Lecture 10 : SYNTHESIS OF SEPARATION SYSTEM HOMOGENOUS MIXTURE SEPARATION

After separating the heterogenous mixture, attempt can then be made to separate the homogenous
mixture produced from the reaction.
This is a harder separation !
Remember from your earlier courses in separation !
We need to create or add an extra phase in order to perform the separation.
Most common example : Distillation, Liquid Extraction,
Super Critical Fluid Extraction etc...

Some guidelines to consider !

1

There used to be a preferred rule long practised by industry whereby

distillation was given the first priority as chosen method for separating
homogenous mixture. Now, it is used as a benchmark against other methods.

In sequencing the separator for homogenous mixture, a guide which

can be used is to develop/design the sequence which consumes the least
energy for the required separation.

To illustrate the guidelines .

First choice !

What circumstances ? Discuss !

ABSORBER

if cannot perform
separation or
economically
unattractive

ADSORBER

Extraction

DISTILLATION

MEMBRANE

Liquid-Liquid
Solid-Liquid

2
Sequence preferred should be
the sequence that has highest
energy efficiency.
HOW ?

Eg. For distillation, assess the

vapour flow required for the entire
separation

Circumstances not favouring distillation

1. Separation of low molecular wt. materials
2. Separation of high molecular wt. heat sensitive material.
3. Separation of components with low concentration.
4. Separation of classes of components

Multi-component distillation

How many distillation columns are required?

One distillation column can be optimized to separate one
pair of volatile components.
D, xD,1

F
zF,1
zF,2

We can specify two fractional recoveries:

FR1 = (DxD,1)/(FzF,1) = 0.95
FR2 = (BxB,2)/(FzF,2) = 0.98

If the feed contains more than two volatile components,

we cannot specify the recoveries of the additional
components.
However, we can add more distillation columns.
B, xB,1

Key components
Each column is designed to separate two components of adjacent relative
volatility. These components are the keys.
All other components are non-keys.
component

design for
separation

designation

1.5 Light non-key (LNK)

assume exclusively in distillate

1.4 Light key (LK)

specify recovery in distillate

1.3 Heavy key (HK)

specify recovery in bottoms

1.2 Heavy non-key (HNK)

assume exclusively in bottoms

1.0 Heavy non-key (HNK)

Distributions in the distillate and bottoms streams are specified for the two
key components.
If we assume that the non-keys do not distribute, the overall mass balance
is easily solved.

Stages of Calculation for the Short Cut (FUG) Method for the multicomponent distillation
i. Calculation of Minimum Number of Stages using Fenske Equation.

Nmin Minimum no. of

stages at total reflux

Geometric average of the

relative volatility between light
key (LK) to heavy key (HK) at
the top and bottom of column.

Short Cut Design Method for Distillation Column for multi-component separation
Stages of Calculation for the Short Cut Method.
ii. Calculation of component distribution using Fenske equation.

di
log m log a ij C
bi

Log (di/bi)

Log (di/bi) for LK

di
Log (di/bi) for HK

bi

aHHK aHK

aLK

aLLK

Log (aij)

Short Cut Design Method for Distillation Column for multi-component separation
Stages of Calculation for the Short Cut Method.
ii. Calculation of component distribution using Fenske equation.

1 +

di

bi

=
=

1 +
1 +

Example

Minimum number of stages (Nmin)

Minimum number of stages (Nmin)

Alternatively, Nmin can be obtained by using:

N min

d L bH
log .
d H bL

log a LH

Try yourself!!

Calculate component distribution

1 +

Calculate component distribution

Doing for the other components!!

Stages of Calculation for the Short Cut Method.

iii. Calculation of Minimum Reflux Ratio using Underwood Equation.
NC

i 1

a i , j xi , F
1 q
a i, j

Rmin 1

NC

i 1

a i , j xi ,D
a i, j

The equation is used to determine the

root which is then used to solve the
minimum reflux ratio equation.

q feed quality
ai,j relative volatility of component i
x i,F feed composition , x i,D Distillate composition

Calculating minimum reflux Rmin

Calculating minimum reflux Rmin

NC

i 1

a i , j xi , F
1 q
a i, j

What is the value of q?

Notice that when = 7.2487, the

summation is equal 0, therefore, this
is the answer!!!

Calculating minimum reflux Rmin

Rmin 1

NC

i 1

a i , j xi ,D
a i, j

Stages of Calculation for the Short Cut Method.

iv. Determination of Actual No of Stages based on Set Reflux Ratio (Gilliland Correlation)
The correlation was originally represented in graphical form before an empirical was developed.
Based on the calculated Rmin from Underwood equation, the X value is determined based on a set Reflux
Ratio R.

=
+1

Rmin is determined from Underwood Eqn.

Then a Y value is determined from the X value using the correlation below;

= 0.2788 1.3154 + 0.4114

0.2910

+ 0.8628 ln + 0.9020 ln +

The Y value obtained is then used to determined the number of stages N corresponding to the Reflux Ratio R
using the equation below based on the Nmin determined from Fenske Eqn.

=
+1

Stages of Calculation for the Short Cut Method.

The correlation allows for the determination of corresponding No. of Stages N required as the
Reflux Ratio R is varied from the minimum reflux ratio.
No. of Stages

x
x
x
x
x
x

Reflux Ratio

This will allow for the capital energy trade off to be investigated. (Discuss how it is being done?)

Calculating actual number of stages

=
+1

= 0.2788 1.3154 + 0.4114 0.2910

+ 0.8628 ln + 0.9020 ln +

Calculating actual number of stages

=
+1

Stages of Calculation for the Short Cut Method.

v. Determination of Feed Location

z B x
NR
log
0.206 log H . . B , L
NS
z L D xD , H

Kirkbride Equation

Ratio of the no. of stages in

rectifying to stripping section.

ZH and ZL mole fraction of heavy and light key respectively in feed.

XB,L and XD,H mole fraction of light key in bottom product and heavy key in top product respectively.
B and D molar flow of bottom product and distillate.

Example for Short Cut method calculation

Given the separation specified below;

Component

Xfeed

Distillate Flow

Bottom Flow

Mean Relative
Volatil1ity

Propane
i-Butane
n-butane
i-pentane
n-pentane

0.05
0.15
0.25
0.20
0.35

5
14.9
24
1
0.4

0
0.1
1
19
34.6

5
2.6
2.0
1
0.85

45.3

54.7

Total

The separation cut is between n-butane and i-pentane

Determine the minimum number of stages and minimum reflux ratio.

Solution
Calculate the minimum no of stages using Fenske eqn.

24 19
log .
1 1 8.8
N min
log 2

Solution
Calculate the minimum Reflux Ratio using Underwood Eqn. (Assume sat. liq and therefore q = 1)
i. Determine the root of Underwood equation value.
NC

i 1

a i , j xi , F
1 q
a i, j

Component

a i . zi
ai-

a i . zi

= 1.5
Propane
i-butane
n-butane
i-pentane
n-pentane

0.25
0.39
0.50
0.20
0.30
Sum

= 1.3

= 1.35

0.071
0.355
1.0
-0.4
-0.462

0.068
0.30
0.714
-0.667
-0.667

0.068
0.312
0.769
-0.571
-0.600

0.564

-0.252

-0.022

Close enough, take value = 1.35

Solution
ii. Using the calculated root of the Underwood equation , determine Rmin.

Rmin 1
Component

NC

i 1

a i , j xi , D
a i, j
a i . xDi
ai-

x Di

= 1.35
Propane
i-butane
n-butane
i-pentane
n-pentane

0.15
0.69
1.66
-0.06
-0.02

0.11
0.33
0.53
0.02
0.01
Sum

Therefore Rmin = 1.42

2.42

= Rmin + 1

Exercise

Distillation of multicomponent mixtures

1

Alternative?
1

1,
2

II

2
2,3,4

F
zF,1
zF,2
zF,3
zF,4

3
3,4

3, 4

III
Separation of C components requires (C-1)
distillation columns.

Heuristic for distillation column

sequencing
Heuristic 1. Separations where the relative volatility of the key
components is close to unity or that exhibit azeotropic
behavior should be performed in the absence of nonkey
components. In other words, do the most difficult separation
last.
Heuristic 2. Sequences that remove the lightest components
alone one by one in column overheads should be favored. In
other words, favor the direct sequence.
Heuristic 3. A component composing a large fraction of the
feed should be removed first.
Heuristic 4. Favor splits in which the molar flow between top
and bottom products in individual columns is as near equal as
possible.

Sequencing using minimum vapour flow

Use short cut method to determine minimum reflux ratio for specified separation
UNDERWOOD EQUATION
Comparison is based on a consistent basis : infinite no. of stages
Calculate vapour flow for each required separation (as specified) in every alternative
sequence. Go for the sequence with the least total vapour flow.

DISTILLATION

DISTILLATION

DISTILLATION

DISTILLATION

DISTILLATION
DISTILLATION

calculate vapour flow

for each column !

Use the Underwood Equation

We will look at this in more detail later

Example on Distillation Sequencing

Given the mixture to be separated;

Component

Xfeed

Feed Flow

Relative Volatil1ity

A - Propane
B - i-Butane
C - n-butane
D - i-pentane
E - n-pentane

0.05
0.15
0.25
0.20
0.35

45.4
136.1
226.8
181.4
317.5

8.09
3.49
2.68
1.23
1.00

Total

907.2 kmol/hr

Each component is to be separated with a specification of 99 %. Assume that the non key
component will not distribute but end up either at the top or bottom depending on their relative
volatility compared to the key component.
Determine the best sequence(s).

Example on Distillation Sequencing

The possible sequences are :

A/BCDE

AB/CDE

B/CDE

C/DE
CD/E

D/E
C/D

BC/DE

B/C

D/E

BCD/E

BC/D

B/C

B/CD

C/D

C/DE

D/E

CD/E

C/D

AB/C

A/B

D/E

A/BC

B/C

D/E

AB/CD

A/B

C/D

A/BCD

B/CD

C/D

BC/D

B/C

A/BC

B/C

AB/C

A/B

A/B

ABCDE
ABC/DE

ABCD/E

ABC/D

Example on Distillation Sequencing

For each of the column, we need to calculate the
minimum vapour flow using Underwood Eqn.
A/BCDE

AB/CDE

B/CDE

C/DE
CD/E

D/E
C/D

BC/DE

B/C

D/E

BCD/E

BC/D

B/C

B/CD

C/D

C/DE

D/E

CD/E

C/D

AB/C

A/B

D/E

A/BC

B/C

D/E

AB/CD

A/B

C/D

A/BCD

B/CD

C/D

BC/D

B/C

A/BC

B/C

AB/C

A/B

A/B

ABCDE
ABC/DE

ABCD/E

The minimum vapour flow for each column in the

sequence is added up to give the total minimum
vapour flow for the sequence.

ABC/D

Example on Distillation Sequencing

Calculation done for some of the sequences
ABC/DE

AB/C

A/B

D/E

ABC
B

ABCDE

BC

Mixed Sequence
D

C
DE

S Vmin = 5584 kmol/hr

E

Example on Distillation Sequencing

Calculation done for some of the sequences
A/BCDE

BC/DE

ABCDE

B/C

D/E

BC

C
D

DE

Mixed Sequence

S Vmin = 5670 kmol/hr

E

Example on Distillation Sequencing

Calculation done for some of the sequences
ABCD/E

AB/CD

A/B

C/D
A

AB

ABCD
B
C

Mixed Sequence

ABCDE

S Vmin = 5106 kmol/hr

CD

Example on Distillation Sequencing

Calculation done for some of the sequences
ABCD/E

ABC/D

AB/C

A/B
A

CD

ABC
B

Indirect Sequence

ABCD
C

ABCDE

S Vmin = 5188 kmol/hr

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 is a sequence. The sequence of these separators can be determined using
established methods such as the short cut method (Fenske-Underwood Equation) for distillation column