DISTILLATION

SEQUENCING

Prepared by:
Qurat-ul-ain Rafiq (2010-MS-CH-32)
Sumreen Sabir (2010-MS-CH-20)
Contents:

• Definition
• Simple Columns
-Separation of multicomponent mixtures
-Practical constrains
-Heuristic rules
-Minimum -vapour flow
-Heat Integration
• Complex columns
-Columns with more than two products
-Sloppy Distillation
-Dividing wall column
-Thermal coupling
• Relationship between heat load and level
• Summary
Definition:

The sequence adopted to separate multicomponent

mixtures by distillation is called distillation
sequencing.
Distillation Sequencing Using Simple Columns:

Simple columns employ :

• One feed splits into distillate and bottoms (F  D + W).

• Key components adjacent in volatility.
• A reboiler and a condenser.
D

W
Simple Columns:
Separation Of Multicomponent Mixtures
Alternative separation sequencing in a ternary mixture.

1. Direct Sequence

The sequence in which

the lightest component
is taken overhead in
each column is the
Direct Sequence.
Simple Columns:
Separation Of Multicomponent Mixtures

Alternative separation sequencing in a ternary mixture.

2. Indirect Sequence

The sequence in which the heaviest

component is taken as bottom
product in each column is the
Indirect Sequence.
Simple Columns:
Heat Integration Within Ternary Separation System

1. Within Direct sequence

The pressure of the second column could be increased relative to
the first column to allow the condenser heat from the second
column to provide the reboiler heat for the first column.

2. Within Indirect sequence

The pressure of the first column could be increased relative to the
second column to allow the condenser heat from the first column to
provide the reboiler heat for the second column.
The Number Of Possible Distillation Sequences
For Multicomponent Mixtures

Number of Number of Possible

Components Sequences
2 1
3 2
4 5
5 14
6 42
7 132
8 429
Alternate Sequences For The Separation Of A Four-
component Mixture:
Simple Columns:
Practical Constrains

• Remove from the sequence as early as possible:

• Hazardous components.
• Reactive and heat-sensitive components.
• Corrosive components.
• Finished products must be taken from column distillates
(degradation, polymerization, additives, salts,...).
• Light components are normally removed from the top of the first
column to minimize the use of refrigeration and high pressures.
Simple Non-integrated Distillation Columns:
Heuristic Rules

Heuristic 1 Do the most difficult separation last.

Heuristic 2 Favor the direct sequence.

Heuristic 3 Large fraction components should be removed first.

Heuristic 4 Favor equimolar splits.

Example 1:
Flow Normal Relative
Components
rate Boiling αADJACENT
(kmol/h) Point(K) Volatility α

A. Propane 45.4 231 5.78

B. i.Butane 136.1 261 2.98 1.94
C. n.Butane 226.8 273 2.36 1.26
1.95
D. i.Pentane 181.4 301 1.21 1.21
E. n.Pentane 317.5 309 1.00

Heuristic 1: Do the most difficult separation last.

D/E
Heuristic 2: Favor the direct sequence.

A
B
C
D
E
 Example cont…..

Heuristic 3: Large fraction components should be removed first

A
B
C
D
E

Heuristic 4: Favor equimolar separation first.

A
B 408.3 kmol/hr
C
D 498.9 kmol/hr
E
 Example cont…..

Conclusion:

All heuristics are in conflict. The conflicts that have

arisen in this have not been helpful in identifying sequences that
are candidates for further evaluation. A little more intelligence
could be used in the application of the heuristics and they could
be ranked in order of importance. However, the rank order might
well change from process to process. Although in the above
example the heuristics do not give a clear indication of good
candidate sequences, in some problems they might. It does seem
though that a more general method than the heuristics is needed.
Simple Columns:
Minimum Vapour Flow

Influence on column costs and energy demand:

• Capital costs
• Diameter
• Condenser
• Reboiler

• Operating costs and energy demand

• Reboiler duty
• Condenser duty
 Minimum Vapour Flow Calculation:

• Underwood method

• Porter & Momoh method

Vmin= D(1 + Rmin)

RR
V Definition : RF 
RRmin
Condenser balance: V  D(1  RF RRmin )

F L D 1  xDLK xDHK 
Underwood equation : RRmin     
  1  xFLK xFHK 

1 xDLK 
xDHK  0  RRmin   1 F
  1 xFLK   RRmin 
   1D
LK balance : FxFLK  DxLDK 
W
 RF F  RF
V  D 1    D  F
 (  1) D   1
Example 2:
Components F (kmol/h) α αADJACENT
Benzene 269 3.53
1.96
Toluene 282 1.80
1.80
Ethyl Benzene 57 1.00

RF
Porter & Momoh: V  D  F
 1

1.10 
DIRECT V1  269  608  965 
1.96  1 
  V1  V2  1714 kmol/h
1.10
V2  282  339  748 
1.80  1 

1.10 
INDIRECT V1  551  608  1387 
1.80  1 
  V1  V2  2287 kmol/h
1.10
V2  269  551  900 
1.96  1 
 Example 3:
Determine The Best Sequence For The Following Mixture Of
Alkanes:

Assumption :

Ratio of actual to minimum reflux to be 1.1

Components Flow rate Normal Boiling Relative

αADJACENT
(kmol/h) Point(K) Volatility α
A. Propane 45.4 231 5.78
B. i.Butane 136.1 261 2.98 1.94
C. n.Butane 226.8 273 2.36 1.26
1.95
D. i.Pentane 181.4 301 1.21 1.21
E. n.Pentane 317.5 309 1.00
 Example cont…..

Total Vapour Flow For The 14 Possible Sequences

For The Separation Of A Mixture Of Alkanes:
 Example cont…..

Best Sequence With Respect To Heuristic :

Heuristic Rank Order Of

Sequence
1 3
2 5
3 10
4 1

The above table shows that best sequence is

obtained by the heuristic 4(favor near equimolar
splits).

It is not necessary that best sequence in all problems

Note: is always obtained by applying heuristic 4.
Heat Integration Of Sequences Of Simple Distillation
Columns:

1. Freshwater and Ziogou approach

2. Stephanopoulous , Linnhoff and Sophos approach

Non-Integrated
Costs

Integrated

Solutions
Conclusions:
• Two problems of separation sequencing and heat
integration can be decoupled.
• The best non integrated sequence turns out to be the
best few integrated sequences in terms of total cost
(capital and operating).
Internal Mass Flows In Sequences Of Simple
Distillation Columns
Compare two possible separation sequences ....
B
A A
B
ABC
ABCD BC
BC
ABCD
C
BCD
D C
D

 mK  A  2B  2C  D  mK  A  2B  2C  D

 mno  K  B  C  D  mno K  A  B  C
Effect Of Non-key Components Flow On Column
Operation:
•Larger liquid and vapour flows (capital & operating
costs, energy consumption).
•Lower condenser temperature
•Higher boiler temperature

Non-Keys
Σ(m)

Non keys

Keys

solutions

Look for minimum  FLOW non K !!

 Effect Of Flow Rates Of Non Key Components

1. On Condenser Temperature 2. On Reboiler Temperature

T T High ΣmΣm
High Non-keys
Non-keys
Low Σm Non-keys

High Σm Non-keys Low Σm Non-keys

Low Σm Non-keys

Q Q
Complex Columns:
Columns With More Than Two Products

Three products are taken from same column

Pure middle product is achieved by

1. Small flow of Heavy product

2. High flow of middle product
Complex Columns:
Columns With More Than Two Products

Pure middle product is achieved by

1. Small flow of light product

2. High flow of middle product
Complex Columns:
Sloppy Distillation

Three-product separation in which the

lightest and heaviest components are
chosen to be the key separation in the
first column. Two further columns are
required to produce pure products,
This arrangement is known as
distributed distillation or sloppy
distillation.
Complex Columns:
Prefractionator

The arrangement when the second

and third columns are operated at the
same pressure, then the second and
third columns could simply be
connected and the middle product
taken as a side stream .The
arrangement in is known as a
prefractionator arrangement.
 Complex Columns:
Thermal Coupling

Direct
Sequence

Prefractionator
Complex Columns:
Comparison Of Prefractionator With Direct Sequence

Prefractionator arrangement is more efficient because:

1. 30% less energy requirements.

2. Reduced mixing effects.
Complex Columns:
Thermal Coupling

The use of materials flow to provide some of the necessary heat

transfer by direct contact instead of using reboiler or condenser is
known as thermal coupling.
1. Thermal Coupling Of The Direct Sequence

Direct Sequence Thermally Coupled Side-Rectifier

Direct Sequence Arrangement
 Complex Columns:
Thermal Coupling

2. Thermal Coupling Of The Indirect Sequence:

Indirect Sequence Thermally Coupled Side-Stripper

Indirect Sequence Arrangement
Complex Columns:
Thermal Coupling

3. Thermal Coupling Of The Prefractionator:

Thermally coupled prefractionator requires extra plates to substitute

for the prefractionator condenser and reboiler.

Prefractionator Thermally Coupled Prefractionator

Petlyuk Column
Complex Columns:
Thermal Coupling

Dividing Wall Prefractionator:

Thermally coupled prefractionator

which uses a single shell with a
vertical baffle dividing the central
section of a the shell into two parts is
known as dividing wall column or
partition column.
Complex columns:
Dividing Wall Column
Advantages:

1.30 percent less energy consumption.

2.30 percent less capital cost.
3. The material is only reboiled once and its residence time in the high
temperature zones is minimized. This can be important if distilling
heat sensitive materials.

Disadvantages:

1.Heat supply at highest temperature and heat rejected at lowest

temperature.
2.Partition columns are not suited to replace sequences of two simple
columns that operate at very different pressures.
3.Material of construction.
Relationship Between Heat Load And Level In Simple
Column And Thermally Coupled Prefractionator:

Simple Column: A

A
1. High heat loads.
B B
2. More extreme levels. C
3. Freedom to choose the pressure of
two columns independently.

T
C

C2
C
1 Simple Column

H
Relationship Between Heat Load And Level In Simple
Column And Thermally Coupled Prefractionator:

Prefractionator:

1. Low heat loads B

2. More of the duties are at extreme levels. A
B
3. No freedom to choose the pressures.
C

C
T

Thermally Coupled Prefractionator

C2

H
Distillation Sequencing-Summary
Sequencing of simple distillation columns can be carried out in two
ways:

1. Identify the best few non-integrated sequences.

2. Study the heat integration.

There is no need to solve the problem simultaneously.

The best few non-heat-integrated sequences can be identified most

simply using the total vapor load as a criterion.

Complex column arrangements, such as the prefractionator and

thermally coupled arrangements, offer large potential savings in energy
compared to sequences of simple columns. Partitioned columns (or
dividing-wall columns) also offer large potential savings in capital cost.
Thank You