Ki 2 A - Eche 461 Fa 17 Group 2 Per I Exp Bde

Batch Distillation with Rectification:
Separation of Ethanol and Water Using an Oldershaw

Distillation Column
Group 2
E1: M. A. Al-Ruzeiqi
E2: E. L. Cox
E3: H. E. Winton
E4: J. D. Duncan
Group 2 Period I
To: Dr. James A. Ritter
From: Group 2: Marwah Al-Ruzeiqi-E1, Evan Cox-E2, Hannah Winton-E3, Daniel Duncan-E4
Date: October 6, 2017
Subject: Batch Distillation with Rectification: Separation of Ethanol and Water Using an
Oldershaw Distillation Column
Abstract
In this study, batch distillation with rectification under finite reflux in a ten tray
Oldershaw Distillation Column is analyzed for its effectiveness as a method of separation of
ethanol and water. An initial charge of ethanol-water mixture is fed to the heated still pot of the
column. After the initial charge, only the distillate is removed as product.
The objective of this experiment is to study the performance of the Oldershaw
Distillation Column under a finite reflux of one for the separation of ethyl alcohol from water.
Samples from the distillate and bottoms are taken every ten minutes and then ran through a Paar
digital density meter with an ethanol/water calibration curve to analyze the composition of the
samples. Secondary objectives of the study are to use Rayleigh Analysis, the Block Equation,
and McCabe-Thiele analysis to predict the final ethanol concentration in the still pot, the average
concentration of ethanol in the distillate, the time required for the separation to take place, the
theoretical number of stages needed in the column, and the tray efficiency, and then compare
these predicted values to those found experimentally.
Predicted values from Rayleigh’s analysis of still pot residue and average concentration
of ethanol in the distillate were found to be consistent with experimental data with a percent
1
M. A. Al-Ruzeiqi (E1), E. L. Cox (E2), H. E. Winton (E3), J. D. Duncan (E4)
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difference of 4.642% and 4.174% respectively. The Block equation proved to be a poor
estimation of the time required for the separation of ethanol and water with a percent difference
of 35.3% between predicted and actual time recorded. Tray efficiency was found to decrease
from 54.5% to 18.18% excluding an outlier at t=10 minutes where the efficiency jumped to
90.91%. This abnormality is also seen in the McCabe-Thiele figures for the distillation because
the operating line at the 10 minute interval is above the previous time interval’s (t=0min)
operating line.
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Table of Contents
Introduction .................................................................................................................... 4
Experimental Objectives ................................................................................................ 5
Literature Review ........................................................................................................... 5
Apparatus and Procedure ............................................................................................... 7
Engineering Principles and Working Equations .......................................................... 10
Experimental Plan ........................................................................................................ 17
Results and Discussion ................................................................................................. 18
Conclusions .................................................................................................................. 31
Literature Cited and References ................................................................................... 33
Appendices
Appendix A: Sample Calculations
Appendix B: Figures
Appendix C: Laboratory Notebook
Appendix D: Documentation
Appendix E: Statistical Design of Experiment
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Introduction:
Distillation, also known as fractionation or fractional 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. Distillation is done
by heating liquids with different boiling points, turning them into gas, then condensing the gas
back into liquid form and collecting the liquid. The process can be repeated to further purify the
liquid and can be reversed in order to separate gasses [1].
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.
Other use for distillation includes the production of xylene, alcohol, kerosene, etc. There are
many types of distillation such as azeotropic distillation, extraction distillation, vacuum
distillation, simple distillation, etc. Each type of distillation is used for a different reason, but
follow the main idea of mass separations.
Furthermore, there are two main ways of carrying out distillation process: in batch or
continuous. Batch distillation is one that separates a mixture into its component before being
charged with more mixture. It is useful with a smaller scale production, such that in laboratories
or for separating products of high value. Another useful case for batch distillation is when
working with the presence of solids in the system as they can be cleared out between batches.
Continuous Distillation on the other hand is one where the feed is added and the distillate drawn
off without interruptions and in this case approaches steady state. This is mostly useful in large-
scale process such as refineries were distillation is done continuously for long periods.
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The experiment dealt with fractional batch distillation, usually a vertical column
comprised of different stages or trays. The process of distillation is repeated throughout the
different stages. In elaboration, the liquid is heated, rises as vapor to the next tray, and
condenses, and then the process is repeated at every stage. This helps in purifying the liquid
further and further as the component moves up the column.
Objectives:
The experiment in hand deals with fractional batch distillation used to separate ethyl
alcohol from water. The objective of this experiment was to study the performance of a batch
distillation and be familiar with the system with the use of an Oldershaw sieve plate column.
Moreover, the groups were to perform Rayleigh analysis, perform McCabe-Thiele, and use the
Block Equation in aims of studying the relationship between the total moles in the system and
the moles of the more volatile component, finding the number of stages and stage efficiencies of
the column, and find the theoretical distillation time, respectively.
Literature Review:
The article “Optimization of a Batch Extractive Distillation Process with Recycling Off-
cuts,” studies both conventional and extractive distillation process and ways to optimize their
use, efficiency and the recycling process as it is clear how important the recovery of organic
solvents from waste mixtures in the chemical and pharmaceutical industries from an economical
and environmental standards is. Recycling or recovery of these organic waste help tremendously
in lowering operation costs as well as the costs of incineration of waste mixtures. Not only is that
the incineration of waste materials costly and done in hazardous plants, it also produces 𝐶𝑂2 as
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the process involves burning waste material. Therefore, it is important to note the importance of
recycling.
The process used in the article involves the use of a multiple step solvent recovery
distillation to recover methanol from a waste solvent mixture while trying to optimize the
process. The process is done by first incinerating an initial part or amount, and then recycling
following batches to cut the cost of methanol loss. The optimization process is done by “a
generic algorithm coupled with a professional flow-sheet simulator performing the dynamic
simulation.” The optimization was done concentrating on the profit of each batch while studying
the effects of recycling, and comparing the optimized batch distillation and batch extractive
distillation with one another and with the distillation process used in the experiment.
Results from the study show that the extractive process gave 67% higher profit than the
optimized batch distillation process, which in turn gave 25% profit. Also, the study showed that
extractive process, emissions of 𝐶𝑂2 were less by 20% than the optimized process, further, the
non optimized batch distillation showed 22% less 𝐶𝑂2 emissions than that of the optimized
process [2].
The article “Intermittent Feeding Batch Distillation with Liquid Exchange Between Two
Columns for Separation of Binary Mixtures,” is one of the many studies done on batch
distillation, as it is one of the most common and wildly used distillations in the chemical and
pharmaceutical industry. It is known that batch distillations are important in purifying and
recovering components, especially ones of high value and in small volumes. During the past two
decades, there have been many studies and proposed operating modes on the batch distillation
coming forward with the goal of improving the distillation’s efficiency or flexibility. This article
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puts forward a mathematical model and proposes a new operation strategy of liquid exchange
between two columns in order to separate mixtures. The thing that separates this study from
other studies is the use of two columns that are set to operate in parallel under total reflux in
order to separate the liquid mixtures. The design consists of two top vessels and two bottom ones
added to a batch distillation column where the vessels work alternatively and the operation is
achieved by switching valves.
The article discusses the advantages to the proposed model, which includes: more
flexible column capacity, Easy separation of different concentrations of feed by the same column
without having to start-up every time, and most importantly, both more volatile and less volatile
product can be collected even before separation is completed. Results from the study shows the
potential of the proposed model for separation with higher efficiency and lower pressure drop.
The study also shows that with the increase of the total charge, the total yield and the optimal
holdup for different feeding concentration increases [3].
Apparatus and Procedure:
The batch distillation experiment apparatus involved an Oldershaw column with ten sieve
plate trays, and a jacket to prevent heat loss. At the bottom of the column, a still pot containing a
mixture is heated with a Variac power supply. The still pot, in combination with the ten trays in
the column, represents eleven total stages of distillation. A peristaltic pump is used to mix and
recirculate the contents of the still pot and for the extraction of the still pot sample. At the top of
the column, the reflux rate is controlled with a reflux controller. Throughout the column, the
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distillate rises containing more of the more-volatile component, while liquid falls down the
column. This idea can be seen in Figure 1 below.
Figure 1: Example of a distillation column design
Two thermocouples (K-type) are attached to the bottom and top of the column for temperature
readings of the bottom still pot and overhead distillate, respectfully, and displayed on a
thermometer reader. The Anton Paar DMA 4500 Densitometer is used to determine
compositions of the distillate and still pot samples. The apparatus is modeled below in Figure 2.
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Figure 2: The Oldershaw batch distillation column and apparatus
The Oldershaw column was charged with an initial mixture of 5.5L of water and .5L
ethanol, and the Variac and reflux controller were set several hours before the experiment. The
Variac was set to 90 V and the reflux ratio was set to 30:30 (sec. D : sec L) to operate the batch
distillation under finite reflux. The peristaltic pumped was turned on more than five minutes
before data collection began.
Initial temperature readings of the bottoms and tops of the distillation column were taken
(t=0) to begin the data collection for the experiment. Measurements of the cumulative distillate
volume, overhead temperature, and bottoms still pot temperature were taken every five minutes
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and recorded in the lab notebook. Samples from the overhead distillate and still pot were taken
every ten minutes for the extent of the experiment. The samples were tested for composition
after cooling using the Anton Paar Densitometer, which was repeatedly tested for standard by
running deionized water and pure ethanol. The experiment ran under finite reflux for a total of
120 minutes.
Engineering Principles and Working Equations:
The objective of this study is to evaluate the performance of the batch distillation with
rectification process via an Oldershaw Sieve Plate Column with finite reflux for the separation of
ethyl alcohol and water. Periodic samples of the distillate and bottoms are taken and their
compositions are analyzed using a DMA 48 Density/Specific Gravity/Concentration Meter with
an ethanol/water calibration curve.
In this experiment, the still pot and distillate of the column are sampled every ten
minutes. From these samples, the distillate flow rate (𝐷), overhead vapor rate (𝑉1), and reflux
rates (𝐿0 ) as functions of time, are calculated. To determine the distillate flow rate as a function
𝑚𝐿
of time (D, ), the volume of distillate product taken (𝑣, 𝑚𝐿) is divided by the time elapsed
ℎ𝑟
between samples (𝑡, ℎ𝑜𝑢𝑟). The distillate rate expresses the rate at which liquid distillate, rich in
light key, is removed from the top of the column and is defined by the equation below.
𝑣
𝐷= [1]
𝑡
𝑚𝐿
The reflux rate (𝐿0 , ℎ𝑟 ) is the rate of liquid condensate from the condenser that is returned
to the top most tray of the column. Under the assumption that all flows are reported as
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condensed liquid and the densities of all streams in the column are approximately equal, the
reflux rate is determined from the value for the reflux ratio (𝑅) via Equations 2 and 3.
𝐿0
𝑅= [2]
𝐷
𝐿0 = 𝑅 ∙ 𝐷 [3]
The reflux ratio is a constant for the column. Therefore, different reflux rate values can
be determined at varying distillate flow rates.
After defining the distillate flow rate and reflux rate, it is possible to solve for the
𝑚𝐿
overhead vapor rate (𝑉1 , ℎ𝑟 ) from a material balance around the condenser. The overhead vapor
rate defines the rate at which vapor leaves the topmost tray in the column. This value is often
𝑚𝐿
reported in of the equivalent condensed liquid flow instead of as a vapor stream and is
ℎ𝑟
defined by Equation 4.
𝑉1 = 𝐿0 + 𝐷 [4]
After calculating the distillate flow rate, overhead vapor rate and reflux rate, it is
necessary to calculate the mole fraction of ethanol in both the distillate and the bottoms product.
The mole fraction of ethanol in the distillate (𝑦𝐷 ) and the mole fraction of ethanol in the bottoms
(𝑥𝑤 ) can be derived from the weight percent of ethanol in the distillate (𝑤𝐷 ), the weight percent
of ethanol in the bottoms (𝑤𝐵 ), the molecular weight of ethanol (𝑀𝑊𝐸 ), and the molecular
weight of water (𝑀𝑊𝑊 ) via Equation 5 and 6 respectively.
𝑤𝐷
𝑀𝑊𝐸
𝑦𝐷 = 𝑤𝐷 (1−𝑤𝐷 )∙𝜌𝑊 [5]
+
𝑀𝑊𝐸 𝑀𝑊𝑊
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𝑤𝐵
𝑀𝑊𝐸
𝑥𝑊 = 𝑤𝐵 (1−𝑤𝐵 )∙𝜌𝑊 [6]
+
𝑀𝑊𝐸 𝑀𝑊𝑊
The composition of distillate and bottoms in this study change instantaneously with time,
to determine the final still contents or residue in the still pot (𝑊𝐹𝑖𝑛𝑎𝑙 ) and 𝑥𝐷,𝑎𝑣𝑔 , differential
mass balances are necessary. The Rayleigh analysis is used to determine these values assuming
constant molar overflow, negligible liquid hold up, and negligible heat losses in the column. For
this analysis, a component balance is written for the instantaneous rate of depletion of a
component in the still pot. This is shown in Equations 7 where the left most term is equal to the
change in total amount of that component in the still, the middle term represents the change in
composition in the still, and the right most term equals the change in the total amount of liquid in
the still pot.
𝑑(𝑊𝑥𝑤 ) −𝑊𝑑𝑥𝑊 𝑥𝑤 𝑑𝑊
− = − [7]
𝑑𝑡 𝑑𝑡 𝑑𝑡
It is known that the rate of component depletion in the still pot is equal to the component
flowrate in the distillate. This is defined by Equation 8.
𝑑(𝑊𝑥𝑊 )
− = 𝐷𝑦𝐷 [8]
𝑑𝑡
Equation 9 is achieved by combining Equations 7 and 8.
𝜕(𝑊𝑥𝑊 ) 𝑊𝜕𝑥𝑊 𝑥𝑤 𝜕𝑊
= + = −𝐷𝑦𝐷 [9]
𝜕𝑡 𝜕𝑡 𝜕𝑡
Equation 9 is simplified by multiplying through by 𝑑𝑡.
𝑊𝑑𝑥𝑤 + 𝑥𝑤 𝑑𝑊 = 𝑦𝐷 (−𝐷𝑑𝑡) [10]
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To simplify further, it is known that the rate of total liquid depletion is equal to the
distillate flow rate leaving the column.
𝑑𝑊 = −𝐷𝑑𝑡 [11]
Substituting Equation 11 into Equation 10 derives Equation 12 below that is easily
separated and integrated to arrive at a solvable equation where 𝑊 shows the moles remaining in
the still pot, 𝑊0 represents the initial moles in the still pot, and 𝑥𝑊,0 is the initial composition in
the still pot.
𝑊𝑑𝑥𝑤 + 𝑥𝑤 𝑑𝑊 = 𝑦𝐷 𝑑𝑊 [12]
𝑑𝑥𝑊 𝑑𝑊
= [13]
𝑦𝐷 −𝑥𝑊 𝑊
𝑥𝑊 𝑑𝑥 𝑊
∫𝑥 = ln⁡(𝑊 ) [14]
𝑊,0 𝑦𝐷 −𝑥𝑊 0
1
Equation 14 is solved by graphical integration of experimental data by plotting 𝑦𝐷 −𝑥𝑊
𝑊
versus 𝑥𝑊 . The area under the curve of the plot is then equated to ln⁡(𝑊 ) and 𝑊, or the moles
0
remaining in the still pot, can be determined using numerical integration of Equation 14 by the
Trapezoidal Rule as shown in Equation 15.
𝑥𝑊 𝑑𝑥 𝑊
∫𝑥 = ln⁡(𝑊 ) [14]
𝑊,0 𝑦𝐷 −𝑥𝑊 0
𝑊 𝑥 𝑑𝑥 1
ln (𝑊 ) = ∫𝑥 𝑊 ≈ ∆𝑥 [𝑦−𝑥] [15]
0 𝑊,0 𝑦𝐷 −𝑥𝑊 𝑎𝑣𝑔
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To determine 𝑥𝐷,𝑎𝑣𝑔 , a mass balance is performed on the system. The mass balance
defines that the initial charge to the still pot (𝑊0 ) is equal to the amount of distillate removed (𝐷)
and the amount that remains in the still pot (𝑊) as defined by Equation 16.
𝑊0 = 𝐷 + 𝑊 [16]
The mass balance is valid only under the assumption of negligible liquid hold up in the
column. This equation can be put into terms of 𝑥𝐷,𝑎𝑣𝑔 by multiplying each term by the
respective molar fraction term.
𝑊0 𝑥𝑊,0 = 𝐷𝑥𝐷,𝑎𝑣𝑔 + 𝑊𝑥𝑊 [17]
Then by combining the overall mass balance equation and the component balance, it is
possible to solve for 𝑥𝐷,𝑎𝑣𝑔 , the average composition of liquid in the still pot.
𝑊0 𝑥𝑊,0 −𝑊𝑥𝑊
𝑥𝐷,𝑎𝑣𝑔 = [18]
𝑊0 −𝑊
To determine the time required for the batch distillation of ethanol and water with
constant reflux to run to completion, the equation due to Block is used.
𝑊0 −𝑊𝑡 𝑅+1
𝑡= 𝐿 = (𝑊0 − 𝑊𝑡 ) [19]
𝑉(1− ) 𝑉
𝑉
In Equation 19, 𝑊0 is the initial still pot content in mL, 𝑊𝑡 is the still pot content at time
𝑚𝐿
𝑡 in mL, 𝑉 is the vaporization rate in ℎ𝑜𝑢𝑟, and 𝑅 is the reflux ratio.
To complete the analysis of the Oldershaw distillation column for the separation of
ethanol and water, a McCabe-Thiele analysis is performed to determine the number of trays
necessary for separation. To begin, a mass balance around the nth tray in the column is written.
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𝐿𝑛−1 𝑥𝑛−1 + 𝑉𝑛+1 𝑦𝑛+1 = 𝐿𝑛 𝑥𝑛 + 𝑉𝑛 𝑦𝑛 [20]
Equation 20 demonstrates that the amount of material entering the nth tray is equal to the
amount of material leaving the tray. The 𝑛 − 1 terms and the 𝑛 + 1 terms in the equation
represent the liquid and vapor streams flowing into the 𝑛𝑡ℎ tray respectively. The liquid enters
the 𝑛𝑡ℎ tray from the top from the 𝑛 − 1 tray and the vapor stream enters from the bottom of the
𝑛𝑡ℎ tray from the 𝑛 + 1 tray. The 𝑛 terms in the equation represent the liquid and vapor streams
leaving the 𝑛𝑡ℎ tray. The molar fractions of the chemical component in the liquid phase is 𝑥 and
𝑦 represents the molar fraction of the component in the vapor phase. Rearranging Equation 20
and solving for 𝑦𝑛 gives the equation for the rectifying section operating line for the McCabe-
Thiele analysis as defined below.
−𝐿 𝐿𝑥𝑛−1 +𝑉𝑦𝑛+1
𝑦𝑛 = 𝑥𝑛 + [21]
𝑉 𝑉
Equation 21 assumes constant molar overflow in the column. The compositions of the
two entering streams for the tray (𝑥𝑛−1 , 𝑦𝑛+1 ) are fixed values at each time interval and 𝐿 and 𝑉
−𝐿
are constant phase flow rates making Equation 21 a straight line with a slope of . The material
𝑉
balance for the rectifying section gives the equation below if 𝐿 and 𝑉 are constants for a fixed
distillate flowrate (𝐷).
𝑉𝑛+1 = 𝐿𝑛 + 𝐷 [22]
Using Equation 22 to redefine the operating line of the rectifying sections gives the final
operating line.
𝐿 𝐷
𝑦 = 𝑉 𝑥 + 𝑉 𝑥𝐷 [23]
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The operating line defined by Equation 23 is used to plot the stages required for
separation at a specific time interval. The line begins at the point (𝑥𝐷 , 𝑦𝐷 ) where it intersects the
45-degree-line and then continues until it reaches the equilibrium curve for the ethanol water
mixture. The number of stages for the separation are determined by stepping off from 𝑥𝐷 until
no more steps can be made, and then counting the number of times the steps intersect the
equilibrium curve. The point at which the final step intersects the equilibrium curve is the point
𝑥𝑊 as predicted by the McCabe-Thiele analysis. This process is demonstrated in the figure
below.
Figure 3: McCabe-Thiele process at time intervals 0 and 1 within a two stage column with
reflux value of one. The process at time 0 and 1 both yielded two stages necessary for the
separation.
The efficiency of the trays in the Oldershaw column is determined by taking the ratio of
the actual stages in the column to the ideal stages found in the equilibrium stage model. Tray
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efficiency is essentially a correction factor used for the comparison of practical stages to the
ideal stage model at equilibrium.
𝑁
𝐸0 = 𝑁𝑡 [24]
𝑎
In Equation 24, 𝐸0 is the tray efficiency, 𝑁𝑡 is the number of equilibrium stages
calculated in the analysis, and 𝑁𝑎 is the number of actual stages required for the separation.
Experimental Plan:
The batch distillation experiment ran for a total of 120 minutes. During that period,
measurements of properties of the bottom and overhead streams of the Oldershaw column were
recorded. The experiment ran under finite reflux at a set reflux ratio and Variac voltage. The
initial charge composisiton was also fixed in the experiment. A complete summary of the fixed,
manipulated, and measured variables can be seen below in Table (X).
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Table 1: Experimental Plan
Results and Discussion
The main objective of this experiment was to study the performance of the Oldershaw
Distillation Column under a finite reflux of one for the separation of ethyl alcohol from water.
As the distillate was removed from the column, the volume of the distillate, temperatures of the
top and bottom of the column, and weight percents of ethanol in the distillate and still pot were
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recorded. The volume of the distillate was plotted as a function of time in Figure 4 and then used
to determine the flow rates of the distillate in Figure 5 below.
Cumulative Distillate 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)
Figure 4: Volume of the Distillate sample removed from the system as function of time
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Distillate Flow Rate

700
600
500
FLow Rate (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)
Figure 5: Distillate flow rate as a function of time
The rate at which the distillate sample flowed out of the system becomes more linear after the
first half hour of running the experiment. The flow rate is also seen to level out after the first
half hour while also having decreased significantly from the original flow rate at t1. The
distillate flow rate was then used to determine the reflux flow rate and overhead vapor flow rate
using the reflux ratio. The reflux ratio used in this experiment was 30 seconds to 30 seconds or
1. This means the reflux flow rate is equal to the distillate flow rate and the overhead vapor rate
is just twice the distillate flow rate since it is the sum of the distillate flow rate and the reflux
flow rate. The flow rates were graphed in Figure 6 below to show the comparison between them.
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Flow Rate of Distillate, Reflux, and Overhead Comparison

1200
1000
800
Flow Rate (mL/hr)
600 Distillate
Reflux
Overhead
400
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)
Figure 6: Comparison of flow rates between the distillate, reflux, and overhead vapor
Because the column refluxes at a ratio of 1, the distillate and reflux flow rates overlap in Figure 6
above. The flow rates become constant over time as the concentration of ethanol in the column
decreased. The temperature of both the top of the column and the still pot were then plotted as a
function of time in Figure 7 below.
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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)
Figure 7: Still pot and overhead temperature plotted as a function of time
The temperature in the still pot gradually approached the boiling point of water over the course
of the experiment. The temperature of the overhead vapor rose sharply between 20 and 30
minutes and then slowly approached the boiling point of water. This trend mirrors the trend
found when the concentration of ethanol is plotted as function of time as in Figure 8. The
concentration of ethanol in the distillate experiences a sharp decrease between the 20 and 40-
minute marks and then from there continues to decrease but at a slower rate. The concentration
of ethanol in the still pot decreases gradually over the entire duration of the experiment and does
not experience the same sharp decline around the 20 minute mark like the concentration or
temperature in the distillate does. This shows that the temperature is directly related to the
ethanol concentration remaining; as the concentration decreases, temperature increases towards
the boiling point of water.

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Concentration of Ethanol
0.8 0.025
0.7
0.02
Concentration (mol/mol)
0.6
0.5
0.015
0.4
Distillate
0.3
0.01
Still Pot
0.2
0.005
0.1
0 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)
Figure 8: Distillate (left axis) and still pot (right axis) concentration of ethanol as a function of
time.
There was a jump in the initial concentration in both the distillate and still pot that could have
been caused by the process not running for a long enough period before removing distillate. This
was caused by the column operating at an initial dynamic steady state where the actual steady
state oscillates around a mean value. The concentration plotted in Figure 8 was determined using
Equation 5 and 6 along with the weight percent of ethanol in water that was measured by the
densitometer. The weight percent and concentrations are found in Table 2 below.
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Table 2: Weight percents and mole fractions of ethanol in the distillate (Top/yD) and in the still
pot (Bottom/xW)
Time (hr) Top (wt%/wt) Bottom (wt%/wt) yD xW
0 85.1 4.62 0.6907 0.01859
0.1667 88.81 5.34 0.7563 0.02158
0.3333 78.43 4.96 0.5871 0.02000
0.5 65.87 4.62 0.4301 0.01859
0.6667 62.01 4.54 0.3896 0.01826
0.8333 60.9 3.9 0.3785 0.01562
1.1667 54.77 3.19 0.3214 0.01272
1.5 50.02 2.75 0.2813 0.01094
1.8333 45.73 2.25 0.2478 0.00892
2 42.74 1.97 0.2259 0.00780
The Rayleigh analysis was applied to the data using trapezoidal integration in order to determine
a theoretical volume of still pot residue remaining. The trapezoidal sum and final still pot
volumes are given in Table 3 below. The percent difference between the Rayleigh still pot
volume and the actual still pot volume was 4.64%.
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Group 2 Period I
Table 3: Rayleigh still pot volume analysis.
Trapezoidal Sum -0.036958446
exp(sum) 0.9637
Wfinal (mL) 5782.30
Wfinal.actual (mL) 5520
% Difference 4.6415
The theoretical average concentration of the distillate was determined using Equation 18 and is
displayed in Table 4 below where W0 is the initial charge before heat up and xW0 is the
concentration of the initial charge before heat up. The actual average of xD was found to have a
percent difference of 4.17% from the theoretical average. We assumed column hold up was
negligible for material balances.
Table 4: Rayleigh distillate concentration average analysis.
xD.avg 0.4493
xD.actual avg 0.4309
% Difference 4.1736
Equation 19 from Block was then applied to the data to predict the distillation time. The overall
Block time and actual total time is given in Table 5 below and the percent difference was
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Group 2 Period I
determined to be 35.3% higher than the actual. Each Block distillation time was plotted against
the actual time in a parity plot shown in Figure 9 below.
Table 5: Block equation analysis
Block Time (hr) 2.857
Time (hr) 2
% Difference 35.29
Block Equation Parity Plot

3
2.5
2
Block Time (hr)
1.5
Block Time
Actual Time
1
0.5
0
0.0 0.2 0.4 0.6 0.8 1.0 1.2 1.4 1.6 1.8 2.0
Actual Time (hr)
Figure 9: Parity plot of Block distillation time plotted against the actual time.
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Group 2 Period I
A McCabe-Thiele analysis was conducted in order to determine tray efficiency and theoretical
still pot concentration. A vapor-liquid equilibrium curve for EtOH/water at one atmosphere was
plotted on a y-x diagram for all the McCabe-Thiele figures. The operating lines were plotted
from yD at that time on the 45° y-x line. All operating lines had a slope equal to L/V as
described in Figure 3, which for this experiment was ½. The operating lines at all times are
plotted in Figure 10 below.
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Group 2 Period I
McCabe-Thiele for All Operating Lines

1
0.9
0.8
0.7 Equilibrium
X-Y
0.6 T=0 min

T=10 min
Y (mol/mol)
T=20 min
0.5
T=30 min
T=40 min
0.4 T=50 min
T=70 min
0.3 T=90 min

T=110
T=120 min
0.2
0.1
0
0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1
X (mol/mol)
Figure 10: McCabe-Thiele for all operating lines.
For each operating line, a separate McCabe-Thiele diagram was plotted and steps were drawn
from the starting yD (equal to xD on the 45° line) to the equilibrium line and then down to the
operating line and repeated until the difference in the steps are too small. The resulting number
of steps on the McCabe-Thiele is equal to the theoretical number of plates required at that
28
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Group 2 Period I
starting concentration. The McCabe-Thiele diagrams for t0, t1, and t9 are shown below in
Figures 11, 12, and 13 respectively. The other diagrams are in Appendix B.
T=0 min McCabe-Thiele

1.2
0.8
Y (mol/mol)
Equilibrium
0.6 Rectifying Line
Stages
XD
XW
0.4
0.2
0
0 0.2 0.4 0.6 0.8 1
X (mol/mol)
Figure 11: McCabe-Thiele at t=0 minutes.
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Group 2 Period I

1
0.9
0.8 Equilibrium
Rectifying Line
0.7
Stages
XD
Y (mol/mol)
0.6
0.5
0.4
0.3
0.2
0.1
0
0 0.2 0.4 0.6 0.8 1
X (mol/mol)

1.2
0.8
Y (mol/mol)
Equilibrium
0.6 Rectifying Line
Stages
0.4 XD
XW
0.2
0
0 0.2 0.4 0.6 0.8 1
X (mol/mol)

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Group 2 Period I
As the experiment ran, the number of theoretical trays required for separation decreased from a
maximum of 10 trays to a minimum of 2 trays. The efficiency of the distillation column was
calculated using Equation 24 and then the calculated xw was determined from each McCabe-
Thiele diagram at the final step down. The stages, efficiency, and still pot concentrations are in
Table 6 below.
Table 6: McCabe-Thiele Analysis of Tray Efficiency
time (hr) No. Stages Actual Eo xW(t) predicted xW(t) measured
0.0000 6 11 0.545 0.06932 0.01859
0.1667 10 11 0.909 0.10090 0.02158
0.3333 3 11 0.273 0.05504 0.02000
0.5000 2 11 0.182 0.03226 0.01858
0.6667 2 11 0.182 0.02661 0.01823
0.8333 2 11 0.182 0.02527 0.01562
1.1667 2 11 0.182 0.01915 0.01272
1.5000 2 11 0.182 0.01596 0.01093
1.8333 2 11 0.182 0.01341 0.00892
2.0000 2 11 0.182 0.01179 0.00779
The efficiency was plotted as function of time in Figure 14 and the predicted concentrations in
the still pot were plotted against the measured concentrations in Figure 15 below. The efficiency
of the column starts at 54.5% and decreases over the course of the experiment, having a
maximum of 90.9% and a minimum of 8.2%. The concentrations in Figure 15 are labeled with
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Group 2 Period I
their respective times for t0 through t3 because the concentration increases from t0 to t1. The
concentrations for t4 through t9 decrease as time increases.
Tray Efficiency
1
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)
Figure 14: Tray Efficiency as a function of time.
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Xw Parity Plot
0.1
0.08
Xw Measured (mol/mol)
0.06
0.04
t2 t0 t1
0.02 t3
t4-t9
0
0 0.02 0.04 0.06 0.08 0.1
Xw Predicted (mol/mol)
Figure 15: Parity plot of still pot concentrations predicted from McCabe-Thiele analysis.
Conclusions:
The distillate flow rate out of the Oldershaw Distillation column started off high and
decreased rapidly in the first thirty minutes of the experiment. As the distillation continued, the
flow rate decreased at a slower rate and then eventually became constant as the concentration of
ethanol in the column decreased. When comparing the temperature of the still pot and the
overhead, little to no temperature change is observed in the first fifteen minutes. Between 15-40
minutes, the temperature in the overhead increased rapidly. After the 40 minute mark, the
temperature in both the still pot and the overhead converge and slowly approach the boiling point
of water over the course of the experiment as ethanol is continuously removed in the distillate.
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Group 2 Period I
The predicted values from Rayleigh’s Analysis of 𝑊𝑓𝑖𝑛𝑎𝑙 and 𝑥𝐷,𝑎𝑣𝑔 were found to be consistent
with experimental values. A percent difference of 4.642% and 4.174% were found for the
predicted and experiment values of the final still pot volume and 𝑥𝐷,𝑎𝑣𝑔 respectively. However,
use of the Block equation to predict the time required for the separation proved to be a poor
estimation with a percent difference of 35.3% from the predicted Block equation time and the
actual time experienced for the separation in the study due to the column operating at dynamic
steady state during the start of the study. Further analysis of the column’s effectiveness was
conducted using the McCabe-Thiele Analysis to determine tray efficiency and to predict the
concentration of ethanol in the still pot as a function of time. McCabe-Thiele Analysis suggests
that as the batch distillation runs, and as the concentration of EtOH decreases, less and less
stages will be required to separate the remaining ethanol starting with 6 stages and going down to
2 stages. The tray efficiency was found to decrease from 54.5% to 18.18%, excluding the point
at t=10 min where the efficiency jumped to 90.91%. It should be noted that this spike in tray
efficiency can also be seen in the operating line at the 10 minute interval in the McCabe-Thiele
Analysis that is above the previous time interval’s (t=0min) operating line. The abnormality in
the analysis can be attributed to the column being at dynamic steady state at the start of the
study. Reflux increased slightly during this period and caused the abnormalities in the tray
efficiency and the McCabe-Thiele figures. Finally, the parity plot of the measured and predicted
values of the concentrations in the still pot showed poor correlation. The measured
concentration was lower than the values predicted by McCabe-Thiele. However, as time
increased and the column reached steady state, the McCabe-Thiele analysis did a better job at
predicting concentration values.
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Group 2 Period I
Literature Cited:
1. Helmenstine, P.A. (n.d.) Understand How Distillation Works. Retrieved October 01, 2017, from
https://www.thoughtco.com/what-is-distillation-601964
2. 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/j.jclepro.2016.04.140
3. 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/j.cep.2015.11.003
4. Seader, J.D. and Henley, Ernest J., Separation Process Principles. John Wiley & Sons, New York,
1998.
5. Batch Distillation- No Author. <homedistiller.org/Lecture15-Batchdist.ppt>
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Appendix A: Sample Calculations
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Appendix B: Figures

1.2
0.8
Y (mol/mol)
Equilibrium
0.6 Rectifying Line
Stages
0.4 XD
XW
0.2
0
0 0.2 0.4 0.6 0.8 1
X (mol/mol)

1
0.9
0.8 Equilibrium
Rectifying Line
0.7
Stages
0.6 XD
Y (mol/mol)
0.5
0.4
0.3
0.2
0.1
0
0 0.2 0.4 0.6 0.8 1
X (mol/mol)
39
6 October 2017
Group 2 Period I

1.2
0.8
Y (mol/mol)
Equilibrium
0.6 Rectifying Line
Stages
0.4 XD
XW
0.2
0
0 0.2 0.4 0.6 0.8 1
X (mol/mol)

1.2
0.8
Y (mol/mol)
Equilibrium
0.6 Rectifying Line
Stages
0.4 XD
XW
0.2
0
0 0.2 0.4 0.6 0.8 1
X (mol/mol)
40
6 October 2017
Group 2 Period I

1.2
0.8
Y (mol/mol)
Equilibrium
0.6 Rectifying Line
Stages
0.4 XD
XW
0.2
0
0 0.2 0.4 0.6 0.8 1
X (mol/mol)

1.2
0.8
Y (mol/mol)
Equilibrium
0.6 Rectifying Line
Stages
0.4 XD
XW
0.2
0
0 0.2 0.4 0.6 0.8 1
X (mol/mol)
41
6 October 2017
Group 2 Period I

1.2
0.8
Y (mol/mol)
Equilibrium
0.6 Rectifying Line
Stages
0.4 XD
XW
0.2
0
0 0.2 0.4 0.6 0.8 1
X (mol/mol)

1.2
0.8
Y (mol/mol)
Equilibrium
0.6 Rectifying Line
Stages
0.4 XD
XW
0.2
0
0 0.2 0.4 0.6 0.8 1
X (mol/mol)
42
6 October 2017
Group 2 Period I

1.2
0.8
Y (mol/mol)
Equilibrium
0.6 Rectifying Line
Stages
0.4 XD
XW
0.2
0
0 0.2 0.4 0.6 0.8 1
X (mol/mol)

1.2
0.8
Y (mol/mol)
Equilibrium
0.6 Rectifying Line
Stages
0.4 XD
XW
0.2
0
0 0.2 0.4 0.6 0.8 1
X (mol/mol)
43
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Group 2 Period I
Appendix C: Laboratory Notebook
44
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Group 2 Period I
Appendix D: Documentation
45
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Group 2 Period I
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Appendix E: Statistical Design of Experiment
Experimental Design:
For this experiment, the three manipulated variables are Heat Rate (A), Reflux Ratio (B),
and Volume Ratio (C) as shown in the table below and a 23 factorial was used for this
experimental design. This particular factorial model requires 8 trials to study the effect of the
manipulated variables. Calculations were carried out as shown in the response table attached, and
graphs were made accordingly. The effects graph shows the effect of the variables on the volume
where Volume Ratio (C) was found to have the greatest effect followed by Heat Rate (A), and
then Reflux Ratio (B).
Given: Manipulated variable

Batch Distillation Factorial Design
Heat Reflux Volume
Rate (V) Ratio Ratio
1
(Low) 90 1.0 0.25:5.75
2
(High) 110 1.5 0.50:5.50
Response Table:
68
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Group 2 Period I
Effects Plot
Data
-1 1 avg.
A 139.25 283.5 211.375
B 257.25 165.5 211.375
C 185 237.75 211.375
AB 232 190.75 211.375
AC 195.25 227.5 211.375
BC 213.25 209.5 211.375
ABC 219 203.75 211.375
AC Interaction Plot
Data
A C avg
1 1 160 298 229.00000
1 2 169 402 285.50000
2 1 98 184 141.00000
2 2 130 250 190.00000
C1 C2
B1 229.00000 B1 285.50000
B2 141.00000 B2 190.00000
AB Interaction Plot Data

A B avg
1 1 160 169 164.5
1 2 98 130 114
2 1 298 402 350
2 2 184 250 217
B1 B2
A1 164.5 A1 114
A2 350 A2 217
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Group 2 Period I
BC Interaction Plot Data

B C avg
1 1 160 98 129.00000
1 2 169 130 149.50000
2 1 298 184 241.00000
2 2 402 250 326.00000
C1 C2
A1 129.00000 A1 149.50000
A2 241.00000 A2 326.00000
Diagrams:
Diagram (1): Effects of Manipulated Variables
Effects
300
250
200
150
Vol (mL)
100
50
0
A B C AB AC BC ABC
Diagram (2): AB Interaction
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Group 2 Period I
Vol (mL)
356
306
256
206
156
106
56
6
A1 A2
Diagram (3): BC Interaction
355
305
255
205
155
105
Vol (mL)
55
5
B1 B2
AC Interaction
400
350
300
Vol(mL)
250
200
150
100
50
0
A1 A2
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6 October 2017

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Batch Distillation with Rectification:

Separation of Ethanol and Water Using an Oldershaw

To: Dr. James A. Ritter

Date: October 6, 2017

Oldershaw Distillation Column

Oldershaw Distillation Column is analyzed for its effectiveness as a method of separation of

The objective of this experiment is to study the performance of the Oldershaw

these predicted values to those found experimentally.

Experimental Objectives ................................................................................................ 5

Literature Review ........................................................................................................... 5

Apparatus and Procedure ............................................................................................... 7

Engineering Principles and Working Equations .......................................................... 10

Experimental Plan ........................................................................................................ 17

Results and Discussion ................................................................................................. 18

Literature Cited and References ................................................................................... 33

Appendix A: Sample Calculations

Appendix C: Laboratory Notebook

Appendix E: Statistical Design of Experiment

Distillation, also known as fractionation or fractional distillation, is one of the most

liquid and can be reversed in order to separate gasses [1].

many types of distillation such as azeotropic distillation, extraction distillation, vacuum

follow the main idea of mass separations.

further and further as the component moves up the column.

the column, and find the theoretical distillation time, respectively.

achieved by switching valves.

holdup for different feeding concentration increases [3].

Apparatus and Procedure:

column. This idea can be seen in Figure 1 below.

Figure 1: Example of a distillation column design

Figure 2: The Oldershaw batch distillation column and apparatus

before data collection began.

Engineering Principles and Working Equations:

compositions are analyzed using a DMA 48 Density/Specific Gravity/Concentration Meter with

an ethanol/water calibration curve.

be determined at varying distillate flow rates.

weight of water (𝑀𝑊𝑊 ) via Equation 5 and 6 respectively.

the still pot.

flowrate in the distillate. This is defined by Equation 8.

Equation 9 is achieved by combining Equations 7 and 8.

Equation 9 is simplified by multiplying through by 𝑑𝑡.

𝑊𝑑𝑥𝑤 + 𝑥𝑤 𝑑𝑊 = 𝑦𝐷 (−𝐷𝑑𝑡) [10]

distillate flow rate leaving the column.

Substituting Equation 11 into Equation 10 derives Equation 12 below that is easily

the still pot.

Trapezoidal Rule as shown in Equation 15.

respective molar fraction term.

𝑊0 𝑥𝑊,0 = 𝐷𝑥𝐷,𝑎𝑣𝑔 + 𝑊𝑥𝑊 [17]

constant reflux to run to completion, the equation due to Block is used.

𝐿𝑛−1 𝑥𝑛−1 + 𝑉𝑛+1 𝑦𝑛+1 = 𝐿𝑛 𝑥𝑛 + 𝑉𝑛 𝑦𝑛 [20]

Thiele analysis as defined below.

distillate flowrate (𝐷).

𝑥𝑊 as predicted by the McCabe-Thiele analysis. This process is demonstrated in the figure

ideal stage model at equilibrium.

In Equation 24, 𝐸0 is the tray efficiency, 𝑁𝑡 is the number of equilibrium stages

manipulated, and measured variables can be seen below in Table (X).

Table 1: Experimental Plan

Results and Discussion

to determine the flow rates of the distillate in Figure 5 below.

Cumulative Distillate Volume

Distillate Flow Rate

Figure 5: Distillate flow rate as a function of time

Flow Rate of Distillate, Reflux, and Overhead Comparison

function of time in Figure 7 below.