CHAPTER 3: Part I

SEPARATION SYSTEM

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 Learning Outcomes
After studying this topic, participants should be able to:

• Familiar with industrial separation methods and basis for separation.

• Understand the concept of separation factor and choose appropriate

separation methods for liquid and solid-fluid mixtures.

• Understand the distillation columns are sequenced/arranged.

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Hierarchical Method: Process Flow-sheeting

The “Onion” Model (Smith and Linnhoff, 1988)

Reactor

Separation &
Recycle System

Heat Exchanger
Network

Utilities

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 What are Separation Operations?

Separates a multicomponent input stream into two or more

output stream which the compositions differ from the
input stream

OR

Separates a multiphase stream into its constituent/basic

sub-streams

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 Typical Applications : Separations Fractional
Crystallization

• Separation of Multicomponent Stream

– Distillation
– Gas Absorption and Stripping/Desorber
– Liquid-liquid Extraction
– Fractional Crystallization
– Pressure Swing Adsorption (PSA) PSA

Distillation column Liquid-liquid extraction

Gas absorption/desorber

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 Typical Applications : Separations (cont.)
• Separation of Multiphase stream
– Filtration (solid-liquid)
– Decantation (liquid-liquid)
– Electrostatic Precipitation (gas-solid)
– Knock-out Drum (gas-liquid)
Decantation:
“process for the
separation of mixtures,
by removing a layer of
liquid, generally one
from which a
precipitate has settled”

Filter Press

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 Basic Rules for Separation
• Do separation involving phase split (in the presence of heterogeneous
mixture) before performing the separation for homogenous mixture.

• Separation involving phase split normally does not involve complex decision
as compared to the homogenous mixture.

• As distillation is the most widely used for separation of homogenous

mixture attention will be to sequencing the distillation column.

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 General Separation System Process Flowsheet

Liquid 1 recycle
Product(s)- Byproduct(s)

Vapor recycle Vapor Separation Recycle

Separation
System Product(s)-
Byproduct(s)
Vapor Liquid 1
Liquid 1 Separation
Reactor Purge
Phase System
Feed(s) effluent
Reactor Separation Liquid 2
System System
Liquid 2
Purge
Separation
Solids or slurry System
Product(s)-
Byproduct(s)
Solid recycle
Solid-Slurry Separation Recycle
Separation
System

Purge Product(s)- Byproduct(s)

Liquid 2 recycle

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 Process Example: Hydrodealkylation of Toulene to Benzene

T + H2 B (benzene) + CH4 (methane)

2B D (diphenyl) + H2

CH4 CH4
H2 Vapor Vapor
Separation Separation
System System
Vapor Vapor

T Reactor Reactor
Phase T Phase
effluent effluent
Reactor Separation Reactor Separation
H2 System H2 System

Liquid Liquid
Recycle
B Toluene (T) & B
Recycle Liquid Diphenyl (D) Liquid
Toulene Separation Separation
System System
D

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 Physical Basis of Separation
All separation are differ based on property of the material being separated.

• Physical properties
– Vapor pressure (distillation, gas absorption, drying)
– Solubility (Crystallization)
– Density (Decantation, floatation, sedimentation)

• Phase Creation
– Energy separating Agent (ESA) (simple distillation)
– Mass separating agent (MSA) (gas absorption, liquid-liquid extraction, extractive
distillation column)

• Use of a Barrier (Membrane Separation)

– Gas (gas permeation)
– Liquid (dialysis, RO)
– Liquid-Solid (Ultrafiltration)

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 Common Industrial Separation Methods
Separation Feed Separating Added Separation
Method Phase Agent(s) Phase Property
Flash L/V Pressure reduction/ V/L Volatility
Heat transfer ESA
Distillation L/V Heat transfer or V/L Volatility
Shaft work ESA
Gas absorption V Liquid absorbent MSA L Volatility
Stripping L Vapor stripping agent MSA V Volatility
Extractive distillation L and/or V Liquid solvent & heat transfer MSA L&V Volatility
Azeotropic distillation L and/or V Liquid entrainer and heat transfer MSA L&V Volatility
Liq-liq extraction L Liquid solvent MSA Second L Solubility
Crystallization L Heat transfer ESA S Solubility or
melting point
Gas adsorption V Solid adsorbent MSA S Adsorbability
Liquid adsorption L Solid adsorbent MSA S Adsorbability
Membrane L/V Membrane ESA Membrane Permeability
and/or solubility
Supercritical L/V Supercritical solvent MSA Supercritical fluid Solubility
extraction S Liquid solvent MSA L Solubility
Leaching S&L Heat transfer ESA V Volatility
Drying V Heat transfer ESA S Volatility
Desublimation

ESA : Energy Separating Agent

MSA : Mass Separating Agent

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 Separation Performance Criteria
• Product Purity
– Meet product spec (product)
– Meet regulatory spec to be disposable (by-product/wastes)

• Fractional/Small of Recovery/Profit
– High enough to make process operable and economic
– Trade off/Exchange between equipment cost and operating penalties
(e.g. loss of product, disposable cost)

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 Heuristics Column Sequencing

Simple Columns
A B,C Separate B
design task C
a
A 3.2
Feed B 1.7
C 1.6 D
D 1.0
E 0.4 D, E

If 2 neighboring components having a relative

volatility (a) is less than 1.1 in a mixture, group this
component together and treat this group as a single E
component in a mixture

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 Column Sequencing – Ternary Mixture

A/BC B/C
Alternative Distillation Volatility order:
Sequences for a ABC
A>B>C
ternary mixture AB/C A/B

A A/B
B A

A A
B B
C C
C C B
B/C
Direct sequence Indirect sequence
Lightest component is taken as overhead product Heaviest component is taken as bottom product
in the 1st column before separating the other 2 in the 1st column before separating the other 2
components in the 2nd column components in the 2nd column
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 Column Sequencing - Quaternary Mixture

Alternative Sequences for

Four Component System B/CD C/D

A/BCD
BC/D B/C

ABCD AB/CD A/B C/D

A/BC B/C

ABC/D
AB/C A/B

+ 2 others indirect sequences

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 Group Working Session

• Reactor effluent consist of hydrogen, toluene, methane,

benzene and diphenyl. Design alternative sequences for 5
component system.

• Assume volatility:
Hydrogen>methane>benzene>toluene>diphenyl

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 Process Example: Production of Monochlorodecane (MCD)
MCD is to be produced from decane (DEC) and chlorine via the reaction. The byproduct (DCD) is not
required for this project.

C10H22 + Cl2 C10H21Cl + HCl

DEC MCD

C10H21Cl + Cl2 C10H20Cl2 + HCl

MCD DCD

Determine the possible separation sequences that can be considered for these 4 scenarios:
1. Complete conversion of both feeds
2. Incomplete conversion of both feeds
3. Excess chlorine
4. Excess decane
Material Normal Boiling Point (K)

HCl 188
Cl2 239
DEC 447
MCD 488
DCD 514
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 Number of Alternatives Sequences

Number of Number of possible

components sequences
2 1
3 2
4 5
5 14
6 42
7 132
8 429
9 1,430
10 4,862
As the number of components increases, more alternative
sequences are possible !!!

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THANK YOU

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