NORTHEASTERN UNIVERSITY

Department of Chemical Engineering

CHME 3313 Transport 2 Laboratory March 25th, 2016
TO: Professor Roy
FROM: Kiersten Campbell
SUBJECT: Batch Distillation Technical Report

Abstract:

In this experiment, the main objective was to study the inner-workings of a batch distillation
column process, and to determine the most efficient conditions for separating a water and
denatured alcohol mixture and achieve pure results. This was done by testing four different
combinations of alcohol concentration and system pressure to determine which yielded the purest
results. The distillation column was analyzed by viewing it as two separate processes (simple
distillation, and fractional distillation.) It was expected that a high concentration of alcohol and a
high pressure would yield the purest results, but it was experimentally determined that the lowest
concentration and highest pressure were the best solution to the problem. The water samples from
the Tank and Stage 1 had densities closest to 1 g/cm3, staying consistent around 0.995 g/cm3 toward
the end of the hour-long distillation. The denatured alcohol samples (Reflux and Distillate) at the
top of the column yielded densities that stayed most consistently close to 0.805 g/cm3, from about
0.795 g/cm3 to 0.806 g/cm3.

Background:

Batch distillation is an unsteady state process in which a mixture is distilled to separate it into its
component fractions. Generally, a fixed amount of mixture is put into a still, or tank, and vapors
pass upward through the distillation column as the mixture components reach their boiling points
during heating. The vapor of the component with the lower boiling point condenses to be collected
at the top of the column. Some is returned to the column as reflux, or withdrawn as distillate. [1]

There are various types of designs of distillation columns, differing in size as well as type of
distillation. In this specific experiment, both simple and fractional distillation occur. Simple
distillation is often performed for two liquids that are not particularly close in boiling point. As the
name suggests, the mixture is boiled and the component with the lower boiling point condenses
on the walls of the column for collection. Fractional distillation requires a more complex apparatus,
as it is used for separating components closer in boiling point. A longer column allows the liquid
to vaporize and condense multiple times, often going through a packed bed section, in which
metal pieces or other materials are used to increase the condensation surface area. This type of
distillation is used to ensure a pure product at the top of the column. [2]

The purpose of this experiment is to optimize the separation of water from a mixture of denatured
alcohol and water. By changing the operational components of the process, the most efficient
combination of alcohol concentration and system pressure are able to be determined. This will be
done by performing multiple trials of different combinations, and comparing the densities of the
samples from different outlet points in the distillation apparatus.

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This experiment requires a high pressure steam boiler to heat the process fluid to steam for
separation. The difference in boiling points for the denatured alcohol and water allows for the
separation to happen. In the boiler, the fluid is vaporized and continued to be heated at a high
pressure, ranging specifically from 16-25 psig. This presents safety concerns, as if steam escapes,
it could cause harm if one were to come into contact with it.

The steam then enters the distillation column, where the vapor will be converted back into a liquid
for separation. This distillation column utilizes the packed bed design, in which it is packed with
saddle-shaped metal materials. The packing provides a large surface area for vapor-liquid contact
and makes it more effective. When the packing comes into contact with the rising vapor steam, the
more volatile steam is picked up by the packing. This exits the column and enters a condenser to
be collected. The liquid at the bottom enters a reboiler, from which two streams exit. A vapor
stream returns to the column, and a liquid stream exits as a product. [3]

The quality of the distillation is measured by testing the density of the liquid products.

There were four trials done for this experiment run in the same fashion. The solution of water and
alcohol at the desired concentration was made based on calculations performed in the pre-lab stage.
The concentrations chosen to begin with were 15% alcohol (at 20 and 25 Psig) and 20% alcohol
(at 20 and 25 Psig.) After performing the provided start-up procedure, the mixture was charged
into the tank, and the system was turned on with collection samples being taken every 5 minutes
during the hour process. The Labview interface was also set up to measure temperature at different
locations in the column and tank. Additionally, condensate flow rate was measured at checkpoints
during the process as well. [4]

Results/Analysis:
There were three separate sets of data that were collected over the course of this experiment for
each trial: the densities at each timestamp for each of the four sample points, the average
temperatures for each probe location, and the condensate volume progression over the process.
There were some corrections that needed to be made in terms of the concentration of the water and
alcohol solution used in each of the trials. While the initial aim was to run two trials at 20%
denatured alcohol, and two trials at 15%, the density data collected and determined at Time 0 from
the tank did not correspond to those concentrations. To make the correction, the overall density
determined in the tank at Time 0 was plotted along the calibration curve determined in the pre-lab.
The output determined from there was the volume fraction of water in that specific sample.
Subtracting that value from 1 gave the volume fraction of the alcohol. From here, a simple mass
fraction equation was developed to determine the actual concentrations used:

=
+
Above, v is the volume fraction corresponding to alcohol and water. This concludes that the
trials actually run were as follows:

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Table 1: Actual Concentration/Pressure Combinations
Concentration of Alcohol Pressure (Psig)
15.5% 20
13.5% 26
16.0% 20
10.1% 25

The most qualitative data in terms of determining how well the water and the denatured alcohol
were separated were the density values. By taking samples every five minutes for the hour-long
trials, the trend of how the density increased or decreased (depending on sample location)
illustrated the amount of separation happening. However, due to the range of temperatures of the
samples, it was difficult to take the density readings at room temperature for consistency.
Therefore, the density samples taken outside the range of room temperature needed to be corrected
since it is known that density is dependent on temperature. This was done by using data found in
Perrys Chemical Engineers Handbook [5], in which there are values of density corresponding to
percent alcohol concentration as well as temperature. The figures below reflect the corrected
densities for accuracy.

Figure 1: Tank Sample Density

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In Figure 1, it can be noted that there are seven data points for the 16.0% trial that have been
singled out as outliers to this data set (in red.) This is due to the fact that the density of these
samples were taken when the temperature was above 40 C, above which the denseometer becomes
inaccurate.

1.01
1
0.99
0.98
Desnity (g/cm^3)

0.97
0.96 15.5% Conc 20 Psig
0.95 13.5% Conc 26 Psig

0.94 16.0% Conc 20 Psig

0.93 10.1% Conc 25 Psig

0.92
0.91
0.9
0 20 40 60 80
Time (min)

Figure 2: Stage 1 Sample Density

Figure 1 and 2 illustrate an increasing trend in denisty in all trials. This was expected because these
two samples are taken from the bottom of the distillation column. In other words, they are taken
where the water remains within the column. The vapor of the denatured alcohol continues to climb
up the column, while the more dense water returns to the liquid phase on the sides of the column
and drips back down to these two outlets (Tank and Stage 1.) The density increases toward 1 g/mL
(the density of pure water) as the alcohol evaporates toward the top of the column to be collected
from the reflux and distillate sample points.

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 0.808
0.806
0.804
0.802
Density (g/cm^3)

0.8
0.798 15.5% Conc 20 Psig
0.796 13.5% Conc 26 Psig

0.794 16.0% Conc 20 Psig

0.792 10.1% Conc 25 Psig

0.79
0.788
0.786
0 10 20 30 40 50 60 70
Time (min)

Figure 3: Distillate Sample Density

0.815

0.81

0.805
Desnity (g/cm^3)

15.5% Conc 20 Psig

0.8
13.5% Conc 26 Psig
16.0% Conc 20 Psig
0.795 10.1% Conc 25 Psig

0.79

0.785
0 20 40 60 80
Time (min)

Figure 4: Reflux Sample Density

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The density trends illustrated in Figures 3 and 4 are not as uniform as those for Tank and Stage 1.
However, there still remains an overall decrease in density, which qualitatively means that the
alcohol was indeed being separated from the solution. Due to the lower boiling point, the alcohol
vapor remained vapor and travelled up the distillation column, farther than the water vapor, to
eventually be cooled down and collected as a liquid. These densities approach 0.805 g/mL, the
density of pure denatured alcohol.
Over the course of this experiment, the volume of condensate collected in 30 seconds was
recorded, which allows conclusions to be drawn pertaining to the energy lost during each
experiment.

Figure 5: Volume of Condensate over Time

Figure 5 shows a consistent trend of decreasing condensate volume as the distillation process
progressed, for each concentration and pressure trial. At approximately 10 minutes, the flow rate
of condensate leaving the system leveled out and became steady for the remaining 50 minutes. The
condensate is often collected to be a measure of how much energy is being lost from the system in
the form of steam. In this system, the steam condensed at an outlet, but was not returned to the
system. Since this condensate enters the general surroundings of the room, it returns to atmospheric
pressure and flash steam is generated, causing a significant energy loss from the system.
There is a much greater amount of energy lost during the first ten minutes of the process, since
that is the time during which the steam boiler is using the most energy to heat up the system, hence
the volume of condensate collected being much higher then. As the process progresses, the system
is heated to a maximum temperature and the energy loss is lower since the overall energy required
for the system is lower.

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The final component of data collection during the experiment was the average temperature for
each probe at different locations in the distillation column at timestamps during the process. For
analytical purposes, the column was viewed as having two sections: one for simple distillation,
and one for fractional. The simple distillation happened more toward the bottom of the column,
while the fractional happened all the way up through the packed column. From this, a boiling point
graph was able to be created in all trials for both liquid and vapor water based on the temperature
readings in the tank, and at the steam outlet.

Figure 6: 20 psi and 15.5%

Figure 7: 26 psi 13.5%

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Figure 8: 16% 20 psi

Figure 9: 10.1% 25psi

The information to be gathered from this type of graph ideally is the concentration of the vapor
and liquid within the system at various temperatures. The curves shown in Figures 6-9 are not
ideal, and only reflect the boiling graphs for the part of the column characterized as simple
distillation and a solid trend is not able to be determined from this. The curves were not able to be
created correctly for fractional distillation because the calibration curves previously created were
off, and the y-intercept was too large. The y-intercept is supposed to represent pure alcohol, but it

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was higher than the pure alcohol density. This resulted in volume fractions with negative values,
which is not possible.
Conclusions/Recommendations:
There are some conclusions to be drawn about how alcohol concentration and system pressure
affect the efficiency of the separation of denatured alcohol and water. The goal of these
experiments was to find an ideal set of conditions in which this separation would happen to yield
the purest water and denatured alcohol. The best illustration of this is in the density analysis.
It was expected that the best combination for this separation would be a high concentration of
alcohol and high operating pressure. However, it can be concluded from the density graphs that
the instance that illustrates the purest (based on true values of water and alcohol density) is the
10.1% concentration and 26 Psig pressure. It can be noted that this was the highest pressure and
lowest concentration tested. This combination yielded the highest purity, and therefore is the best
solution to the problem statement.
For the samples gathered in the tank and at Stage 1, the density values for this instance get closest
to 1 g/cm3 (density of water.) The distillate and reflux samples for this instance stay closest to
0.805 g/cm3, the value determined for density of the pure denatured alcohol. The properties of an
azeotrope describe this, in that after distillation of a mixture the result is closer to the azeotrope
than the original. [6] A lower concentration of alcohol can better achieve more pure results.
Due to the time allowed and the scope of this experiment, there were a few parts of this lab that
were less than idea. The density corrections made to the data based on actual temperature could
have been avoided if the samples were able to be set aside for longer to return to room temperature.
This would yield more accurate density results and allow more analysis to be done into the exact
concentration of each sample. Additionally, the solutions made at the start of each trial seem to
have changed as the liquid was put into the tank. If this had been more accurate to the initial
experimental design, more concrete conclusions could have been made pertaining to the most
efficient concentration/pressure combination in separating the water and denatured alcohol.
It is recommended for further study that more combinations of alcohol concentration and pressure
be tested to acquire a larger set of conclusions. This would allow for the theory to be tested further
in determining the best system conditions for the separation to happen fully. It would also be
beneficial to the process to run the system for longer than 60 minutes to see if better quality (more
accurate to pure water or pure alcohol) density results can be yielded.

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 References

1. "Batch Distillation." Batch Distillation. Separation Processes, n.d. Web. 25 Mar. 2016.
2. "How to Explain Simple Vs. Fractional Distillation." How to Explain Simple Vs.
Fractional Distillation. Hearst Seattle Media, n.d. Web. 25 Mar. 2016.
3. Flow Schematic for Packed Column Distillation Column. Northeastern Chemical
Engineering Department, E-files. Web 25 Mar. 2016.
4. Jonathan Soucy. Batch Distillation: SOP. Working paper. N.p., 23 Feb 2016. Web. 26
Feb 2016.
5. Perry, Robert H., Don W. Green, and James O. Maloney. Perry's Chemical Engineers'
Handbook. New York: McGraw-Hill, 1984.
6. Hilmen, Eva-Katrine (November 2000). "Separation of Azeotropic Mixtures: Tools for
Analysis and Studies on Batch Distillation Operation" (PDF). Norwegian University of
Science and Technology, Dept. of Chemical Engineering.

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