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Evaluation of the batch distillation process in the ethanol production

Chapter  in  Computer Aided Chemical Engineering · December 2012

DOI: 10.1016/B978-0-444-59519-5.50127-1

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Ian David Lockhart Bogle and Michael Fairweather (Editors), Proceedings of the 22nd European
Symposium on Computer Aided Process Engineering, 17 - 20 June 2012, London.
© 2012 Elsevier B.V. All rights reserved.

Evaluation of the batch distillation process in the

ethanol production
a
Alvarez M.E.T., a Moraes E.B., a,b Rodrigues J.C., a Bonon A.J., a Wolf-Maciel M.R.
a
Separation Process Development Laboratory, School of Chemical Engineering, State
University of Campinas-UNICAMP, Av. Albert Einsteins, 500 Campinas-SP 13083-852,
Brazil
b
Federal University of ABC – UFABC, Av. dos Estados, 5001 – Santo André-SP 09210-
580, Brazil

Abstract
Experimental data and simulations in Aspen Plus® for the batch distillation process
were obtained from an ethanol/water mixture. The simulation was carried out in order to
verify the effectiveness of the calculations for the batch distillation process for
recovering ethanol, using a plate column. The experimental data were taken from a
packed batch distillation column. The separation of ethanol/water mixture was studied
at different reflux ratios. The ethanol was quantified through a gas chromatography
analyses. The simulation and the experimental data were performed considering the
ethanol concentration in the wine that comes from the sugarcane fermentation. It was
verified that the higher ethanol concentration was obtained in one hour of distillation
and the accumulate ethanol concentration was above to 80% (mole) when operated at
constant reflux. So, it is possible to obtain high yields and concentrations of ethanol in a
short time.

Keywords: ethanol, distillation, experimental data, simulation.

1. Introduction
In the 1970s, the Brazilian government started a program for ethanol production from
sugarcane in order to effectively to replace gasoline in a large scale. For a time, this
program was dropped, but due to the production instability of the world´s largest oil
producers and energy concerns, the search for alternative sources of energy,
preferentially from renewable sources, has again sparked interest in this subject (Dias,
2011; Junqueira et al., 2009). The fermentation processes employed in the Brazilian
ethanol industry require low substract concentration and produce wine of low ethanol
content (around 7.0 to 8.5 w/w).When the intention is to use ethanol as a fuel, ethanol
concentration must be of at least 92.5 a 93.8 w/w. In the batch distillation column, the
feed is loaded to the distillation flask at the beginning of the process. It is then heated to
its boiling point, and the products are withdrawn sequentially from the column’s top,
according to its boiling point. (Demicoli and Stichlmair, 2004). Batch distillation has
been used to evaluate the effect of the recycling of foreshots and feints in the grappa
distillation (Porto et al. 2010) and in the separation of a complex azeotropic mixture,
comparing two methods of separation, showing that the columns hold-ups have
influence on the component separation (Watson et al. 1995). On the other hand, the use
of the Aspen Plus Commercial Simulator can simulate the batch distillation in order to
perform the process as well as to know the operating conditions. In this work, a batch
distillation column was used to obtain hydrated ethanol. The feed was composed of
ethanol/water (around 7.0 w/w of ethanol). In simulations were considered a plate
Evaluation of the batch distillation process in the ethanol production 633

distillation column and in the experiments, a packed column was used. Finally, the
results were compared, in order to evaluate the ethanol recovery.

2. Batch Distillation column

2.1. Details of the batch distillation column
A batch distillation column, model Autodest 800AC of Fischer Technology with a
capacity of 80 Lt was used and conditioned for ethanol distillation. The packed column
is filled with Propak 316 and equipped with a silvered vacuum mantle. Distillation flask
and the packed column have an external heat mantle and the temperature is controlled
by a Pt 100. The vapour temperature at the top of the column is also verified by a Pt
100. In the main condenser, a cryostat was used with a capacity of 360 Kcal at 0°C. All
system is controlled through Indusoft Web studioTM v6.2 supervisory installed in PC
that allows data acquisition of the batch column distillation. The batch column
distillation, Autodest 800AC, is equivalent to a column of 15 theoretical plates (ASTM
D 2892).
2.2. Distillation
In order to evaluate the ethanol recovery by batch distillation of wine coming from the
fermentation of sugarcane, a binary mixture of ethanol/water was considered as the feed
with approximately 7% (w/w) of ethanol concentration, produced in Brazilian alcohol
refineries.
The distillation was carried out at atmospheric pressure and operating temperatures have
been adjusted after different experiments. The distillate flask and column temperatures
were 170°C and 100°C, respectively. The temperature of the cryostat condenser was
maintained at 0°C. When the condensation starts at the top of the column, the distillate
was withdrawn after 15 minutes of stabilization of the system and the temperature of the
initial vapor was 69°C. In each 5 minutes, samples were collected for the following
reflux ratio (L/D): 0.75, 1.5, 2.5, 3.5 and 4.5. The ethanol content in the collected
samples was subsequently quantified by gas chromatography method.

3. Experimental
3.1. Materials
The reagents, n-propanol (99.1% - Fisher Scientific) HPLC grade, ethanol (99.9%
Merck) analytical grade were used for analytical methods.
3.2. Analytical Techniques and Procedure
Ethanol was determined by gas chromatography using an Agilent Technologies, 6850A
model with BP-225 capillary column (SGE) (50% cianopropifenil –PDMS; 25.0m ×
3.2×10-4m × 2.5×10-7m) and equipped with a flame ionization detector (FID). Hydrogen
was used as carried gas and synthetic air to burn the flame. The flow rate of nitrogen
was 1.6×10-3 L/min while the flow rate of synthetic air was 450.0×10-3 L/min and the
column temperature was 40°C for 2.5 min. A calibration curve was made with five
different points (5, 10, 15, 20 and 25% v/v of ethanol, with 5% n-propanol as internal
standard), all analyses were carried out in duplicate. 1×10-6 L of samples were
transferred to 10.0×10-3 L of volumetric flask, 0.3×10-3 L of n-propanol was added as
internal standard, using ultrapure water as solvent. 1.0×10-6 L of samples was injected
into a chromatograph and all measurements were made also in duplicate.
634 Alvarez et al.

4. Simulations
Aspen Plus® is one of the most used commercial simulator in the world, because its
complete package of thermodynamics properties and estimative methods. So, Aspen
Plus® was used to simulate the batch distillation process. Simulations in this work were
made considering a plate column, equivalent to the packed column of the Fischer
Technology, due the absence of the identical column in Aspen Plus database. Ethanol
recovery was, then, evaluated using a batch distillation column, considering a plate
column. The feed was composed of ethanol/water (7.02 %w/w of ethanol). The feed
temperature was maintained at 170°C. The simulation was carried out at atmospheric
pressure and the feed charged was 50 Kg. In setup of the block was considered 10
minutes as feed time in initial charge. The stop specification was defined as 3.4 hours of
distillation. Obtained results were compared with experimental data obtained from a
batch packed distillation column.

5. Results and discussion

Experimental data results for packed batch distillation at different reflux ratios are
presented in Fig. 1. It was observed that the ethanol composition was between 82 to 92
% (w/w) in the first 80 minutes of distillation. After this time, there was a sharp decline
in ethanol composition, reaching values close to 65 % (w/w). It was also verified that
the reflux ratio did not influence when the purpose is to reach high ethanol composition,
because the conposition profile follows the same tendency for all reflux ratios studied.

94
92 Reflux ratio
90 0.75
88
Ethanol composition (% w/w)

1.5
86
2.5
84
3.5
82
4.5
80
78
76
74
72
70
68
66
64
62
0 20 40 60 80 100 120 140
Distillation time (min)
Figure 1. Variation of the ethanol composition in the Distillate vs time at different reflux ratios

A random value of reflux ratio was assumed for study and comparison of the
performance between a packed column and a plate column. Experimental data were
collected using a packed column at a constant reflux ratio of 2.5. The distillate fractions
were collected every 18 minutes and, then, analyzed the ethanol composition in the
mixture by gas chromatography.
The results are shown in Fig.2. Simultaneously, considering the operating conditions of
the experimental data, a simulation in Aspen Plus was performed. In this case, taking
into account a column of 15 theoretical plates, equivalent to the packed column. Fig.2,
Evaluation of the batch distillation process in the ethanol production 635

the intention is to show the variation in ethanol composition as a function of time for the
simulated data and experimental data from a plate column and from a packed column,
respectively.
Figure 2 shows the same ethanol composition profile in the distillate, ie, when time
increases, the ethanol composition decreases. Moreover, it is possible to observe that in
the first 40 minutes of operation, both columns have the same performance, ie, the
ethanol composition remains the same in both cases. However, after this time it is
verified that the ethanol composition in the distillate tends to decrease more rapidly in
the case of packed column than if working with a plate column.

90
85
80
Ethanol composition (% mole)

75
70
65
60
55
50
45
40
35
0 20 40 60 80 100 120 140 160 180 200 220
Distillation time (min)

Figure 2. Variation of the ethanol composition in the Distillate vs time (reflux = 2.5; ż –
experimental data-packed column, Ƒ – simulation – plate column)
Table 1 shows the mass flow rate and the mixture composition of the steams in the
batch distillation column. The simulation results show that at the end of 204 min of
operation and at a reflux ratio of 2.5, ethanol is obtained at a concentration of 69.5%
(mole), however, it is observed that only 7.18 kg were recovered.

Table 1. Stream compositions and Flows of the component in a plate column destillation
Component Feed Reboiler Distillate
Mass Flow Rate Kg/hr
Ethanol 21.050 13.870 7.180
Water 278.950 277.719 1.231
Mole Fraction
Ethanol 0.029 0.019 0.695
Water 0.971 0.981 0.305
Mass Fraction
Ethanol 0.070 0.048 0.854
Water 0.930 0.952 0.146

The results of accumulated composition and the percentage of ethanol recovery are
presented in Table 2. It can be verified that in the first hour of operation, the
 636 Alvarez et al.

accumulated ethanol concentration is around 82% (mole), which can be concluded that
at this time interval both columns have the same performance and purpose in a final
ethanol concentration. On the other hand, in the simulation of the plate column, only
34.1% of ethanol is recovered at an accumulated concentration of 69.61% (mole), which
can result in a higher energy consumption and operating costs in a given operation time
if compared to a recovery of 51.81% (mole) in a packed column. Although the
accumulated concentration in a packed column is a little smaller, the recovery is
51.81%, just over 50% recovered when compared with a plate column.

Table 2. Ethanol composition and recovery in the distillation process

Acumulated ethanol
Distillation (% mole) Recovery (%)
Packed column
60 min 82.33
204 min 58.63 51.81
Plate column
60 min 82.59
204 min 69.61 34.10

6. Conclusions
Experimental data and simulated data were obtained and compared in the batch
distillation process using a packed column and a plate column, respectively. It was
developed an analysis method by gas chromatography using an internal standard to
quantify ethanol in the samples, while water was calculated by difference. The results
showed that operating in a packed column, more than 50% of ethanol is recovered when
compared with a plate column. Therefore, if the option is to operate a plate column, it
can require more time to achieve a higher yield and, therefore, excessive energy
consumption is required. The batch distillation with a packed column can be a good
alternative when the interest is to get a greater ethanol recovery in a shorter time,
regardless of accumulated ethanol concentration.

Acknowledgements
The authors are grateful to CNPq and FAPESP for the financial support.

References
American Society for Testing Material, ASTM D 2892, Standard test method for distillation of
crude petroleum (15-theoretical plate column), West Conshohocken, (Pennsylvania): ASTM
International, 2005. 32p.
Demicoli, D., Stichlmair, J., 2004. Computers Chem. Engng. 28, 643.
Dias, M.O.S., 2011. Desenvolvimento e otimização de processos de produção de etanol de
primeira e segunda geração e eletricidade a partir da cana-de-açucar, D Sc. Thesis,
FEQ/Unicamp, Campinas, (in portuguese).
Junqueira, T.L., Dias, M.O.S., Maciel, M.R.W., Filho, R.M., Rosell, C.E.V., Atala, D.I.P. 2009.
Computer Aided Chem. Engng. 26, 827.
Porto, C., Natolino, A., Corti, D. 2010. Food Sci. Technol. 45, 271.
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