Batch Distillation with Rectification
Separation of Ethanol and Water
Using an Oldershaw Distillation
Column
Group 2
Marwah Al Ruzeiqi (E1), Evan
Cox (E2), Hannah Winton (E3),
Daniel Duncan (E4)
Introduction
• Distillation is one of the most important mass
transfer operations used in the industry.
• Distillation is a process used to separate pure
liquids from a mixture of liquids without the
need of further processing.
• The production of pure oxygen,
used in steel making, and crude
petroleum, used in kerosene,
fuel oils and gasoline, are some
products that are easily
produced with distillation.
A Ruzeiqi (E1), Cox (E2), Winton (E3),
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Duncan (E4)
Introduction (Cont.)
• Example of types of Distillation: azeotropic
distillation, extraction distillation, vacuum
distillation, simple distillation, etc.
• Two main ways of carrying out distillation process: in
batch (small scale) or continuous (larger scales).
• Our experiment dealt with fractional batch
distillation.
3
Literature Analysis 1
Title: Optimization of a Batch Extractive Distillation Process
with Recycling Off-cuts [1]
• A multiple step solvent recovery distillation process (with
the use of both conventional and extractive batch
distillation) is optimized. The components form several
azeotropes, and the off-cuts are recycled.
• The recovery of methanol from an industrial waste solvent
mixture is studied.
• The environmental impact is also assessed by calculating
the related CO2 emission and the waste water production.
• The optimization of both processes is performed by a
genetic algorithm coupled with a professional flow-sheet
simulator performing the dynamic simulation.
A Ruzeiqi (E1), Cox (E2), Winton (E3),
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Literature Analysis 1: Continue
Results:
• The extractive process gives
a 67% higher profit than the
optimized batch distillation,
whose profit was in turn by
25% higher than without
optimization. Fig.: Variation of the specific emissions (kg emission/kg
main-cut) for basic Batch Distillation.
• The specific CO2 emission
(kg CO2/kg product) is by
20% lower for the extractive
process than for the
optimized and by 22% lower
than for the non-optimized
batch distillation.
A Ruzeiqi (E1), Cox (E2), Winton (E3), Fig.: Variation of the specific emissions (kg emission/kg
main-cut) for Batch Extractive Distillation. 5
Duncan (E4)
Literature Review 2
Title: Intermittent Feeding Batch Distillation
with Liquid Exchange Between Two
Columns for Separation of Binary Mixtures
[2]
• The proposed strategy is of two columns
operating in parallel with liquid exchange
under total reflux to separate binary
mixtures.
• A mathematical model is setup for the
simulation.
• The design consists of two top vessels and
two bottom vessels added to a batch
distillation column as shown in the figure.
• The two vessels work alternatively, & the
operation is achieved by switching valves.
A Ruzeiqi (E1), Cox (E2), Winton (E3),
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Literature Review 2: Continue
• Advantages to this:
– The capacity of the column is more flexible.
– Different amount of feed can be separated by the same
column without start-up many times.
– The product of both the light component and the heavy
component can be collected before the separation is
completed.
• Results:
– Optimal holdup for different feeding concentration and the
total yield increases with the growth of total charge.
– The proposed operation mode is verified experimentally
and it reveals significant potential for separation with
higher efficiency and lower pressure drop.
A Ruzeiqi (E1), Cox (E2), Winton (E3),
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Objective
• Study the performance
of the batch distillation
with finite reflux.
• Run the column under
total reflux.
A Ruzeiqi (E1), Cox (E2), Winton (E3),
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Apparatus
Condenser
Cooling Water
Thermocouple
Reflux
Control
1
Distillate
2
Sample
3
Thermometer 5
6
7
Anton Paar 8
Densitometer 9
10
Thermocouple
Peristaltic
Still Pot
Pump
Variac
A Ruzeiqi (E1), Cox (E2), Winton (E3),
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Procedure
• Oldershaw column was charged with an initial mixture
of ethanol and water, and the Variac is turned on
several hours prior to the experiment
• Experiment run for an ethanol-water mixture of 5.5L
water and 0.5L EtOH under finite reflux
• The peristatic pump is turned on +5 mins prior to
beginning the experiment
• Initial temperatures were recorded at finite reflux and a
sample of the still pot was taken to start the experiment
• Temperatures of the still pot and of the distillate and
cumulative distillate volume recorded every five
minutes
A Ruzeiqi (E1), Cox (E2), Winton (E3),
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Procedure
• Still pot and distillate were sampled every ten
minutes
• Once cooled, still pot and distillate samples
were run through the Anton Paar
densitometer to determine compositions
• Deionized water and pure ethanol were ran
through the densitometer as standards to
improve accuracy
• The column was run for a total of 120 minutes
A Ruzeiqi (E1), Cox (E2), Winton (E3),
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Duncan (E4)
Experimental Plan
Fixed Variables Units Range
Reflux Time (sec. D: sec, L) ---- 30:30
Variac Setting V 90
Volume of Liquid in Still (W0) L 6
Manipulated Variables Units Range
Feed Composition Ratio L. Water: L. EtOH 5.5 : 0.5
Time Minutes 0-120
Measured Variables Units Range
Overhead Vapor Temperature oC 77-93.3
Still Pot Temperature oC 93.9-98
Distillate Volume mL 0-480
Distillate Density g/cm3 .8306-.9295
Still Pot Density g/cm3 .9886-.9945
A Ruzeiqi (E1), Cox (E2), Winton (E3),
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Engineering Principles
• Preliminary Analysis
𝑚𝐿
– Distillate (Product) Rate - 𝐷,
ℎ𝑟
– Reflux Ratio - 𝑅
𝑚𝐿
– Reflux Rate – 𝐿0 ,
ℎ𝑟
𝑚𝐿
– Vaporization Rate - 𝑉1 ,
ℎ𝑟
• Flow Balance – Top of Column
𝑉1 = 𝐷 + 𝐿0 [1]
A Ruzeiqi (E1), Cox (E2), Winton (E3),
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Engineering Principles
𝑚𝐿
• Distillate (Product) Rate - 𝐷,
ℎ𝑟
𝑣
𝐷= [2]
𝑡
• Reflux Ratio - 𝑅
𝐿0
𝑅= [3]
𝐷
𝑚𝐿
• Reflux Rate – 𝐿0 ,
ℎ𝑟
𝐿0 = 𝑅 ∙ 𝐷 [4]
𝑚𝐿
• Vaporization Rate - 𝑉1 ,
ℎ𝑟
𝑉1 = 𝐷 + 𝐿0 [1]
A Ruzeiqi (E1), Cox (E2), Winton (E3),
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Volume to Mole Fractions
• Mole Fraction of Ethanol in Distillate - 𝑦𝐷
𝑣𝐷 ∙𝜌𝐸
𝑀𝑊𝐸
𝑦𝐷 = 𝑣𝐷 ∙𝜌𝐸 (1−𝑣𝐷 )∙𝜌𝑊 [5]
𝑀𝑊𝐸
+ 𝑀𝑊
𝑊
𝑣𝐷 = Volume percent of ethanol in distillate
𝜌𝐸 = Density of ethanol
𝑀𝑊𝐸 = Molecular weight of ethanol
𝜌𝑊 = Density of pure water
𝑀𝑊𝑊 = Molecular weight of pure water
• Mole Fraction of Ethanol in Still Pot - 𝑥𝑊
𝑣𝐵 ∙𝜌𝐸
𝑀𝑊𝐸
𝑥𝑊 = 𝑣𝐵 ∙𝜌𝐸 (1−𝑣𝐵 )∙𝜌𝑊 [6]
𝑀𝑊𝐸
+ 𝑀𝑊
𝑊
𝑣𝐵 = Volume percent of ethanol in the still pot
A Ruzeiqi (E1), Cox (E2), Winton (E3),
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Determining 𝑊𝐹𝑖𝑛𝑎𝑙 and 𝑥𝐷,𝑎𝑣𝑔
• Composition of distillate and bottoms changes
instantaneously with time
– Differential Mass Balances
• Rayleigh Analysis
• Assumptions
• Constant molar overflow
• Negligible hold up
• Negligible heat losses in the column
A Ruzeiqi (E1), Cox (E2), Winton (E3),
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Rayleigh Analysis
• Component Balance – Rates
– Rate of depletion of the liquid in the column =
the rate of distillate output
• Instantaneous Rate of Depletion of a Component in the Still
𝑑 𝑊𝑥𝑤 −𝑊𝑑𝑥𝑊 𝑥𝑤 𝑑𝑊
− = − [7]
𝑑𝑡 𝑑𝑡 𝑑𝑡
Change in total Change in Change in the
amount of that composition in total amount of
component in the still the still liquid
𝑑
− 𝑊𝑥𝑊 = 𝐷𝑦𝐷 [8]
𝑑𝑡
A Ruzeiqi (E1), Cox (E2), Winton (E3),
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Duncan (E4)
Rayleigh Analysis
𝑑 𝑊𝑑𝑥𝑊 𝑥𝑤 𝑑𝑊
𝑊𝑥𝑊 = + = −𝐷𝑦𝐷 [9]
𝑑𝑡 𝑑𝑡 𝑑𝑡
• Multiply Equation 9 by 𝑑𝑡
𝑊𝑑𝑥𝑤 + 𝑥𝑤 𝑑𝑊 = 𝑦𝐷 −𝐷𝑑𝑡 [10]
• Known: the rate of total liquid depletion = distillate flow rate
𝑑𝑊 = −𝐷𝑑𝑡 [11]
𝑊𝑑𝑥𝑤 + 𝑥𝑤 𝑑𝑊 = 𝑦𝐷 𝑑𝑊 [12]
𝑑𝑥𝑊 𝑑𝑊
= [13]
𝑦𝐷 −𝑥𝑊 𝑊
𝑥𝑊 𝑑𝑥 𝑊
𝑦 𝑥−𝑥 = ln [14]
𝑊,0 𝐷 𝑊 𝑊0
A Ruzeiqi (E1), Cox (E2), Winton (E3),
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Duncan (E4)
Solving Rayleigh Analysis
• Use Experimental Data to Solve Equation 14 by Graphical
Integration
1
– Plot versus 𝑥𝑊
𝑦𝐷 −𝑥𝑊
• Numerical Integration by the Trapezoidal Rule
𝑥𝑊 𝑑𝑥 𝑊
𝑥 = ln [14]
𝑊,0 𝑦𝐷 −𝑥𝑊 𝑊0
𝑊 𝑥 𝑑𝑥 1
ln = 𝑊 𝑥 ≈ ∆𝑥 [15]
𝑊0 𝑊,0 𝑦𝐷 −𝑥𝑊 𝑦−𝑥 𝑎𝑣𝑔
𝑊 = Moles remaining in still pot
𝑊0 = Initial moles in still pot
𝑥𝑊,0 = Initial composition in still pot
A Ruzeiqi (E1), Cox (E2), Winton (E3),
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Determining 𝑥𝐷,𝑎𝑣𝑔
• Overall Balance Around the Column
𝑊0 = 𝐷 + 𝑊 [16]
• Component Balance
𝑊0 𝑥𝑊,0 = 𝐷𝑦𝐷 + 𝑊𝑥𝑊 [17]
• Combing Overall and Component Material
Balances
𝑊0 𝑥𝑊,0 −𝑊𝑥𝑊
𝑥𝐷,𝑎𝑣𝑔 = [18]
𝑊0 −𝑊
𝑥𝐷,𝑎𝑣𝑔 = average composition of liquid in still pot
A Ruzeiqi (E1), Cox (E2), Winton (E3),
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Theoretical Distillation Time -
𝑡 (ℎ𝑜𝑢𝑟𝑠)
• The time required for batch rectification with
constant reflux ratio was estimated using the
equation due to Block [3]
𝑊0 −𝑊𝑡 𝑅+1
𝑡= 𝐿 = (𝑊0 − 𝑊𝑡 ) [19]
𝑉 1− 𝑉
𝑉
𝑊0 (mL) = Initial still pot content
𝑊𝑡 (mL) = Still pot content at time 𝑡
𝑚𝐿
𝑉 = Vaporization Rate
ℎ𝑟
𝑅 = Reflux Ratio
A Ruzeiqi (E1), Cox (E2), Winton (E3),
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McCabe Thiele Analysis
• Mass Balance Around the nth Tray
𝐿𝑛−1 𝑥𝑛−1 +𝑉𝑛+1 𝑦𝑛+1 = 𝐿𝑛 𝑥𝑛 + 𝑉𝑛 𝑦𝑛 [20]
A Ruzeiqi (E1), Cox (E2), Winton (E3),
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McCabe Thiele Analysis
• Obtain Column Operating Line Equation by Rearranging
Equation 20
– Assuming constant molar flow
−𝐿 𝐿𝑥𝑛−1 +𝑉𝑦𝑛+1
𝑦𝑁 = 𝑥 + [21]
𝑉 𝑁 𝑉
– Composition of the two entering streams for the tray 𝑥𝑛−1 , 𝑦𝑛+1 are
fixed values at each time interval
– 𝐿 and 𝑉 are constant phase flow rates
−𝐿
– Equation 21 is a straight line with slope =
𝑉
• Stages found by stepping off at each time interval from
𝑥𝑊 to 𝑥𝐷
A Ruzeiqi (E1), Cox (E2), Winton (E3),
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McCabe Thiele Analysis
Batch Distillation of a two-stage column with 𝑅 = 1 [4]
A Ruzeiqi (E1), Cox (E2), Winton (E3),
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Overall Tray Efficiency
• Correction factor used for the comparison of
practical stages to the ideal stage model at
equilibrium
𝑁𝑡
𝐸0 = [22]
𝑁𝑎
𝑁𝑡 = Number of equilibrium stages calculated
𝑁𝑎 = Number of actual stages required
A Ruzeiqi (E1), Cox (E2), Winton (E3),
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Cumulative Volume
500
450
400
y = 225.38x + 51.422
350 R² = 0.9869
Volume (mL)
300
250
200
150
100
50
0
0.0 0.2 0.4 0.6 0.8 1.0 1.2 1.4 1.6 1.8 2.0
Time (hr)
A Ruzeiqi (E1), Cox (E2), Winton (E3),
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Distillate Flow Rate
700
600
500
FLow (mL/hr)
400
300
200
100
0
0.0 0.2 0.4 0.6 0.8 1.0 1.2 1.4 1.6 1.8 2.0
Time (hr)
A Ruzeiqi (E1), Cox (E2), Winton (E3),
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Flow Rate Comparison
1200
1000
800
Flow Rate (mL/hr)
600 Distillate
Reflux
400 Overhead
200
0
0.0 0.2 0.4 0.6 0.8 1.0 1.2 1.4 1.6 1.8 2.0
Time (hr)
A Ruzeiqi (E1), Cox (E2), Winton (E3),
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Temperature Comparison
375
370
365
Temperature (K)
360
Still Pot
Overhead
355
350
345
0.0 0.2 0.4 0.6 0.8 1.0 1.2 1.4 1.6 1.8 2.0
Time (hr)
A Ruzeiqi (E1), Cox (E2), Winton (E3),
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Concentration of Ethanol
0.8
0.7
0.6
Concentration (mol/mol)
0.5
0.4
Distillate
0.3 Still Pot
0.2
0.1
0
0.0 0.2 0.4 0.6 0.8 1.0 1.2 1.4 1.6 1.8 2.0
Time (hr)
A Ruzeiqi (E1), Cox (E2), Winton (E3),
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Rayleigh Analysis and Block Equation
Block Equation Parity Plot
3
Predicted Measured % Error
2.5
Wfinal (mL) 5782.3 5520 4.536
Block Time (hr)
2
1.5
[Link] (mol/mol) 0.4493 0.4309 4.095
timefinal (hr) 2.857 2 29.996 0.5
0
0.0 0.5 1.0 1.5 2.0
Actual Time (hr)
A Ruzeiqi (E1), Cox (E2), Winton (E3),
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McCabe-Thiele Analysis
All Operating Lines
1
0.9
Equilibrium
0.8
X-Y
0.7 T=0 min
0.6 T=10 min
Y (mol/mol)
T=20 min
0.5
T=30 min
0.4 T=40 min
0.3 T=50 min
T=70 min
0.2
T=90 min
0.1 T=110
0 T=120 min
0 0.2 0.4 0.6 0.8 1
X (mol/mol)
A Ruzeiqi (E1), Cox (E2), Winton (E3),
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McCabe-Thiele Analysis
T=0 min McCabe-Thiele T=10 min McCabe-Thiele
1 1
0.9 0.9
0.8 0.8
0.7 0.7
Y (mol/mol)
Y (mol/mol)
0.6 0.6
0.5 0.5
0.4 0.4
0.3 0.3
0.2 0.2
0.1 0.1
0 0
0 0.2 0.4 0.6 0.8 1 0 0.2 0.4 0.6 0.8 1
X (mol/mol) X (mol/mol)
A Ruzeiqi (E1), Cox (E2), Winton (E3),
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Tray Efficiency
0.9
0.8
0.7
0.6
Efficiency
0.5
0.4
0.3
0.2
0.1
0
0.0 0.2 0.4 0.6 0.8 1.0 1.2 1.4 1.6 1.8 2.0
Time (hr)
A Ruzeiqi (E1), Cox (E2), Winton (E3),
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XD Parity Plot
0.1
0.09
0.08
XD Measured (mol/mol)
0.07
0.06
0.05
0.04
0.03
0.02
0.01
0
0 0.01 0.02 0.03 0.04 0.05 0.06 0.07 0.08 0.09 0.1
XD Predicted (mol/mol)
A Ruzeiqi (E1), Cox (E2), Winton (E3),
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Citation
1. Hegely, L., & Lang, P. (2016). Optimization of a batch
extractive distillation process with recycling off-
cuts. Journal of Cleaner Production,136, 99-110.
doi:10.1016/[Link].2016.04.140
2. Zhao, J., Wang, B., Bai, P., Guo, X., & Ding, H. (2016).
Intermittent feeding batch distillation with liquid
exchange between two columns for separation of binary
mixtures. Chemical Engineering and Processing: Process
Intensification,99, 41-50. doi:10.1016/[Link].2015.11.003
3. Seader, J.D. and Henley, Ernest J., Separation Process
Principles. John Wiley & Sons, New York, 1998.
4. Batch Distillation- No Author.
<[Link]/[Link]>
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