Separation

Department of Process & Systems Engineering
Synthesis of Separation System Dr Ade Lawal
Process Simulation and Design
Slide 1
Outline
Determination of the General Structure of the Separation System Synthesis of Vapour Recovery System Synthesis of Liquid Separation System
Slide 2
Determination of the General Structure of the Separation System
Slide 3
Phase of the reactor effluent stream

Purge
Feed streams
Reactor System
Separation Products System
Focus on reactor exit stream

Slide 4
When the reactor effluent is all liquid
Feeds
Reactor System
Liquid
Liquid Separation Products System
Liquid recycle
From Douglas, AIChE, 31: 353 (1985)

Slide 5
When the reactor effluent is a vapour and liquid mixture

Gas recycle Purge Vapour recovery system Liquid
Use the reactor as a phase splitter

Cooler Vapour Vapour Phase split Liquid
Send the liquid to the liquid separation system

Feeds Reactor system
Liquid
Cool the vapour and phase split it
Liquid separation Products system
Liquid recycle

Slide 6
When the reactor effluent is all vapour

Gas recycle Vapour recovery system Vapour Reactor system Vapour Cooler Phase split Liquid Liquid recycle Liquid separation system Liquid Purge
Feeds
Products

Slide 7
Phase split
Phase split is the cheapest method of separation
The phase split operation is preferred
Methods for obtaining a phase split

use cooling water pressurise the reactor system use both high pressure and a refrigeration partial condenser send the reactor effluent stream directly to a vapour recovery system
Slide 8
Synthesis of Vapour Recovery System

The best location of vapour recovery system The cheapest vapour recovery system
Slide 9
Possible Locations for Vapour Recovery System

The purge stream The gas-recycle stream The flash vapour stream None
Vapour stream Recycle stream Purge stream
Slide 10
Rules to locate the vapour recovery system

If significant amounts of valuable materials are being lost in the purge
Gas recycle
Purge
on the purge stream

Prevent recycle of certain components Prevent loss of valuable or undesirable material
If materials that are deleterious (harmful) to the reactor operation
on the gas-recycle stream
If both items are valid
Vapour from phase split
on the flash vapour stream
None
Neither item is important

Slide 11
Types of the Vapour Recovery System

Condensation process
high pressure or low temperature, or both
Absorption process Adsorption process Membrane separation process Reaction systems

[1] Douglas, 1988. [2] McCabe, etc.,1993 [3] Sinnott, 1999. [4] Geankoplis, 1993.
Slide 12
Absorption
Used to remove a solute from a gas mixture The solute is removed from
Water Air
the gas mixture by treatment with a liquid. The solute is absorbed from the gas phase into the liquid phase in absorption.
Air+ammonia
Water+ammonia Packed tower for absorption

Slide 13
Adsorption
Used to remove a
A
component from a gas or a liquid stream The component is adsorbed by a solid adsorbent. The remaining components can not be adsorbed
Solid adsorbent
A fluid (A+B)
Slide 14
Membrane Separation
Used to separate a solute from a fluid using a semipermeable membrane barrier The solute can pass through the membrane barrier, the remaining components can not.
A fluid (A+B)
Membrane barrier
Slide 15
Liquid Separation System
Slide 16
Decisions to synthesise the liquid separation system

How should light ends be removed if they might contaminate the product? What should be the destination of the light ends? What separations can be made by distillation? What sequences of columns do we use? How should we accomplish separations if distillation is not feasible?
Slide 17
Light Ends
.
Gas recycle Vapour recovery system Vapour Reactor system Vapour Phase split Liquid Liquid recycle Liquid separation system
Purge
Light ends
Feeds
Liquid
Products
Slide 18
Alternatives for Light-ends Removal

Light ends
Remove the light ends in a phase splitter
Use a partial condenser on the product column
Top Product
Use a stabiliser column before the product column
Light ends
To product column Slide 19
Destinations of the Light Ends

Gas recycle Purge
Vapour recovery system Vapour Feeds Reactor system Vapour Phase split Liquid Liquid recycle Liquid separation system Liquid
Waste treatment
Vent
Flare system
Fuel Light ends
Products
Slide 20
Distillation for Liquid-liquid Separation

Distillation is the cheapest separation method for separating liquid mixtures If the relative volatility of two components is less than 1.1, distillation becomes very expensive

A large reflux ratio A large column diameter A large condenser and a large reboiler Large steam and cooling water costs
Slide 21
Strategies for Distillation

Group components having a relative volatility of less than 1.1 and treat the group as one component Develop the best distillation sequence for the group and the other components Separate the lumped components by using other procedures A B,C B Other types of separations C
Lump
A B C D E
volatility 3.2 1.7 1.6 1.0 0.4 D,E
E Slide 22
Column Sequencing Simple Columns

A B A
A B C
A B C
C Option 1
C Option 2
Possible column sequences for a three-component mixture

Slide 23
Work Session1
How many simple columns are required to separate a fourcomponent feed? How many possible column sequences are there to separate a four-component feed?
Slide 24
The five sequences for a four-component feed

A B C A B A D
A B C D
B C D
C D D A A
A B C D B
B C D D
B C C A A
A B C D
A B
C D B D
A B C D D
A B C
B C C
A B C D D
A B C C
A B B
Slide 25
Column sequences for a five-component feed

1 2 3 4 5 6 7 8 9 10 11 12 13 14 Column 1 A/BCDE A/BCDE A/BCDE A/BCDE A/BCDE AB/CDE AB/CDE ABC/DE ABC/DE ABCD/E ABCD/E ABCD/E ABCD/E ABCD/E Column 2 B/CDE B/CDE BC/DE BCD/E BCD/E A/B A/B D/E D/E A/BCD A/BCD AB/CD ABC/D ABC/D Column 3 C/DE CD/E B/C B/CD BC/D C/DE CD/E A/BC AB/C B/CD BC/D A/B A/BC AB/C Column 4 D/E C/D D/E C/D D/E D/E C/D B/C A/B C/D B/C C/D B/C A/B
Slide 26
Number of alternatives
Number of components Number of columns Number of sequences
2 1 1
3 2 2
4 3 5
5 4 14
6 5 42
Slide 27
It will be a major task to decide which distillation column sequence to select for a particular process! Methods are required!
Slide 28
Methods to determine the best column sequence

Heuristic Method Mathematical Programming Method (Optimsation of chemical processes, Edgar,2001 & Analysis, Synthesis and Design of Chemical Processes, Turton 1998)
Slide 29
General Heuristics
Remove corrosive components as soon as possible
The special construction material is much more expensive than carbon steel if the corrosive components are present
Remove reactive components or monomers as soon as possible

Reactive components will change the separation problem Vacuum columns are required to separate monomers
Remove products as distillates
To avoid contamination of the product with heavy material
Remove recycle streams to a reactor as distillates
To avoid contamination of the recycle streams to reactors with heavy material
Slide 30
Column Sequencing Heuristics for Simple Columns

1. Most plentiful first (i.e. to remove the biggest amount first). 2. Lightest first. 3. Difficult separations last.
More heuristics refer to Tedder Rudd, AIChE J., 24: 303 (1978) Nishida, Stephanopoulos, and Westerberg, AIChE J., 29: 326 (1981) Malone, Glinos, Marquez, and Douglas, AIChE J., 31: 683 (1985)
Slide 31
Working Session 2
Use heuristics to determine a good sequence of simple distillation columns to separate the five hydrocarbons with 98% recoveries.
C3 98% recovery
iC4 98% recovery
Component pair C3/iC4
Approximate at 1 atm 3.6 1.5 2.8 1.35
Feed kmol/h 45.4 136.1 226.8 181.4 317.5
nC4 98% recovery
iC4/nC4 nC4/iC5
Propane (C3) IsoButane(iC4) n-Butane(nC4) i-Pentane(iC5) n-Pentane(nC5)

iC5 98% recovery
iC5/nC5
nC5 98% recovery

Slide 32
Solution
iC4
C3 iC4 nC4 nC4 C3 iC4 nC4 iC5 nC5 iC4 nC4 iC5 nC5 iC5 nC5 nC5
Component pair C3/iC4 iC4/nC4 nC4/iC5 iC5/nC5
Approximate at 1 atm 3.6 1.5 2.8 1.35
iC5
Slide 33
Column Sequencing Heuristics for Complex Columns

The heuristics for complex column sequencing can be found in Tedder and Rudd, AIChE J., 24: 303, 1978. Glinos and Malone,Chem. Eng. Res. Des., 1985.
Complex Columns (with side streams)
Slide 34
Heat integration in distillation columns Dividing wall columns
Slide 35
Is there an alternative to sequential arrangement of distillation columns?

A B
Column 2
volatility 3.2 1.7 1.3
Lump
A B C
Column 1
Almost pure B formed, but not isolated
Concentration of B
Alternative 1: Pre-fractionator + a column

A+ B A
Lump
A B C
volatility 3.2 1.7 1.3
B+C
This alternative has same number of columns + energy consumption is likely to be similar to the base configuration
Alternative 2: Thermally integrated column Dividing wall columns

A
Dividing wall
Lump A B C volatility 3.2 1.7 1.3 B
Pre-fractionation section
This alternative has one less column (but additional internals) + lower energy consumption (due to heat integration)
Advantages of Dividing wall columns Lower capital investment
Reduction in number of columns + condensers and reboilers
Lower operating costs

Lower energy consumption due to heat integration ~ 30% lower energy costs
When to consider Dividing wall columns heuristics

When the middle component is 20% or more in the feed If the pressure difference between adjacent columns in a conventional setup is high, do not consider this option Energy consumption is low, but that doesnt account for the level of energy being used
Liquid liquid separation operations
Slide 41
Types of Liquid-liquid Separation Operations

Distillation Extraction Crystallisation Adsorption Membrane
Most expensive Cheapest
Slide 42
Situations where other types of separations are used

Separation not feasible by distillation Energy requirements of distillation are prohibitive The material is heat sensitive The material is non-volatile
Slide 43
Extraction
Used to remove a solute from a liquid solution The solute is removed by contacting with another liquid solvent which is relatively immiscible (cannot be mixed) with the solution The solute is more soluble to the liquid solvent than the solution
solvent
Solution
Weaker solution
Extraction
Mixture of solvent and solute
Slide 44
Extraction process
5
B
3
() B+S
2
Extraction
6 C(+B)
Distillation
Distillation
7
In extraction process, other distillation columns are needed for the recovery of solvent
Distillation
B+C
B+C
C+S(+B) S
Slide 45
Crystallisation process
Vapour C (+B?) B+C
Crystalliser
Centrifuge
Dryer
B: higher freezing point C: lower freezing point

Liquid C
B Crystals
Crystallisation operation often requires other unit operations to separate a stream

Slide 46
Adsorption process
A Heater
Cooler A, B B Bed on-line Bed being regenerated
In a adsorption process, the desorption operation always accompanies

Slide 47

Separation

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Separation

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Department of Process & Systems Engineering

Synthesis of Separation System Dr Ade Lawal

Process Simulation and Design

Department of Process & Systems Engineering

Process Simulation and Design

Department of Process & Systems Engineering

Determination of the General Structure of the Separation System

Process Simulation and Design

Department of Process & Systems Engineering

Phase of the reactor effluent stream

Separation Products System

Focus on reactor exit stream

Department of Process & Systems Engineering

When the reactor effluent is all liquid

Liquid Separation Products System

From Douglas, AIChE, 31: 353 (1985)

Department of Process & Systems Engineering

When the reactor effluent is a vapour and liquid mixture

Use the reactor as a phase splitter

Send the liquid to the liquid separation system

Cool the vapour and phase split it

Liquid separation Products system

From Douglas, AIChE, 31: 353 (1985)

Department of Process & Systems Engineering

When the reactor effluent is all vapour

From Douglas, AIChE, 31: 353 (1985)

Department of Process & Systems Engineering

The phase split operation is preferred

Methods for obtaining a phase split

Process Simulation and Design

Department of Process & Systems Engineering

Synthesis of Vapour Recovery System

Process Simulation and Design

Department of Process & Systems Engineering

Possible Locations for Vapour Recovery System

Process Simulation and Design

Department of Process & Systems Engineering

Rules to locate the vapour recovery system

on the purge stream

If materials that are deleterious (harmful) to the reactor operation

on the gas-recycle stream

If both items are valid

Vapour from phase split

on the flash vapour stream

Neither item is important

Process Simulation and Design

Department of Process & Systems Engineering

Types of the Vapour Recovery System

high pressure or low temperature, or both

Absorption process Adsorption process Membrane separation process Reaction systems

Department of Process & Systems Engineering

Water+ammonia Packed tower for absorption

Department of Process & Systems Engineering

Department of Process & Systems Engineering

Department of Process & Systems Engineering

Liquid Separation System

Process Simulation and Design

Department of Process & Systems Engineering

Decisions to synthesise the liquid separation system

Department of Process & Systems Engineering

Process Simulation and Design

Department of Process & Systems Engineering

Alternatives for Light-ends Removal

Remove the light ends in a phase splitter