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Tianna Drew

Squad 4 ChE 433


The Dream Team
University of Idaho

October 29, 2013

Dr. Eric Aston
Lab Instructor
Department of Chemical and Materials Engineering
University of Idaho

Dear Dr. Aston,

On October 15
th
, 2013 the Dream Team, consisting of Zach Campbell, Matt Chapin, and myself,
conducted a distillation laboratory experiment under your supervision and guidance. The purpose of
conducting this experiment was to provide a customer with a product, namely isopropanol with
minimum impurities. This was a multi-component separation process using a liquid feed stream
containing water, 2-butanol, isopropanol, and methanol. Our goal was to recover (in the bottoms
stream) 80% of the isopropanol that was in the original feed. There were two adjustments made to the
reflux ratio before final samples at each stage were taken. The samples were run through a gas
chromatograph. The final reflux ratio was adjusted to 0.93, resulting in a recovery percentage of 89.2%
isopropanol in the bottoms product. ChemSep gave a reflux ratio of 5.2, which was very different from
the reflux ratio obtained experimentally. It was concluded that the experiment be run with a pump
speed of less than 20 to meet the required specifications. A formal report explaining specific methods
and results is attached.
Sincerely,

Tianna Drew

Cc: Matt Chapin, Zach Campbell
LABORATORY REPORT SUBMITTED TO: DR. ERIC ASTON
Multi-component
Distillation
A Report By: Tianna Drew

Experiment Completed By: The Original Dream Team
Zach Campbell, Matt Chapin, and Tianna Drew
10/29/2013




The following is a formal report addressing the methods, data, and conclusions resulting from a
laboratory experiment utilizing the separation process of a distillation column. The major objectives of
the lab were to first separate isopropanol (IPA) to a recovery % of 80 from a liquid feed containing
water, 2-butanol, methanol, and IPA, and to compare the data recovered from the experiment to
theoretical data developed in ChemSep. Sample compositions were determined by using a thermal
conductivity detector gas chromatograph. The report explains in detail the actions implemented in order
to achieve the goals presented.

1

Table of Contents

Introduction..Page 2
Methods..Page 3
Results and DiscussionPage 4
Conclusions and Recommendations.Page 7
Bibliography.....Page 8
Nomenclature..Page 9
Appendices........................................................Page 10

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INTRODUCTION
In this experiment, a method of attaining isopropyl alcohol (IPA) with a low concentration of impurities
was needed to provide to a customer. Some customers, like this one, will pay for IPA because they really
need it, but will only pay for a specific purity. Distillation was used to separate a liquid mixture
containing 50% methanol, 35% IPA, 13% 2-butanol and 2% water. Distillation can be used to separate
these components because they each have a unique boiling point, and the boiling points are what are
used to physically part the mixture. The feed into the distillation column was the aforementioned liquid
mixture that was heated into the vapor phase and then re-condensed later, causing the chemical
composition of the stream to change. This is due to varying volatilities, and makes it easy to divide the
chemicals.
In order to recover the target IPA composition of 80% in the bottoms stream (the first objective), a
simulation of the column at total reflux was first performed in ChemSep. This computer trial was to see
if the objective composition was an attainable goal, determine the maximum separation between top
and bottom, and to supply the initial conditions of the column, to be adjusted later. The maximum
separation was experimentally determined by running the distillation column at total reflux.
Based on the ChemSep theoretical modeling predictions, the column was run and eventually there
were adjustments that needed to be made. The specifications given from the computer program were
to be compared to the settings of the column for the second purpose of this lab, along with fitting the
data recovered from taking feed rate and stage composition samples.
A diagram of the operation used is provided in figure 1. The distillation column has eight stages, plus the
total condenser and partial re-boiler.
Figure 1. P&ID of the distillation column.

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METHODS
THEORETICAL
In order to achieve a product with 80% IPA theoretically, ChemSep was used. The main
parameter altered was boil-up ratio. The boil-up ratio (R) is the ratio of the flow of vapor being reused
(L) to the flow of the bottoms (D). The reflux ratio (R) changed according to the calculations that the
program performed. The reflux ratio is the flow of the liquid being reused (V) to the flow of the distillate
(B). An efficiency of 75% was assumed, and Raoults law was used with Antoines equation to find the K
value and enthalpy assumptions. ChemSep did the calculations and spit out the numbers without any
Dream Team brain power required.
EXPERIMENTAL
A distillation column with eight stages in addition to a partial re-boiler and total condenser, with a fixed
feed stage of five was the apparatus used. It used bubble cap trays for its stages and the column was
steam-heated. The reflux ratio had to be adjusted twice to get close to the predicted composition top
and bottom values. Each adjustment requires down time to reach stead-state. There were
thermocouples at each stage, sending temperature data to the same computer that adjusts the steam
pressure and feed temperature. The profile was the indicator as to whether the column had reached
steady state. Unfortunately the Dream Team did not remember to save the temperature profile from
said computer before turning everything off.
Adjustable parameters:
1) Feed Rate (Volumetric flow)
2) Steam Pressure (Electronically controlled)
3) Feed Temperature (Electronically controlled)
4) Reflux Ratio (Used centrifugal pump)

A thermal conductivity detector - gas chromatograph (TCD-GC) was used to reveal the composition of
the two samples, one vapor and one liquid, that were taken from each tray at the final adjusted
steady state, along with the bottoms and tops samples from each adjustment of the column. The TCD
measures the change in thermal conductivity of the carrier gas (helium) caused by the sample being
analyzed. The machine then sends the data to a computer program, where it produces curves
representing each chemical component. The areas under the curves were calculated (by the program,
again no brain power) and plugged into an excel sheet with pre-entered formulas. The result of these
computer calculations are the compositions of each component, which were then recorded as raw data
to use in the data analysis portion of the experiment.
In order to determine the recovery of IPA, the feed composition, bottoms composition, and the flow
rates for the feed, tops, bottoms, and reflux were used. The flows were measured using a stopwatch
and different forms of graduated cylinders. For the first attempt, the reflux pump speed at total reflux
was set at 39, and the top and bottom samples were tested for IPA content. The speed was adjusted
two more times, to 25 and 20 (mL/x) in an attempt to reach 80% IPA in the bottom. There was a 30-

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minute wait between each adjustment so the column had time to reach steady state. At the final
setting, the Dream Team cautiously took samples from the tops, bottoms, and liquid and vapor streams
from each stage and the flow rates were measured. This was done wearing goggles and gloves to ensure
the safety of the group. It was then noticed upon taking samples from the stages toward the top of the
column that a valve was left open from the group that used the column previously.
RESULTS AND DISCUSSION
In the flowing tables, the compositions are in percentage form. Table 1 depicts the actual feed
composition used in the lab, according to the TCD.

Table 1.



At total reflux the compositions were taken to see what adjustments needed to be made. Table 2 shows
the results of the TCD analysis. Table 3 shows the same information after the pump speed was altered to
25. This data is not used in the final calculations, it just gives an idea of how to adjust the column.

Table 2.



Table 3.



Tables 4a and 4b are the complete raw data from the final adjustment of the column, at a pump speed
of 20mL/x, a feed rate of 90mL/min, a tops rate of 38.28 mL/min and a bottoms rate of 55.66mL/min.
The symbol L indicates the liquid stream as the symbol V indicates the vapor stream.

Component Feed Composition
Water 1.35
MeOH 40.97
IPA 40.78
2-But 16.9
Component Bottom composition Top composition
Water 2.5 0.41
MeOH 12.04 94.29
IPA 56.11 4.92
2-But 29.36 0.38
Component Bottom composition Top composition
Water 2.7 1.05
MeOH 13.37 89.03
IPA 56.8 9.79
2-But 27.13 0.13

5

Table 4a.

Table 4.b
Liquid compositions

Stage 1 2 3 4 5 6 7 8
Water 4.79 5.46 5.68 5.31 6.33 6.84 5.99 3.88
MeOH 23.84 27.18 37.18 45.46 52.4 47.28 59.1 69.29
IPA 57.08 56 48.53 41.97 37.71 42.95 33.32 25.95
2-But 14.3 11.35 8.6 7.26 3.56 2.93 1.59 0.87

Table 4.c
Vapor compositions

Stage 1 2 3 4 5 6 7 8
Water 6.53 6.12 5.61 5.33 5.06 6.84 5.6 6.42
MeOH 35.68 44 49.18 57.39 63.88 46.06 67.04 66.28
IPA 50.59 44.98 41.1 34.08 29.33 44.02 26.48 26.89
2-But 7.2 4.9 4.11 3.2 1.73 3.08 0.88 0.59

The percent recovery is found by the following general equation: (Bottoms flow rate * bottoms
composition IPA)/ (feed flow rate * feed composition IPA). The reflux rate is simply the reflux flow
divided by the tops flow rate. Values for the % recovery and reflux ratio are given in table 5.
Table 5.
Pump
mL/x
Reflux
mL/min
Top
mL/min
Bottom
mL/min
Feed
mL/min
Reflux
Ratio
Recovery
%
20 35.72 38.28 55.66 90 0.93 89.2

The feed rate is supposed to equal the top flow rate plus the bottom flow rate for a mass balance of the
system, but the flow rates of the top and bottom were measured at a different time than the feed rate,
and this causes the error in the balance. If the flow rates were measured using the same size graduated
cylinder for the same amount of time, a more accurate mass balance can be obtained.
Component Bottom composition Top composition
Water 1.06 2.7
MeOH 6.49 75.76
IPA 58.46 21.16
2-But 33.39 0.32

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The final reflux ratio was 0.93, as shown in table 5. The original ChemSep model, it was found to use a
reflux ratio of 5.2. Obviously adjustments were made in order to obtain the target recovery of 80% IPA
in the bottoms product.

Figure 2. McCabe-Thiele Diagram, which indicates that the feed plate location of 5 in a total of 10 stages
is a reasonable stage to enter the distillation column to reach the separation goal.

Figure 3. This graph indicates the percentage of IPA in each stage. The condenser is shown as stage 10,
and the re-boiler, where the product is taken from, is shown as stage 1.
0
10
20
30
40
50
60
70
0 1 2 3 4 5 6 7 8 9 10
M
o
l
e

F
r
a
c
t
i
o
n

Stage
Composition of IPA by Stage (L/D=0.94)
L
V

7

Examining figure 3, it was found that compared to all stages, stage seven of the process clearly exhibited
some abnormal behavior. This could be because when taking samples from the higher stages, a cooling
device with a pump was used to collect the sample, and there may have been some impurities in the
collecting tube on that particular stage. Another possible reason for this behavior could be that at this
temperature, certain chemicals in the mixture could have interacted differently with each other,
possibly forming azeotropes.
The assumptions made in ChemSep that would have affected the overall results are using an ideal
model (in this case, Raoults law and Antoines equations), and neglecting heat loss. No system is ideal,
especially in this case where its about 25 years old (?) and has leaks and isnt insulated (no offense).
Another assumption was that everything was done at one atmosphere, when in reality that isnt 100%
accurate, but this assumption doesnt affect the overall results as much as the previous two
assumptions.
CONCLUSION AND RECOMMENDATIONS
The goal percentage recovery of isopropanol was not quite achieved upon completion of the distillation
experiment. In order to achieve this recovery, the column has to be run at a different reflux ratio, and
therefore a different pump speed. In order to calculate this speed and ratio, a linear relationship must
be established between the pump speeds used and the reflux ratios resulting from these speeds.
Information required for creating such a relationship includes the flow rates at each pump setting.
Unfortunately the only flow rates recorded were at the final adjustment of 20 mL/x. The pump certainly
should be run at a slower setting, but not too much slower considering the recovery was only 9% higher
than it should have been. There were a few hiccups in the process of determining the final value, for
example when some of the higher stage samples were being taken, it was discovered that a valve had
been left open when the column had been last operated. There was a random bump in the temperature
log, the log which normally would be attached in Appendix A, shortly before the column reached steady
state after the final adjustment. The sample compositions for stage 7 were abnormal as well.
In order to improve the methods and results in the multi-component separation experiment in the
future, several measures can be taken. It would be of much benefit if there was a more accurate way to
measure the flow rates of each stream, and possibly at the same time, for instance adding a flow-meter
to the apparatus and even have it connected to the computer to electronically record the flow rates.
The glassware, although large and complex, could use an upgrade. There are slow leaks which if repaired
could be a temporary fix rather than upgrading the whole column. A ChemSep calculation after
knowing the initial composition of the feed stream would have been useful to have, unfortunately the
feed stream composition can be different every day. An inspection of valves and other glassware should
be conducted before starting the lab. All in all, the distillation column is an informative and useful
introduction to equipment and procedures to be used in the real world, but because the recovery had
an error of 11.25%, I would not recommend selling this product to the customer.


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BIBLIOGRAPHY
1) Wankat, Phillip C. Separation Process Engineering, 2
nd
Ed., Prentice Hall, 2006.
2) P&ID created by Kelli Quist.
3) ChemSep distillation column simulation computer software


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NOMENCLATURE
B Bottom product flow rate
D Distillate product flow rate
F Feed flow rate
L Reflux flow rate
R Reflux ratio
R
V
Boil-up ratio


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APPENDIX A
(Pretend temperature profile)