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TCN3132 Separation Processes

Lecture 4: Binary Distillation –


Equilibrium Stage Design

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

Department of Chemical &


Biomolecular Engineering

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Overview

• Binary multistage distillation


 Operating line equations
 McCabe Thiele procedure
 Feed quality and feed line
 Optimum feed stage location

Reference:
Wankat 2nd, 3rd
and 4th editions
Chapters 3 and 4

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Recap: Basics of Distillation

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Recap: Basics of Distillation

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Operating Line Equation for Enriching Section
How to draw TOL?
Stage j envelope
1. Intersects diagonal (𝑦𝑦 = 𝑥𝑥) at 𝑥𝑥 = 𝑥𝑥𝐷𝐷
• Overall mass balance becomes: 𝐿𝐿 𝐿𝐿
𝑥𝑥 = 𝑥𝑥 + (1 − )𝑥𝑥𝐷𝐷
𝑉𝑉 = 𝐿𝐿 + 𝐷𝐷 𝑉𝑉 𝑉𝑉
2. Slope:
• Component mass balance becomes: 𝐿𝐿�
𝐿𝐿 𝐿𝐿 𝐷𝐷 𝑅𝑅𝐷𝐷
𝑉𝑉𝑦𝑦𝑗𝑗+1 = 𝐿𝐿𝑥𝑥𝑗𝑗 + 𝐷𝐷𝑥𝑥𝐷𝐷 = = 𝐿𝐿 =
𝑉𝑉 𝐿𝐿+𝐷𝐷 �𝐷𝐷+1 𝑅𝑅𝐷𝐷 +1

𝑳𝑳 𝑫𝑫 (𝑅𝑅𝐷𝐷 is the external reflux ratio)


⇒ 𝒚𝒚𝒋𝒋+𝟏𝟏 = 𝒙𝒙 + 𝒙𝒙
𝑽𝑽 𝒋𝒋 𝑽𝑽 𝑫𝑫 3. y-intercept:
This is the top operating line (TOL) 𝐷𝐷 𝐿𝐿 𝑅𝑅𝐷𝐷 𝑥𝑥𝐷𝐷
𝑥𝑥 = 1− 𝑥𝑥𝐷𝐷 = 1 − 𝑥𝑥𝐷𝐷 =
equation (that is, above feed stage) 𝑉𝑉 𝐷𝐷 𝑉𝑉 𝑅𝑅𝐷𝐷 +1 𝑅𝑅𝐷𝐷 +1

Use any two of the above to draw TOL

𝐷𝐷 𝑉𝑉−𝐿𝐿 𝐿𝐿
= =1−
𝑉𝑉 𝑉𝑉 𝑉𝑉

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Top Operating Line in McCabe Thiele Diagram

Stage 1 calculation in McCabe Thiele diagram Stepping off stages in the McCabe Thiele method

• Passing streams lie on operating line, that is, 𝑥𝑥0 , 𝑦𝑦1 , 𝑥𝑥1 , 𝑦𝑦2 , 𝑥𝑥2 , 𝑦𝑦3 and so on
• 𝑥𝑥1 , 𝑦𝑦1 , 𝑥𝑥2 , 𝑦𝑦2 , 𝑥𝑥3 , 𝑦𝑦3 , etc. lie on equilibrium curve
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Operating Line Equation for Stripping Section

Stage k envelope How to draw BOL?


• Overall mass balance becomes: 1. Intersects diagonal (𝑦𝑦 = 𝑥𝑥) at 𝑥𝑥 = 𝑥𝑥𝐵𝐵
𝐿𝐿� 𝐿𝐿�
𝑉𝑉� = 𝐿𝐿� − 𝐵𝐵 𝑥𝑥 = � 𝑥𝑥 + (1 − �)𝑥𝑥𝐵𝐵
𝑉𝑉 𝑉𝑉
• Component mass balance becomes: 2. Slope:
� 𝑘𝑘 = 𝐿𝐿� 𝑥𝑥𝑘𝑘−1 − 𝐵𝐵𝑥𝑥𝐵𝐵
𝑉𝑉𝑦𝑦 𝐿𝐿�

𝑉𝑉

⇒ 𝒚𝒚𝒌𝒌 =

𝑳𝑳
𝒙𝒙
𝑩𝑩
− � 𝒙𝒙𝑩𝑩 3. Intersection of TOL and feed line (will be
� 𝒌𝒌−𝟏𝟏
𝑽𝑽 𝑽𝑽
discussed next)
This is the bottom operating line (BOL)
equation (that is, below feed stage)
Use any two of the above to draw BOL

𝐵𝐵 � −𝐿𝐿�
𝑉𝑉 𝐿𝐿�
−�= �
=1−�
𝑉𝑉 𝑉𝑉 𝑉𝑉

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Bottom Operating Line in McCabe Thiele Diagram

Stepping off stages in the McCabe Thiele method

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Feed Quality q
Why is feed quality important?
• It determines how 𝐿𝐿 and 𝐿𝐿� are related, likewise how 𝑉𝑉 and
𝑉𝑉� are related
• q is defined as additional flow of liquid in the stripping
section due to introduction of one mole of feed
• Total flow of liquid in the stripping section:
𝐿𝐿� = 𝐿𝐿 + 𝑞𝑞𝑞𝑞 ℎ𝑓𝑓−1 = ℎ𝑓𝑓 = ℎ
𝐻𝐻𝑓𝑓 = 𝐻𝐻𝑓𝑓+1 = 𝐻𝐻
• Total flow of vapor in the enriching section:
𝑉𝑉 = 𝑉𝑉� + 1 − 𝑞𝑞 𝐹𝐹
• Enthalpy balance on feed stage:
� = 𝐿𝐿� ℎ + 𝑉𝑉𝑉𝑉
𝐹𝐹ℎ𝐹𝐹 + 𝐿𝐿𝐿 + 𝑉𝑉𝐻𝐻
• Combining the above three equations and rearranging:
𝐻𝐻−ℎ𝑓𝑓
𝑞𝑞 =
𝐻𝐻−ℎ

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Feed Quality q

• All feed will enter the stripping section when it is


saturated liquid
=> 𝑞𝑞 = 1, 𝐿𝐿� = 𝐿𝐿 + 𝐹𝐹 and 𝑉𝑉 = 𝑉𝑉�
• All feed will enter the enriching section when it is
saturated vapor
=> 𝑞𝑞 = 0, 𝑉𝑉 = 𝑉𝑉� + 𝐹𝐹 and 𝐿𝐿� = 𝐿𝐿

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Feed Line
• The two operating lines are:
𝑉𝑉𝑦𝑦𝑗𝑗+1 = 𝐿𝐿𝑥𝑥𝑗𝑗 + 𝐷𝐷𝑥𝑥𝐷𝐷 (TOL)
� 𝑘𝑘 = 𝐿𝐿� 𝑥𝑥𝑘𝑘−1 − 𝐵𝐵𝑥𝑥𝐵𝐵 (BOL)
𝑉𝑉𝑦𝑦
• Feed line is a straight line that passes through the point of intersection of
TOL and BOL
• At the point of intersection:
𝑦𝑦𝑗𝑗+1 = 𝑦𝑦𝑘𝑘 = 𝑦𝑦 and 𝑥𝑥𝑗𝑗 = 𝑥𝑥𝑘𝑘−1 = 𝑥𝑥
• Equation of the feed line is obtained by subtracting BOL from TOL:
𝑉𝑉 − 𝑉𝑉� 𝑦𝑦 = 𝐿𝐿 − 𝐿𝐿� 𝑥𝑥 + (𝐷𝐷𝑥𝑥𝐷𝐷 + 𝐵𝐵𝑥𝑥𝐵𝐵 )
⇒ 𝐹𝐹 1 − 𝑞𝑞 𝑦𝑦 = −𝑞𝑞𝑞𝑞 𝑥𝑥 + 𝐹𝐹𝐹𝐹
−𝒒𝒒 𝒛𝒛
⇒ 𝒚𝒚 = 𝒙𝒙 +
𝟏𝟏−𝒒𝒒 𝟏𝟏−𝒒𝒒

Feed line intersects diagonal at 𝒙𝒙 = 𝒚𝒚 = 𝒛𝒛

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Feed Line

Feed condition Feed Temperature q Slope

Subcooled liquid 𝑇𝑇𝐹𝐹 < 𝑇𝑇𝐵𝐵𝐵𝐵 𝑞𝑞 > 1 >1

Saturated liquid 𝑇𝑇𝐹𝐹 = 𝑇𝑇𝐵𝐵𝐵𝐵 𝑞𝑞 = 1 ∞

Two-phase mixture 𝑇𝑇𝐵𝐵𝐵𝐵 < 𝑇𝑇𝐹𝐹 < 𝑇𝑇𝐷𝐷𝐷𝐷 1 > 𝑞𝑞 > 0 Negative

Saturated vapor 𝑇𝑇𝐹𝐹 = 𝑇𝑇𝐷𝐷𝐷𝐷 𝑞𝑞 = 0 0

Superheated vapor 𝑇𝑇𝐹𝐹 > 𝑇𝑇𝐷𝐷𝐷𝐷 𝑞𝑞 < 0 1 > 𝑠𝑠𝑠𝑠𝑠𝑠𝑠𝑠𝑠𝑠 > 0

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Significance of Feed Line
• The feed line represents all possible locations at which the two operating lines can intersect for a given
feed with 𝑧𝑧𝐹𝐹 𝑎𝑎𝑎𝑎𝑎𝑎 𝑞𝑞

Changing reflux ratio changes the If reflux ratio (that is slope of TOL) is
points of intersection but they all lie on fixed, but q varies, the intersection
the feed line point varies

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Optimum Feed Location

• We get optimum feed location when the feed stage


includes the point of intersection of TOL and BOL
• For fixed operating lines, the total number of stages
required for a given separation will be the least when
feed is introduced at the optimum location
• Number of stages will increase when feed is not
introduced at optimum location
• The feed stage triangle ends on the BOL

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Example 1: Distillation Column Design
A distillation column is separating ethylene dichloride from trichloroethane. Equilibrium data can be
represented by 𝛼𝛼 = 2.4. The column has a total condenser and a partial reboiler. Reflux is returned as a
saturated liquid. The feed is 60 mole% ethylene dichloride, the more volatile component. Feed rate is
100 kg moles/hr. Distillate mole fraction is 0.92 ethylene dichloride and bottoms mole fraction is 0.08
ethylene dichloride. Assume CMO. Pressure is 1 atm.

a) Find B and D.
𝐿𝐿 �
𝑉𝑉
b) If the external reflux ratio = 2.0 and the boil-up ratio = 1.2, find the optimum feed stage, and
𝐷𝐷 𝐵𝐵
the total number of equilibrium stages.
c) What is the value of q? What type of feed is this?

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61.9
2
2/3
100
0.92
0.6

38.1

1.833

0.08

𝐿𝐿 𝐿𝐿�
Note: B, D, , � have been calculated in Lecture 3, Example 3
𝑉𝑉 𝑉𝑉

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Equilibrium curve: b)
𝛼𝛼𝛼𝛼 2.4𝑥𝑥
𝑦𝑦 = =
1+ 𝛼𝛼−1 𝑥𝑥 1+1.4𝑥𝑥
 TOL:
One point: 𝑥𝑥𝐷𝐷 = 0.92 on diagonal
x y 𝑥𝑥𝐷𝐷
Second point: y-intercept = =
0 0 𝑅𝑅𝐷𝐷 +1

0.1 0.21
0.2 0.375  BOL:
0.3 0.51 One point: 𝑥𝑥𝐵𝐵 = 0.08 on diagonal
0.4 0.62 𝐿𝐿�
Second point: Slope = �
=
0.5 0.71 𝑉𝑉

0.6 0.78
0.7 0.85
0.8 0.91  Number of ideal stages, 𝑁𝑁 =
0.9 0.96
1 1  Optimum feed stage =

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c)
 Join point of intersection of TOL and BOL with 𝒛𝒛 on diagonal:
−𝑞𝑞
Slope of feed line = =
1−𝑞𝑞

Therefore, 𝑞𝑞 =

Therefore, feed type: _________________

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Example 2: Distillation Column with Partial Condenser
The partial condenser in a multi-stage distillation column may be viewed as a flash unit, as shown in the
figure below. The distillation column is being used to separate toluene-phenol mixture obtained from an
extraction process. This separation gives the desired purified toluene product and allows phenol recovery for
recycle. The x-y and T-x plots for toluene are given on the next slide.

a) What is the operating temperature of the condenser?

b) Calculate 𝐿𝐿⁄𝑉𝑉 ratio for the rectifying section.

c) Calculate 𝐿𝐿��𝑉𝑉� ratio for the stripping section.

d) What is the composition of the feed to the distillate column?

e) Find the number of ideal stages. Clearly state your assumptions.

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a)
 Partial condenser is an equilibrium stage →can be treated as
a flash unit:
𝑥𝑥0 and 𝑦𝑦𝐷𝐷 are in equilibrium

Hence, 𝑥𝑥0 = (from x-y curve)

And 𝑇𝑇 = (from T-x curve)

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b)
 V is the feed to the flash unit and fraction feed vaporized is
𝒇𝒇 = 𝑫𝑫⁄𝑽𝑽:
1−𝑓𝑓
Slope of flash operating line = − =
𝑓𝑓

𝐷𝐷
Therefore, 𝑓𝑓 = =
𝑉𝑉

Overall mass balance: 𝐷𝐷 = 𝐹𝐹 − 𝐵𝐵 =

𝐷𝐷
Hence, 𝑉𝑉 = =
𝑓𝑓

Condenser mass balance: 𝐿𝐿 = 𝑉𝑉 − 𝐷𝐷 =

Can you think of an alternative Hence, 𝐿𝐿⁄𝑉𝑉 =


method to calculate 𝐿𝐿⁄𝑉𝑉?

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c)
 Vapor and liquid flow rates in the stripping section are related
to the vapor and liquid flow rates in the enriching section by
the feed quality:
Given: 𝑞𝑞 = 1.5
What type of feed is this?

𝐿𝐿� 𝐿𝐿+𝑞𝑞𝑞𝑞
Therefore, � = =
𝑉𝑉 𝑉𝑉− 1−𝑞𝑞 𝐹𝐹

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d)
 Feed composition can by obtained by component mass
balance:
𝐹𝐹𝐹𝐹 = 𝐷𝐷𝑦𝑦𝐷𝐷 + 𝐵𝐵𝑥𝑥𝐵𝐵
=>

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e)
 Assumptions:
1) CMO
2) Feed is on optimum stage.
 TOL:
One point: 𝑦𝑦𝐷𝐷 = 0.95 on diagonal
𝑦𝑦𝐷𝐷
Second point: y-intercept = =
𝑅𝑅𝐷𝐷 +1
 Feed line:
One point: 𝑧𝑧 = 0.59 on diagonal
−𝑞𝑞
Second point: Slope = =
1−𝑞𝑞
 BOL:
One point: 𝑥𝑥𝐵𝐵 = 0.05 on diagonal
Second point: point of intersection of feed line and TOL
 Number of ideal stages, 𝑁𝑁 =

 Optimum feed stage =


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