Separation of an ethanol-water mixture in a distillation column.

Reyes Karen Lorena, Rincon Maria Paula.

Separation Operations Laboratory
Universidad de La Sabana, Chía, Cundinamarca.
March 09, 2020.

ABSTRACT
Distillation is the most widely used unitary separation operation at the industrial level and one of the
most energy demanding equipments, therefore the new engineers are confronted in looking for design
alternatives that reduce energy consumption in the design of distillation plants which translates into
economic savings. In this report the distillation of a mixture of ethanol-water is presented by
continuous distillation with the aid of equipment UOP3CC, two alternatives of reflux ratio (2: 1) and
(4: 1) were evaluated and proposed as alternatives to see the effect on energy consumption, obtaining
for a distillate fraction of 0,786 an energy consumption of 486kJ for the first ratio for 9 minutes of
operation and 153kJ during 3 minutes for the second reflux ratio concluding that the reflux ratio not
only affects energy consumption but also affects the time that final concentration is reached and
maintained.

Keywords: Boiling point, distillation, distillation column, ethanol, mixing, operation, refining, bottom,
refractive index, separation, volatility, water.

INTRODUCTION
Distillation is a unit separation operation where the separation of miscible substances is carried out.
The main objective of distillation is to separate a mixture of substances taking advantage of the
difference in volatilities, recovering in the distillate the component of interest which is normally the
lowest volatility presentation. This separation process is based on the difference in boiling temperatures
of the two substances [1] The process consists of heating the liquid mixture with an intermediate
temperature between the two boiling temperatures where its most volatile component passes to the
vapor phase which will subsequently condense to recover the component in liquid form as distillate.
The distillation process is carried out in a generally metal column which has plates or stages where the
liquid-vapor equilibrium is carried out [2] these columns can have several feeds or outlets, condensers
and partial or total boilers, in Figure Nº1 the diagram of a distillation column with a feed and each of
the parts is shown.

Figure Nº1:

There are many applications at the industrial level for this process, one of them and the most important
is the oil industry [3] which has as a separate objective the various components of crude oil through
fractional distillation. Likewise, the alcoholic beverage industry [4] to produce beverages of different
types such as brandy, whiskey, anise, tequila, rum, vodka, and gin.

METHODOLOGY
First, the solution to be distilled with an ethanol concentration of 11% was prepared from a 20% initial
solution by using the following equation:
 C2V 2
V 1=
C1
Equation I:” Volume needed for solution”.

the percentage of ethanol in the solution to be distilled and the refractive index were measured with an
alcohol tester to confirm the concentration of 12 liters of the solution that were prepared and divided
into 8 liters for reboiler and the remaining for feed tank.
Secondly, the calibration curve of six solutions (0.20,30,50,75,100% v / v) was prepared at which the
refractive index was measured, and the results were graphed in order to get the respective calibration
curve.
For the assembly of the equipment, the calibration of the feed pump began, a volume of 50ml was set
and the time it took to reach this volume was recorded by varying the power, taking into account that
the flow of the column does not flood the column. In addition, the column reflux ratio of 1.6: 1 was
adjusted, with the time it would enter the column and what would be the distillate of 13.2s = C- and
7.9s = C + , the reboiler heat duty was set to 1,5kW.
After that, the reboiler was filled with the solution to be distilled and the feed tank and the distillation
equipment was switched on waiting for the temperature to reach 70 ° C without exceeding the boiling
point of ethanol (the most volatile solution of the mixture) recording the time it took to reach that
temperature. Once 70ºc was reached, the service fluid valves for the condenser were opened, collecting
samples of the reflux and condensate valve every 3 minutes and measuring the refractive index at that
conditions, the column flooded so the feed flow was increased, the reflux ratio was set to be 2:1, the
reboiler heat duty was set to 0,9kW and the samples were collected for 15 minutes.
Once 10 samples were taken at the first reflux, the reflux ratio was changed increasing to 4: 1 16.8s =
C- and 4.2s = C + and a heat duty of 0,85kW and samples and their corresponding refractive index
were taken again. Finally, the solution was emptied from the reboiler, take its refractive index as well
as that of the feed tank, measuring the recovered distillate and its refractive index.
The overall column efficiency was calculated from:
Number of theoritical plates
Efficiency= x 100
Number of actual plates
Equation II:” overall column efficiency”.

The number of theoretical plates was calculated with Fenske Equation:

Equation III:” Fenske Equation for theoretical number of plates”.

Where N is the number of theoretical plates, Xd is the mole fraction of ethanol on distillate and Xb is
ethanol mole fraction on the bottoms, α is the average relative volatile of ethanol on bottoms and
distillate.

RESULTS

Feed solution preparation

For 12L of 11% w/w ethanol a total initial volume of 6,6L of 20%w/w ethanol solution was needed.

Refraction Index Calibration curve

The refraction index calibration curve and equation are shown in the following graph:

Figure I:” Refractive index calibration curve”.

The graph presented dismisses the one value corresponding to the 30% w/w ethanol because it didn’t
match the linear tendency.
In order to obtain the ethanol w/w% concentration the following equation was obtain:

Refractive index−1,3354
Ethanol Concentration=
0,0293
Equation III:” Ethanol w/w% concentration”.

Distillation fraction calculation

With equation III, the distillate ethanol mole purity was calculated, the following graph shows the
different distillation fractions through time for the different reflux ratios and the comparison with the
required mole purity as well.

Figure II:” Distillate ethanol fraction through time”.

Reflux ratio influence on heat duty and distillation mole purity

For understanding if the selected reflux ratio could reach the desired mole purity, the following table
was made by selecting the closest mole purities and calculating the respective heat duties to reaching
that composition for that amount of time.

Reflux Constant Ethanol Time Heat Duty Energy

Ratio Concentration (min) (kW) Conssumption (kJ)
2:1 0,786 9 0,9 486
4:1 0,786 3 0,85 153
Table I:” Energy consumption for obtaining desired mole purity”.

Number of theoretical plates calculation

The theoretical plates calculation with the Fenske equation (Eq.III) gives a result of 3,18 plates which
are approximated to 4 plates. Thus, the result for the columns efficiency in order to reach a 0,786-mole
purity is 50%.

For all the results calculations refer to Attachment 1.

ANALYSIS AND COMPARISON TO EXPECTED RESULTS FROM SIMULATION

With the initial conditions with a low feed flow, the composition wasn’t reach and was very high (>0,9)
and the reason is that the column flooded which makes that both, bottoms and distillation, go off
specification. [5] In order to solution the column flood, feed flow increase is an option because the
vapor production on the reboiler will be less and it will allow the column to work as specificity. [6]

On the other hand, if reflux ratio is compared, the results with a reflux ratio of 2:1 were better than with
a 4:1 because the specified distillate composition was constant for more time (9minutes for 2:1 and 3
for 4:1), if it is compared to the previous simulation, the reflux used was 1,56 to reach a 0,77
composition so it is consequent that the most similar reflux will reach the composition.

According to the Aspen simulation, in order to reach a distillation composition of 77% Ethanol, the
reboiler heat duty needed is 1,91kW, if it is multiplied by the time that during the desired composition
reaching, the equivalent is 1031,4kJ, according to Table I the column used on the laboratory required a
47% less energy than the one predicted, even if using a reflux ratio creates a better separation, the use
of different ratios can still perform a good separation and create acceptable products within a suitable
range [7], for that reason, if a 77% composition is required, the reflux can be changed in order to search
for the best configuration to consume the less energy, in this case, the best configuration was a 2:1
reflux ratio that required 486kJ to obtain the mole purity during 9 minutes.
Finally, the final bottoms composition predicted on the simulation was 0,062 and on the practice the
result was 0,066 which means that, effectively, with a feed flow composition of 0,11 and a reflux ratio
bigger than 1,56, a final distillate composition of 77% can be reach and the bottoms composition will
be 0,06 ,the difference is that, on the equipment, the heat duty was less and this can be because on the
practice, the pressure was different from the one putted on aspen and the feed was putted on the
optimal tray and the interval of time measured was a shorter one [7] to check those affirmations, it is
recommended to make a sensibility analysis on the simulation not only changing the reflux ratio but
changing the tray on which the feed is putted too.

CONCLUSIONS
- The optimization of design parameters such as reflux represents a noticeable effect not only on
energy consumption but in the time that the required distillation concentration is reached and
maintained
 - The realization of the study of energy consumption in the ethanol-water distillation process
makes it possible to demonstrate the energy potential that is wasted and could be used in other
processes to save expenses and to apply the principle of green energy in the separation
processes.
- Establishing the correct power in the feed pump, reflux ratio and optimum feed tray can
determine the correct operation of the distillation equipment and not pride a flood of the column
by steam or liquid.
- The viability of the processes depends on a complete previous study simulating in detail the
characteristics of what you want to know and each design variable, in order to develop a
process with the best efficiency in a pilot plant.

ATTACHMENTS
Attachment 1, Excel practice results and calculations: “LG6_Results(DEST)_20200903.xlsx”

REFERENCES

[1] Ivar J., HalvorsenS. (2000) Norwegian University of Science and Technology Department of
Chemical Engineering: “Distillation theory” [Online]
http://folk.ntnu.no/skoge/publications/1999/DistillationTheory/original/distillationtheory.pdf

[2] Wankat, P. (2008). Ingenieria de procesos de separacion. Ciudad de Mexico: Pearson Education.

[3] K.Wanga, B.J.Zhanga, Q.L.Chena “Optimization of a crude oil distillation unit based on total-
process simulation” Computer Aided Chemical Engineering. Vol. 38, 2016, Pages 2163-2168

[4] Spritis Europe, “Distillation process” [Online] Available: https://spirits.eu/spirits/a-spirit-of

tradition/distillation-process
[5] N. Cheremisinoff, Handbook of Chemical Processing Equipment, Woburn, MA: Butterworth-
Heinemann, 2000.

[6] N. Liebermann, Troubleshooting Process Operations, Third Edition ed., Tulsa, OK: Pennwell
Publishing Group, 1991, pp. 256-280.

[7] G. Faagau, "Reduce column energy consumption," 2008. [Online]. Available:

https://www.chemicalprocessing.com/articles/2008/123/. [Accessed 04 03 2020].
AUTO- CO EVALUATION
Name Auto Evaluation Co Evaluation
Karen L. Reyes 100% 100%
Maria P. Rincon 100% 100%