Batch distillation

Camila Carvajal

Paula Gutiérrez Sojo

Karen Romero

12 agosto de 2019

Laboratorio de operaciones de separación 2019-II

Universidad de La Sabana
Abstract
In order to analyze different types of separation, such as in this case, the batch distillation of a 30% v/v
Water-Ethanol solution, a case study was proposed, whose main objective is to develop an
experimental practice, in the one that will study the variation of temperature and will look for to know
the concentrations of ethanol in each stage of the column.

The corresponding calculations were made to prepare eight solutions at different concentrations of
ethanol, to which the refractive index was determined, with two variables a calibration curve was
performed, which served to determine the concentrations of the samples taken in each stage during the
distillation process. Thanks to the thermocouples installed in the column, the temperatures at each stage
could be determined. A simulation of the process was carried out in the Aspen Plus tool, in order to
determine the initial conditions in which the practice would be developed and to make comparisons of
the results obtained.

By means of the equation of the straight line of the calibration curve it was obtained that the
concentration of ethanol in the distillate is 76% v/v, in addition to this method that includes the
refractive indices, it was decided to use another one, which was It is carried out by means of the
breathalyzer, thus giving a concentration of ethanol in the distillate of 96% v/v and finally, according to
the Aspen tool, the concentration of ethanol corresponds to 55% v/v. Large differences can be
evidenced between the 3 values obtained, this is mainly due to errors made in the use of the
refractometer and to the type of simulation performed, since a design was made for continuous
distillation and not for batch distillation.

Keywords: distillation, ethanol, distillation column, water

Introduction

Distillation is a process that consists in separating a liquid mixture into fractions that concentrate the
different components by the differences in relative volatility of the mixture components.

The separation of this mixture is performed in a distillation column and achieved by controlling the
column temperature and pressure profiles. After the mixture is separated the most volatile component
will be more concentrated in the top of the column and will be denominated as distillate. [1]
Distillation can be classified as continuous or batch distillation. The basic difference between these
distillations is that in continuous distillation the feed is continuously entering the column, while in
batch distillation the feed is charged into the reboiler at the beginning of the operation.

Batch distillation is the oldest separation process and the most used unit operation in the batch industry.
It is used in chemical industries where small quantities of materials are to be handled in seasonally
scheduled periods, when the feed composition varies from period to period or where completely
different feed stocks must be handled. [2]

Distillation has a wide variation of applications, including oil and fat extraction in alimentary industry,
separation of benzene from toluene, methanol or ethanol from water, separation of crude oil into
fractions, water purification and desalination, splitting air into its components, distillation of fermented
solutions such as high alcohol percentage beverages and many more separations. [3] For example, in
wine industry distillation is widely used to separate ethanol from fermented grape and in this way the
wine could be purified. [4]

Methodology
To solve this study case the Armfield® distillation column UOP3CC was used. To use this column 8
liters of a solution ethanol/water 30% v/v were prepared and introduced to the reboiler. After the
solution was charged the distillation column and the reboiler were turned on, also the power of the
reboiler was set to the maximum value until the column temperature reached 80,1°C. The following
step consisted in setting the reboiler’s power to 5 kW and taking samples of each plate of the column to
analyze the temperature and concentration of each.

While the reboiler reached the aforementioned temperature, a calibration curve was done with different
concentrations of the mixture ethanol/water and the refraction index. This curve consisted in 8 different
solutions with concentrations of 0%, 10%, 20%, 30%, 40%, 50%, 60% and 90%, that were prepared
diluting a solution of 90% ethanol in 1 mL Eppendorf tubes. Then the refraction index was taken with
an analog refractometer and temperature was measured with the equipment thermocouples.

After taking samples of the plates, the concentration of each sample was obtained by measuring their
refraction indexes and replacing each value in the equation obtained previously from the calibration
curve. Some of the samples were taken two times in order to rectify that the obtained value was the
same, and the refraction indexes were taken by the same person to minimize mistakes in the
measurements.

Finally, a sample of the distillate was taken. In order to do so, the valve that controls the reflux had to
be closed to start collecting the distillate because the column had been working with total reflux.
Subsequently, the concentration of ethanol of the distillate was obtained by measuring its refraction
index and replacing that value in the equation obtained from the calibration curve. Lastly, the distillate
was left at rest to achieve a lower temperature, and then measure the concentration of ethanol with a
breathalyzer, and both results were compared.

In the other hand a simulation of the distillation was done in Aspen Plus selecting a distillation column
and the thermodynamics method NRTL due to this mixture is a polar non electrolytic solution and the
pressure at which the distillation was executed is below 10 bar. The column was defined by a feed
current that content the ethanol/water mixture with molar fraction of 0,12 and 0,88 respectively, room
temperature of 17°C, Bogotá’s atmospheric pressure (565 mmHg) and no pressure drop.

Results and discussion

Three types of results were obtained:

 The theorical results

Ethanol Concentration 90
Solution mL of ethanol mL of water Final volume (mL)
concentration (% v/v)
0 0 1 1
10 0.111111111 0.888888889 1
20 0.222222222 0.777777778 1
30 0.333333333 0.666666667 1
40 0.444444444 0.555555556 1
50 0.555555556 0.444444444 1
60 0.666666667 0.333333333 1
90 1 0 1
Table 1. Calculations for the design of the calibration curve

Solution L of ethanol L of water Final volume (mL)

concentration (% v/v)
25 2.2222 5.7778 8
Table 2. Calculations for the preparation of the feed solution
  The simulation results

Figure 1. Simulation in Aspen  

Description Bottom Distilled

Temperature (°C) 91.908 72.314
Pressure (bar) 0,75327138 0,75327138
Mole Fraction water 0,99999485 0,78897105
Mole Fraction ethanol 5,143089981E-06 0,2110289409

Equipment Heat Duty (KW)

Condenser -58,1110519
Reboiler 70,2356058
Table 3, 4. Simulation data of the column

 The experimental results

Ethanol Concentration Refraction Index

0% 1,33242
10% 1,33842
20% 1,34342
30% 1,34942
40% 1,35742
50% 1,36142
60% 1,36542
90% 1,33242
Table 5. Calibration curve data

With this initial data a calibration curve was constructed, nevertheless it was necessary to eliminate the
atypical points in the curve to have better results and the final calibration curve is shown next.
 Plot 1. Calibration curve

As the methodology says some samples were taken from each plate to evaluate the temperature and
concentration profile. In the following table the experimental results will be shown.

Number of Stages Temperature (°C) Refraction Index Ethanol Concentration

1 71.7 1.36542 0.76187768
2 71.2 1.36542 0.76187768
3 71.6 1.36542 0.76187768
4 71.8 1.36542 0.76187768
5 72.3 1.36442 0.73707368
6 73.6 1.36342 0.71226968
7 75.3 1.36142 0.66266168
8 74.9 1.36342 0.71226968
Distillate 1.36542 0.76187768
Table 6. Experimental data from the column.

The temperature and concentration profiles obtained in the Aspen tool, help us to know the behavior of
these variables with respect to ethanol at each stage of the column
 Plot 2. Temperature Profile of ethanol

Plot 3. Concentration profile of ethanol

To know the variation generated by a change in the feed flow, in the temperature and concentration of
ethanol at each stage, the flow was increased from 3 L / min to 4 L / min and decreased to 1.5 L / min,
from these changes the following profiles were obtained
Plot 4. Concentration profile of ethanol increasing feed flow

Plot 5. Temperature profile of ethanol increasing feed flow

Plot 6. Temperature profile of ethanol decreasing feed flow

 Plot 7. Concentration profile of ethanol decreasing feed flow

Analysis

As said before, the distillation was performed by getting the feed into the reboiler, and the distillation
process started from there, then, when the temperature reached a high value and the liquid started to
vaporize, the samples of each tray were taken, obtaining the results observed on table 6. The
temperatures obtained on every plate were not too similar with each other at the moment of starting the
distillation process, but at the moment of taking the samples of each tray, a considerable time had
passed and the values of temperatures on each plate had gotten closer, that approach in temperatures
means that the column was reaching or had already reached the equilibrium. That also can be
evidenced in the results of the concentration obtained from measuring the refraction index in each tray,
due to the approach between the values of the concentrations it can be concluded that the column had
reached equilibrium and the mixture was no longer able to be separated. The reason why the mixture
could not be separated more than that is that maybe it had already reach its azeotropic composition, that
is the composition at which a mixture boils, but it does not change its composition. [5]

After performing the distillation with complete reflux in order to get a higher efficiency, the reflux
valve was closed, and the distillate was obtained and analyzed in the refractometer obtaining a value of
concentration of 76,18 % v/v. This is a relatively high value considering that the initial concentration of
the mixture was of 30% v/v. However, to make a corroboration of the concentration of ethanol in the
distillate, the concentration was also measured in the breathalyzer, obtaining a concentration of 96%
v/v. The value of concentration of the distillate was also calculated by performing the simulation on
Aspen Plus, and a concentration of 55% v/v was obtained. Because of the similarity in the values
obtained in the simulation and in the refractometer, the value obtained from the calibration curve is
considered the real value of the distillate, even though it is a lower value. The concentration reached
experimentally was higher than the concentration reached in the simulation, that is because the reflux
used in the simulation is partial while the reflux used in the practice was complete.

Although the distillation process was successful because the objective of increasing the concentration
of ethanol in the mixture was accomplished, the reached concentration of ethanol could have been
higher. One way to increase the concentration reached in the distillation is choosing a mixture with a
higher initial concentration, and in that way, the concentration of ethanol in the distillate would be even
higher.

It is possible to observe the differences between the temperatures and concentrations per stage obtained
by the experimental method (See table 6) and those obtained in the ethanol temperature profile (See
plots 2 and 3), this could have occurred because the data of the experimental method is obtained by
means of the refractometer, a device in which a high degree of error can be obtained, also the
difference that exists can be due to the fact that the simulation performed in the Aspen tool is for
continuous distillation, while the performed in the laboratory corresponds to a batch distillation.

An increase in the feed flow of 3 L / min to 4 L / min was made, due to this an increase in ethanol
concentrations was generated at each stage (See plots 3 and 4), but mainly there was an increase in
Ethanol concentration in the distillate, since it went from having a concentration of 55% v / v a
concentration of 60% v / v, this is because when increasing the feed flow there is a greater supply of
energy, so both the purification of ethanol in the distillate is greater, also thanks to this there was a
decrease in temperature, this was more reflected in the stages near the distillate (See plots 2 and 5), this
is logical with respect to the increase in Ethanol concentration, since the lower the temperature, the
greater the amount of steam will condense.

Otherwise we see in plots 2 and 6 as the feed flow decreases to 1.5 L / min, where the temperature
increases in the upper stages compared to the original flow, here the temperature also affects the
ethanol concentration of the distillate, Since the temperature is higher, the lower amount of steam will
condense and therefore the concentration will be lower (See plot 7), also as the feed flow decreases, the
energy supply is reduced and therefore the impurities increase in the distillate
Conclusions

 Due to missing data it was impossible to include in calculations the McCabe-Thiele‘s diagram.
 As the feed flow is increased, the ethanol concentration increases for each stage and the
temperature decreases, while the feed flow decreases, the ethanol concentration decreases and
the temperature increases.
 The concentration of ethanol obtained experimentally in the distillate was higher than the
concentration obtained in the simulation because in the simulation the chosen reflux was partial
and experimentally was a complete reflux.
 The differences in ethanol concentration values in the distillate are mainly due to human errors
and a simulation for continuous distillation rather than one for batch distillation.

References

[1] Neuthrium, Distillation fundamentals, (n.d.). https://neutrium.net/unit-operations/distillation-

fundamentals/.

[2] K.J. Kim, U. Diwekar, Batch distillation, 2005. doi:10.1201/9781420028164.

[3] A.A. Kiss, Advanced Distillation Technologies: Design, Control and Applications, Adv. Distill.
Technol. Des. Control Appl. (2013). doi:10.1002/9781118543702.

[4] Bodega Garzón, Destilación del vino, (n.d.). https://bodegagarzon.com/es/blog/destilacion-vino/.

[5] Mejía, S; Espinal, J; Mondragon,F.(2006). Estudio del azeotrópo Etanol agua. Caracterización
molecular de dímeros de etanol, heterodímeros y heterotrímeros de etanol/agua. Universidad
Nacional de Colombia. Tomado de: https://www.redalyc.org/pdf/1470/147019426001.pdf

*Auto/ Coevaluation

*Diagonal corresponds to auto evaluation

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