Distillation of the ethanol-water mixture
Maria Paula Rincon Torres 1,2
Jonathan Stiven Beltran Correa 1,2
1.Separation operations laboratory
2. University of La Sabana
Introduction:
Worldwide, distillation has been the most
used separation method, so it is also the
most studied separation operation; in this
article we propose to compare the different
methods of analysis of distillation, by
means of experimental data, computer
simulators and graphical method
(McCabe-Thiele method); from this, we
intend to determine how accurate the
computer and graphical methods are in
reference to the experimental data.
Subsequently, to validate the experimental
data in the indirect measurement by means
of the IR, with the real values, and to
determine in a descriptive and quantitative
way the variation of these data; as well as
to determine if the regression is a correct
model for the use of prediction of the
experimental values.
Methodology
The equipment is started up, making sure
that the software is properly connected in
order to be able to record the experimental
data correctly, in addition to ensuring
remote control of the equipment. The tanks
are filled with the feed solution
The tanks are filled with the feed solution,
in this case 30% ethanol-water. This feed
reaches an exchanger where the liquid is
heated so that the most volatile component
can evaporate and the mixture enters the
two phases necessary for the separation.
This is done thanks to the use of a
peristaltic pump that drives the liquid from
the tanks. When the feed is heated it enters
the central part of the column. While the
feed circulates through the plates different
samples must be taken from the bottom
and the top of the column taking into
account the time in this case 10,20,30,40
and 50 min. These samples are taken IR to
determine the composition in the
separation process. Inside the distiller, due
to the difference between phases, the
separation will begin thanks to the design
of the plates inside the column that allows
the vapor and the liquid to flow more
easily. Therefore, the vapor (where the
most volatile component is found in
greater proportion) rises and passes
through the condenser where a change of
state occurs and the feed with higher
concentration of ethanol, this is stored as a
product of the distillate. If a higher
performance in the separation is desired,
the liquid obtained in the reboiler will be
recirculated to evaporate it enters the
column and rises until it passes through the
condenser again. As for the liquid (in this
one is the water in greater proportion)
This will descend until it leaves the Table 1: Data to make the ethanol calibration
column and will be stored in a container at curve.
the bottom. If it is also desired to improve Table 2: Experimental data of the
the yield, this liquid is circulated through distillation equipment.
the reboiler where the aforementioned
phase change is sought and the remaining
ethanol in the bottoms will circulate - Statistical treatment:
through the tower. Linear regression
Figure 1 shows the diagram of the
equipment for a better understanding of
the feed circulation.

Figure 2: Ethanol calibration curve

Figure 1: Operation of the equipment

Results and Analysis

 Presentation of results:

Table 3: actual data and the data predicted by

the regression model
 this residual analysis.

Figure 5: Variance analysis.

Figure 3: graph of model validation.
Based on the fact that to validate a regression
model is correct, it is necessary that its
validation graph has an R-square very close to
1 and the cut-off point is very close to 0; as it
is in this case, so it can be said that this is a
correct model to predict our next data.
In this analysis we found a very small
variation, the F factor is 0.000601, therefore, it
can be stated that the treatment given to the
data does not significantly affect the data, and
it is possible to stay with the model given to
the data.
 Presentation of the methods:
McCabe-Thiele graphical method

 Regression model validation

Figure 6: Schematic diagram of the

distillation column.
Figure 4: Residual analysis.
The residual analysis determines how much
the modeled data differs from the real data,
and as can be seen, it is determined that there
is not a great differentiation of the data, in fact,
they are very close, not differing by more than
0.001, which indicates that the modeled data is
correct in a reduced range of variance; not to
mention that it gives a very high R-squared for
Figura 5: graph del McCabe-Thiele
Ethanol/Water.

 Computer simulator method

(ASPEN plus RADFRAC`s Block).

Figure 8: Aspen distillation diagram.
Aspen was configured with 8 plates in total,
and the feed enters at plate 4 and with a vapor
quality of 0.
Figura 9: Mole fraction of distillation column
Figure 10: Molar flow rate of the distillation
column.
Figure 11: Thermodynamic parameters of the
distillation column.
 Comparison of methods:
Table 4: Comparison of methods.
Note: the data closest to those expected in
the experimental section were taken.
As it could be evidenced in the previous
table, the data of the McCabe-Thiele
graphical method and the Aspen simulator
are very close to the experimental ones,
from this it can be affirmed that both
methods are valid for the prediction of the
behavior in the distillation process of this
mixture at these conditions; on the other
hand, it is also affirmed that the computer
simulation method, Aspen, is closer to the
real data; It is clear that the data taken in
the McCabe-Theile method are
predetermined, i.e. they are assumptions
that are validated according to the result of
the graph and if it is possible to reach these
separation compositions; it should be
clarified that by default Aspen works with
a plate efficiency of 70%, and also uses the
sieve plates. The McCabe-Thiele method
was used assuming a plate efficiency of
100%; therefore, it was able to give this
increased separation in the composition.
 Analysis of the experimental
section:
Figure 12: graph of the distillation equipment
experimental data table
As can be seen, in the case of the distillate,
a composition close to 80% was expected,
and in bottoms a composition close to 5%;
the composition closest to that expected in
the distillate was at 30 minutes with a
composition of 70.34%; the composition
closest to that expected in bottoms was at
10 minutes with a composition of 6.75%.
It should be noted that the concentrations
were found from data found in the
literature and in this case the refractive
indexes obtained experimentally were
replaced in order to be compared with
those found in the paper of Reina, M.
(2010)
This figure also shows a significant
increase during the development time of
the experiment in bottoms, this may
indicate that it was cooling because the
most volatile component (Ethanol) is
increasing its composition, while in the
distillate, at 30 minutes there is a decrease
of the volatile component; it can be stated
that if the compound of interest is Ethanol,
it would be recommended for this
equipment and under these conditions, to
carry out the experiment until 30 minutes
of operation to obtain the highest
concentration of Ethanol.
Conclusions
From all of the above, the following points
can be concluded:
 The one-factor analysis of variance
showed that the treatment
performed on the sample IR data
did not significantly affect the data.
 The residual analysis validated the
use of the regression model as an
adequate model for predicting the
data from which the subsequent
analysis of the methods would be
developed.
 The McCabe-Thiele plot and
Aspen simulation models are
suitable for predicting the behavior
of the mixture in a distillation at
these conditions.
 The Aspen model is more accurate
to the experimental values than the
McCabe-Thiele model.
 Since the values of the
concentrations in the distillate are
similar between the methods, it can
be stated that the reflux of the
distillate assumed in the McCabe-
Thiele model of 1.2 is similar to
the reflux used in the experiment.
Bibliografía
 Manual de operación de la planta:
UOP3CC Issue 38 Instruction Manual,
2014.
 Reina,M,(2010). REFRACTIVE
INDEX, DENSITIES AND EXCESS
PROPERTIES OF BINARY
MIXTURES OF ETHANOL WITH
HEXANE, HEPTANE, OCTANE
AND WATER at (293.15 , 298.15 ,
303.15, and 308.15 )K.Take from:
https://www.redalyc.org/pdf/903/9031
9342013.pdf
 Souto.J,(2016). DESARROLLO
DEL SISTEMA DE CONTROL Y
PUESTA EN FUNCIONAMIENTO
DE UNA COLUMNA DE
DESTILACIÓN. Take from:
http://bibing.us.es/proyectos/abreproy/
90827/fichero/Desarrollo+del+sistema
+de+control+y+puesta+en+funcionam
iento+de+una+columna+de+destilaci
%C3%B3n
%2C+por+Jose+Antonio+Souto+Ale
man.pdf.