TCN3132 Separation Processes

Lecture 5: Binary Distillation

Special Cases

Dr Suraj Vasudevan
Email: chesura@nus.edu.sg

Department of Chemical &

Biomolecular Engineering

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 Overview

• Limiting cases of distillation

 Total reflux
 Minimum reflux

• McCabe Thiele for special cases of distillation

 Open steam
 Double feed

• Efficiency in column design

Reference:
Wankat 3rd edition
Chapter 4

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 Limiting Operating Condition 1: Total Reflux

• All of the overhead vapor is returned to column as

reflux => No distillate
• All of the liquid from last stage is returned as boilup
=> No bottoms product
 Since D and B are equal to 0, feed must also be
equal to 0 at steady state
• Total reflux used for column startup, for keeping a
column operating when another part of the plant is
shut down or for testing column efficiency
 Used for small-scale, batch applications (e.g.,
pharmaceutical industry)

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 Limiting Operating Condition 1: Total Reflux

𝐿𝐿
• Since all vapor is refluxed, 𝐿𝐿 = 𝑉𝑉 and = 1
• Total reflux gives minimum number 𝑉𝑉
of stages for a given separation 𝐿𝐿 �
• Likewise 𝐿𝐿� = 𝑉𝑉� and � = 1
• Also indicates maximum separation 𝑉𝑉

possible for a given number of stages  Hence both operating lines become 𝒚𝒚 = 𝒙𝒙
=> Diagonal

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 Limiting Operating Condition 2: Minimum Reflux
𝐿𝐿
• Minimum reflux is defined as the external reflux ratio at
𝐷𝐷 𝑚𝑚𝑚𝑚𝑚𝑚
which the desired separation could just be obtained with infinite
number of stages => A hypothetical condition
• The operating lines and equilibrium curve must touch
 This happens either at the feed or a point tangent to the
equilibrium curve
 Pinch point – point where the operating line touches the
equilibrium curve
 The concentrations of the liquid and vapor do not change from
stage-to-stage => Inoperable region
𝐿𝐿
• As increases, number of stages decreases and cooling and
𝐷𝐷
heating duties/pumping increases
 Capital cost decreases and operating cost increases

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 Limiting Operating Condition 2: Minimum Reflux

• With 𝑧𝑧, 𝑞𝑞, 𝑥𝑥𝐷𝐷 , 𝑥𝑥𝐵𝐵 known, continue changing

the slopes of the operating lines until they
intersect at equilibrium
𝐿𝐿
• Corresponding slope of TOL gives the
𝑉𝑉 𝑚𝑚𝑚𝑚𝑚𝑚
𝐿𝐿
minimum reflux ratio
𝐷𝐷 𝑚𝑚𝑚𝑚𝑚𝑚
𝑳𝑳 𝑳𝑳
• Actual = 𝜶𝜶 , where 1.2 < 𝛼𝛼 < 1.3
𝑫𝑫 𝑫𝑫 𝒎𝒎𝒎𝒎𝒎𝒎
• Optimum reflux is at minimum total cost

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 Special Case 1: Open Steam
• When the less volatile component in a binary mixture is
water, heat can be added to the column by introducing
saturated steam to the bottom stage => This is called
open steam; the reboiler is eliminated
• TOL remains the same
• Mass balance for stripping section becomes:
� 𝑘𝑘 + 𝐵𝐵𝑥𝑥𝐵𝐵
𝐿𝐿� 𝑥𝑥𝑘𝑘−1 + 𝑆𝑆 0 = 𝑉𝑉𝑦𝑦
𝐿𝐿� 𝐵𝐵
⇒ 𝑦𝑦𝑘𝑘 = � 𝑥𝑥𝑘𝑘−1 − � 𝑥𝑥𝐵𝐵
𝑉𝑉 𝑉𝑉
𝑩𝑩 𝑩𝑩
⇒ 𝒚𝒚𝒌𝒌 = 𝒙𝒙𝒌𝒌−𝟏𝟏 − 𝒙𝒙𝑩𝑩 (because 𝐿𝐿� = 𝐵𝐵 and 𝑉𝑉� = 𝑆𝑆)
𝑺𝑺 𝑺𝑺
 When 𝑦𝑦 = 0, 𝑥𝑥𝑘𝑘−1 = 𝑥𝑥𝐵𝐵
 Hence, BOL cuts x-axis at 𝒙𝒙 = 𝒙𝒙𝑩𝑩
𝐵𝐵
 BOL cuts the diagonal at 𝑦𝑦 = 𝑥𝑥 = 𝑥𝑥
𝐵𝐵−𝑆𝑆 𝐵𝐵

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 Special Case 2: Double Feed
• When we have two feeds with different compositions,
it is counter-productive to mix them and feed to the
distillation column as the natural separation already
present will be lost A
• The two feeds are introduced separately, with the feed
with higher mole fraction of more volatile component
introduced above the other feed (that is, closer to the
top)
• Mass balance around envelope A gives the equation of
the middle operating line (MOL):
𝐹𝐹2 𝑧𝑧2 + 𝑉𝑉 ′ 𝑦𝑦 = 𝐿𝐿′ 𝑥𝑥 + 𝐷𝐷𝑥𝑥𝐷𝐷 Features of MOL:
• Passes through point of intersection of TOL
𝑳𝑳′ 𝑫𝑫𝒙𝒙𝑫𝑫 −𝑭𝑭𝟐𝟐 𝒛𝒛𝟐𝟐
=> 𝒚𝒚 = 𝒙𝒙 + and feed line for 𝐹𝐹2
𝑽𝑽′ 𝑽𝑽′

𝐿𝐿′ 𝐷𝐷𝑥𝑥𝐷𝐷 −𝐹𝐹2 𝑧𝑧2 • Passes through point of intersection of BOL

 Slope = and Intercept =
𝑉𝑉 ′ 𝑉𝑉 ′ and feed line for 𝐹𝐹1

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 Efficiency
• Equilibrium stages represent the ideal scenario
• Performance of actual stages differs from ideal equilibrium stage assumption
• Deviation in performance accounted for by the use of efficiency
• Many different measures of efficiency have been proposed
• One common measure is the overall efficiency
• It is defined as the number of ideal equilibrium stages required for the separation
divided by the actual number of stages required
𝑵𝑵𝒊𝒊𝒊𝒊𝒊𝒊𝒊𝒊𝒊𝒊
𝑬𝑬𝑬𝑬𝑬𝑬𝑬𝑬𝑬𝑬𝑬𝑬𝑬𝑬𝑬𝑬𝑬𝑬𝑬𝑬 =
𝑵𝑵𝒂𝒂𝒂𝒂𝒂𝒂𝒂𝒂𝒂𝒂𝒂𝒂

• The efficiency value is generally based on designer’s experience with other similar
columns

Stage efficiency versus tray efficiency

• Stages include plates, partial condenser and partial reboiler
• Tray only refers to plates
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 Example 1: Open Steam
Consider the separation of methanol from water in a staged distillation column. The feed is 60 mol% methanol
and 40 mol% water and is fed as a two-phase mixture; 30% of this feed flashes. Feed flow rate is 350 kmol/h.
The column is well insulated and has a total condenser. The reflux is returned to the column as a saturated
𝐿𝐿
liquid. An external reflux ratio of = 3.0 is used. We desire a distillate concentration of 95 mol% methanol
𝐷𝐷
and a bottoms concentration of 8 mol% methanol. Instead of using a reboiler, saturated steam at 1 atm is
sparged directly into the bottom of the column to provide boilup (that is, open steam). Column pressure is 1
atm. The equilibrium curve is given.

Calculate the number of equilibrium stages and the optimum feed plate location.

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 𝐷𝐷 =

𝑉𝑉 𝑥𝑥𝐷𝐷 =
𝐿𝐿/𝐷𝐷 =
𝐿𝐿/𝑉𝑉 =
𝐿𝐿

𝐹𝐹 =
𝑧𝑧 =
𝑞𝑞 =

𝑉𝑉� = 𝐵𝐵 =
𝑦𝑦 = 𝑥𝑥𝐵𝐵 =
Pure water 𝐿𝐿� ⁄𝑉𝑉� =
Saturated vapor

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 TOL:
One point: 𝑥𝑥𝐷𝐷 = 0.95 on diagonal
𝑥𝑥𝐷𝐷
Second point: y-intercept = =
𝑅𝑅𝐷𝐷 +1

 Feed line:
One point: 𝑧𝑧 = 0.60 on diagonal
−𝑞𝑞
Second point: Slope = =
1−𝑞𝑞

 BOL:
One point: 𝑥𝑥𝐵𝐵 = 0.08 on x-axis
Second point: point of intersection of feed line and TOL

 Number of ideal stages, 𝑁𝑁𝑖𝑖𝑖𝑖𝑖𝑖𝑖𝑖𝑖𝑖 =

 Optimum feed plate = Optimum feed stage =

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 100

90

80

70
Methanol Mole Percent (Vapor)
60

50

40

30

20

10

0
0 10 20 30 40 50 60 70 80 90 100
Methanol Mole Percent (Liquid)

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 Example 2: Minimum Reflux and Efficiency
The y-x and T-x plots for acetonitrile (CH3CN)-acetic acid (CH3COOH) system are given in Figure Q2. Read the
figure caption carefully. A feed containing 51.35 mole % acetonitrile and 48.65 mole% acetic acid is proposed
to be separated in a multi-stage distillation column. The column has a total condenser and a partial reboiler,
and the total feed flow rate is 1000 kmol/h. The design target is 90% recovery of acetonitrile in the top
product and 95% recovery of acetic acid in the bottom product. The feed is a sub-cooled liquid and
condenses one mole of vapour for every four moles of feed. Operating 𝐿𝐿⁄𝑉𝑉 = 2 𝐿𝐿⁄𝑉𝑉 𝑚𝑚𝑚𝑚𝑚𝑚 . Overall stage
efficiency is 40%. Feed is introduced at the optimum location.

a) Design the distillation column. Show all related calculations and drawings.
b) What is the reboiler temperature?

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 a)

α=4
α=3.5

b)

Figure 2: (a) x-y plot. The symbols are experimental

data. The lines are calculated assuming constant α
values given in the figure. (b) T-x plot.
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 Purities are not given; need to calculate from the given recoveries:
Component In Feed In Distillate In Bottoms
Acetonitrile

Acetic Acid

 Therefore,
𝑥𝑥𝐷𝐷 =

𝑥𝑥𝐵𝐵 =

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 Feed quality:
𝑞𝑞 =

 Feed line:
One point: 𝑧𝑧 = 0.5135 on diagonal
−𝑞𝑞
Second point: Slope = =
1−𝑞𝑞

 Minimum reflux ratio can be determined from point of intersection of TOL and feed
line with equilibrium curve:
𝐿𝐿
=
𝑉𝑉 𝑚𝑚𝑚𝑚𝑚𝑚

𝐿𝐿 𝐿𝐿
 =2 =
𝑉𝑉 𝑉𝑉 𝑚𝑚𝑚𝑚𝑚𝑚

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 TOL:
One point: 𝑥𝑥𝐷𝐷 = 0.95 on diagonal
𝑥𝑥𝐷𝐷
Second point: y-intercept = =
𝑅𝑅𝐷𝐷 +1

 BOL:
One point: 𝑥𝑥𝐵𝐵 = 0.1 on diagonal
Second point: point of intersection of feed line and TOL

 Number of ideal stages, 𝑁𝑁𝑖𝑖𝑖𝑖𝑖𝑖𝑖𝑖𝑖𝑖 =

 Optimum feed stage =

𝑁𝑁𝑖𝑖𝑖𝑖𝑖𝑖𝑖𝑖𝑖𝑖
 Number of real stages, 𝑁𝑁𝑟𝑟𝑟𝑟𝑎𝑎𝑎𝑎 = =
𝐸𝐸

 Reboiler temperature, 𝑇𝑇𝑟𝑟𝑟𝑟𝑟𝑟 =

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