column under
total reflux conditions D refers to the distillate

Fenske Equation can be written for a multicomponent system for any
two reference Components i and j
Where
xi,D = mole fraction of Component i in the distillate
xi,B = mole fraction of Component i in the bottoms
xj,D = mole fraction of Component j in the distillate
xj,B = mole fraction of Component j in the bottoms
αij = relative volatility between Components i and j
Nmin = minimum number of stages

Fenske Equation in terms of the molar flowrates of the products
Where
di = molar distillate flow of Component i
bi = molar bottoms flow of Component i
Fenske Equation in terms of recoveries of the products
Where
ri,D = recovery of Component i in the distillate
ri,B = recovery of Component i in the bottoms
rj,D = recovery of Component j in the distillate
rj,B = recovery of Component j in the bottoms

If component i is the light key component L, and j is the heavy key component H

Fenske Equation can be used to estimate the composition of the products
A plot of log [di/bi ] will be a linear function of log αij

with a gradient of Nmin
Where A and B are constants.

The parameters A and B are obtained by applying the
relationship to the light and heavy key components.

Overall component balance
Combining with
Resulting equations
Fenske Equation
and assumes that relative
volatility is constant.

The Underwood equations can be used to predict the minimum reflux for
multicomponent distillation.
The equations assume that the relative volatility and molar overflow are constant
between the zones of constant composition.
The first equation
where
αij = relative volatility
xi,F = mole fraction of Component i in the feed
θ = root of the equation
q = feed condition
heat required to vaporize one mole of feed
=
molar latent heat of vaporization of feed
= 1 for a saturated liquid feed
= 0 for a saturated vapor feed
NC = number of components
The second equation is then written for each value of θ obtained to determine the
minimum reflux ratio, Rmin
To solve this equation, it is necessary to know the values of not only αi,j and θ but also xi,D.
The values of xi,D for each component in the distillate in above equation are the values at the
minimum reflux and are unknown.
This procedure can be simplified significantly by making some reasonable assumptions
regarding the component distributions to approximate xi,D
It can be a good approximation to assume
• All of the lighter than light key components go to the overheads
• All of the heavier than heavy key components go to the column bottoms

Example 9.1
A distillation column operating at 14 bar with a saturated liquid feed of 1000 kmol/h is to
be separated into an overhead product that recovers 99% of the n-butane overhead and
95% of the i-pentane in the bottoms.
Table 9.1 Distillation column feed and relative volatilities
a. Calculate the minimum number of stages using the Fenske Equation

b. Estimate the compositions of the overhead and bottoms products using the Fenske Equation
c. Calculate the minimum reflux ratio using the Underwood Equations
• The actual number of trays required in the column will be greater than the
number of theoretical stages.
• Mass transfer limitations will prevent equilibrium being achieved on each tray.
• To estimate the actual number of trays, the number of theoretical stages must be
divided by the overall stage efficiency.
• This is most often in the range between 0.7 and 0.9, depending on the design of
the distillation tray.
• In practice, the number of trays is often increased by 5 to 10% to allow for
uncertainties in the design.
• The tray spacing is often taken to be 0.45 m or 0.6 m.
• Additional height of 1 m to 2 m needs to be added at the top of the column for
vapor disengagement and at the bottom of the column for vapor–liquid
disengagement for the reboiler return and a liquid sump.
• The column diameter is usually estimated with reference to the flood point for
the column.
• The flood point occurs when the relative flowrates of the vapor and liquid are
such that the liquid can no longer flow down the column.
The operating parameters to be considered by the designer include:

• operating pressure
• reflux ratio
• feed condition
• type of condenser
Limitations of Distillation
• Separation of materials with low molecular weight
• Separation of high molecular weight components (heat-sensitive materials)
• Separation of components with a low concentration
• Mixtures with low relative volatility or which exhibit azeotropic behavior
• Separation of mixtures of condensable and noncondensable components

Distillation Sequencing
If there is a three-component mixture to be separated into three relatively
pure products
Direct sequence in which the Indirect sequence, takes the

lightest component is taken heaviest component as bottom
overhead in each column product in each column

If the distillation columns have both reboiling and condensation supplied
by utilities, then the direct sequence requires less energy compared to
indirect sequence (as the light material is only vaporized once in the
direct sequence).
The indirect sequence can be more energy-efficient if the feed has a low
flowrate of the light material (Component A) and a high flowrate of
heavy material (Component C).
In this case, vaporizing the light material twice in the indirect sequence
is less important than feeding a high flowrate of heavy material to both
of the columns in the direct sequence.

Alternative sequences for the separation of a four-product mixture

Practical Constraints
• Safety considerations might dictate that a particularly hazardous

component be removed from the sequence as early as possible to
minimize the inventory of that material
• Reactive and heat-sensitive components must be removed early to
avoid problems of product degradation
• Corrosion problems often dictate that a particularly corrosive
component be removed early to minimize the use of expensive
materials of construction
• If thermal decomposition in the reboilers contaminates the product,
then this dictates that finished products cannot be taken from the
bottoms of columns.

Other Methods
Absorption and Stripping
• A gas mixture is contacted with a liquid solvent that preferentially dissolves one or
more components of the gas
CO2 Absorption and Stripping

Other Methods
Liquid–Liquid extraction
• Carries out separation by contacting a

liquid feed with another immiscible
liquid
• The liquid with which the feed is
contacted is known as the solvent
• The solvent extracts solute from the
feed
• The solvent-rich stream obtained from
the separation is known as the extract
• The residual feed from which the
solute has been extracted is known as
the raffinate.

Other Methods
Adsorption
• A process in which molecules of adsorbate become attached to the surface of a solid
adsorbent
2 broad classes:
Physical adsorption, in which
physical bonds form between the
adsorbent and the adsorbate.
Chemical adsorption, in which

chemical bonds form between the
adsorbent and the adsorbate.
Contacting arrangements for adsorber design

Other Methods
Membranes
Membranes act as a
semipermeable barrier between
two phases to create a
separation by controlling the
rate of movement of species
across the membrane
The feed mixture is separated

into a retentate, which is the
part of the feed that does not
pass through the membrane, and
a permeate, which is that part of
the feed that passes through the
membrane.
Flow patterns in
membrane separation

Other Methods
Crystallization
• Formation of solid
product from a
homogeneous liquid
mixture
Crystallizer

Other Methods
Evaporation
Evaporation separates a
volatile solvent from a Forward feed operation
solid
For larger capacity, it is

more usual to employ
multistage systems that Backward feed operation
recover and reuse
the latent heat of the
vaporized material
Parallel feed operation

In Summary,
For homogenous mixture separation,

distillation has always been preferred by
industry due to their established position
over other methods and their versatility
/flexibility in addressing range of feed
mixture.
As most reactor effluent mixture consist of

many components, the separation for the
individual components has to be done in a
sequence. The sequence of these separators
can be determined using established
methods such as the short cut method
(Fenske-Underwood Equations) for
distillation column.

THANK YOU
• © 2017 INSTITUTE OF TECHNOLOGY PETRONAS SDN BHD
• All rights reserved. No part of this document may be reproduced, stored in a retrieval system or transmitted in any form or by any means
(electronic, mechanical, photocopying, recording or otherwise) without the permission of the copyright owner.

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CDB3044 Process Plant Design

Semester May 2019

• Design the optimal sequencing of distillation

• Make judgment and provide appropriate

CDB3044 Process Plant Design 2

CDB3044 Process Plant Design 3

Figure 9.1 A cascade of equilibrium stages

CDB3044 Process Plant Design 5

• Liquid flowrate is high relative to vapor flowrate

CDB3044 Process Plant Design 7

• Column diameter is small (relative cost for

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• Feed, vapor and liquid can enter

1) Material balance for Component i and

2) Equilibrium relation for each

3) Summation equations (one for each stage)

Figure 9.4 General equilibrium stage

CDB3044 Process Plant Design 10

Figure 9.4 General equilibrium stage

Material balance for Component i

To simplify the analysis, it can be

CDB3044 Process Plant Design 12

Figure 9.6 Mass balance for the rectifying section

CDB3044 Process Plant Design 13

Material balance for Component i

Reflux ratio, R, is defined to be

Given the reflux ratio, the vapor flow can be

These expressions can be combined to give an

CDB3044 Process Plant Design 14

On an x–y diagram for Component i this is a straight

Starting at the distillate composition,

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Figure 9.7 Mass balance for the stripping section

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Overall mass balance for the stripping section

Equation relating the liquid entering and the

Figure 9.7 Vapor and liquid flows and

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On an x–y diagram, this is a straight line with

Starting from the bottom composition, xi,,B, a

CDB3044 Process Plant Design 18

q = 1 for saturated liquid;

CDB3044 Process Plant Design 19

An overall mass balance on the feed stage for vapor gives

An overall mass balance on the feed stage for liquid gives

Relationship between compositions of feed and the

This equation is known as the q-line.

▪ In multicomponent distillation, decision must be made between the two key

A component mass balance gives

CDB3044 Process Plant Design 24

Similarly, the composition at Stage N–1 can be related to Stage N

Combining the above two equations

CDB3044 Process Plant Design 25

Continuing up the column to the distillate

Assuming a total condenser and the relative

CDB3044 Process Plant Design 26

CDB3044 Process Plant Design 27

Fenske Equation in terms of recoveries of the products

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A plot of log [di/bi ] will be a linear function of log αij

Where A and B are constants.

CDB3044 Process Plant Design 30