Topic 4 – Process Synthesis: Separation Sequencing

Distillation Column Sequencings

Problem Session 9
Extractive Distillation
 Aim of this Session

▪ Distillation Sequences for separating close-boiling point systems or azeotropes

▪ Extractive Distillation

Extractive distillation (ED) is the vapor–liquid separation process, with two key concepts:
• Addition of a miscible, high boiling or relatively non-volatile component called the
solvent or entrainer.
• Purpose of adding the solvent is to increase the relative volatility of the components
to be separated and hence increase the separation factor.

9–2
 Distillation with Azeotropes
• It is sometimes not possible to change the pressure sufficiently
to “break” or shift the azeotrope.

• Then adding of a third component could help with this.

• For example, adding ethylene glycol to ethanol and water:

Boiling Point Vapor Pressure Relative Volatility

Compound
(°C) @ 25°C (kPa) (α)
α (Water/EtOH) =
Ethanol 78.37 7.87
0.402
α (Water/EG) =
Water 100 3.17
397
α (EtOH/EG) =
Ethylene Glycol 197.3 0.008
983

9–3
 Extractive Distillation: Design Guidelines

• The feed components must have different affinities for the solvent so that the solvent
increases the relative volatility (α) of the key components.

• The solvent should not form azeotropes with any of the feed components.

• Typically, a solvent-to-feed molar ratio of ~1:1 is used.

• The bottoms stream is processed to recover the solvent for recycle and to complete the
separation of feed components.

• For minimum-boiling azeotrope systems, a solvent with lower volatility than the feed
components is introduced just below the column top:
• The solvent flows downward with the liquid.
• Minimal solvent is lost to the overhead vapor.

• For maximum-boiling azeotrope systems, the solvent is introduced with the feed.

9–4
Example Extractive Distillation System

EDC

SRC
“Heavy Entrainer”

9–5
 Question 1
Consider the feed mixture of 65 mol% methanol and 35 mol% acetone that need to be separated.
Methanol and acetone form an azeotrope. Water could be used as a solvent.

Use the ternary diagram and design an

extractive distillation system as to obtain
“pure” methanol and acetone products.

Draw a flowsheet of this system (with all

stream information) and clearly label
(indicate) on the ternary diagram each
stream and mixing points.

9–6
 Question 1 - Answer
Three Column Design Approach: The typical three column extractive
distillation sequence:
• First consisting of simple distillation
Almost Pure Pure concentrating the feed to the
Acetone Methanol azeotrope composition,
• Followed by the extractive distillation
column (EDC) with the added solvent,
• and then simple distillation to
Methanol + recover the solvent.
Acetone

SRC
EDC
Often a pre-concentration distillation
column is used as this reduces the
Preconcentrator amount of material passing through the
two distillation columns with the solvent.
This reduced the size of these columns
and the amount of solvent needed, thus
Pure the cost of the system is reduced.
Methanol (S)
If the feed composition is similar to the
azeotrope then it may not be necessary
to have the pre-concentration distillation
column - this is an economic balance.

9–7
 Question 1 - Answer

D3 B1

A+B
Feed (F1)
Preconcentrator
S

D1
F3 = B2 F2
S = B3
Solvent (S)
Water D2
9–8
 Question 1 - Answer
Two Column Design Approach:

D2
S
D1 D2

B1
Feed
B2

B1 Mixture point
B2
Solvent (S)
Water D1
9–9