Distillation of Acetic Acid and Water Mixture

By

Gutierrez, Anne Lourdes 201510474

Isidro, Maridil Joy 201510311

Peralta, Janine Abiegale 201511022

Sumagui, Maria Francesca 201510437

Sta Teresa, Jabin 201320092

Submitted to
Engr. Pinky Joy Janaban Unit
Operations Laboratory 2

Chemical Engineering Department

College of Engineering
Adamson University

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 2nd Semester 2019-2020

Distillation of Acetic Acid and Water Mixture

ABSTRACT
In this experiment entitled ‘Distillation of Ethanol and Water Mixture’ the primary
objective is to separate an ordinary mixture of acetic acid and water by means of simple batch
distillation technique. Knowing that acetic acid is highly soluble in water and the two
components have distinct boiling point compare to one another, it is the aim of the experiment to
record and analyze the distillation extent of the binary mixture. A distillation set-up illustrated in
the procedure was utilized. Both distillate and residual portions of the mixture will be subjected
to titration using sodium hydroxide solution. It was evident based from the gathered data and
values that even though there was a difficulty in the batch distillation of acetic acid from the
water component, due to its deviation from the azeotrope table, the distillation process was fairly
completed and obtained. It was observed that the mole content of water in the distillate is higher
than the acetic acid, while the mole of acetic acid in the residual liquid was obviously higher than
the moles of water in terms of mole composition. Comparison based on the experimental value
and the theoretical values were determined by means of Rayleigh equation. It showed that the
calculated value was not significantly far from the experimental data and therefore proved that
the experimental values were acceptable.

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 Table of Contents

Introduction…………………………………………………………………………… 4

Theory………………………………………………………………………………… 4

Experimental Procedure……………………………………………………………… 5

Result & Discussion…………………………………………………………………… 7

Conclusion & Recommendation…………………………………………………….. 9

References………………………………………………………………………………. 11

List of Figures
Figure 1: Distillation of Acetic Acid-Water Solution Set-up…………………… 6
Figure 2: Titration of Distillate and Liquid Residue with NaOH solution Set-up.. 6
Figure 3: Schematic Diagram of Distillation…………………………………… 8

List of Tables
Table 1: Result of Titration of the Distillate……………………………………… 7
Table 2: Result of Titration of the Liquid Residue……………………………….. 7
Table 3: Feed Solution Composition……………………………………………... 8

Appendices
Appendix 1 : Sample Calculation………………………………………………… 9

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INTRODUCTION:

In the oil and petroleum industry, Distillation is a common separation process to be

utilized. Distillation is the systematic method of separating two or more components from its
mixture having significant difference in boiling point through several number of evaporation or
condensation stages. Distillation is commonly adopted due to its flexibility and low utilization
and maintenance cost unlike other separation processes. There are various types of distillation
processes namely, fractional distillation, vacuum distillation, and batch (differential) distillation
to name a few. In this experiment the efficiency of binary distillation of acetic acid-water
mixture will be tested knowing that despite of the difficulty, it could be a possible option for the
separation of the water-acetic acid mixture and to determine what could be done to increase its
utilization.

THEORY:

Binary distillation refers to the separation of a mixture having only two primary
component such as water-acetone mixture distillation. It is the type of distillation process that is
extensively utilized in laboratory conditions such as, pharmaceutical, polymer and purification
and retrieval of valuable solvent. However, there are certain binary mixture such as water-acetic
acid that is tough to separate specially when the acetic acid is highly diluted in water. Acetic acid
is highly soluble in water however, they do not form an azeotrope. Azeotrope occurs when the
two components of a mixture shares a constant boiling point due to the vapour phase
composition is equivalent to its liquid phase composition.
Since two components are present in a binary mixture, naming one component as ‘A’
denotes the more volatile component that has higher vapor pressure while the other component is
‘B’ that has greater boiling point or less volatile. Batch distillation works through the concept of
volatility difference. The vapor component generated by the heating process contains more ‘A’
than B while a higher content of component ‘B’ would be present in the residual liquid.

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 In this experiment, a binary mixture of water-acetic acid will be subjected to binary batch
distillation. Raleigh equation will be used as a mathematical counterpart of the physical
experiment to provide evidence of the results and findings of the experiment.

Rayleigh Equation Distillation:

X1
L1 1
ln
[ ]
L2 ∫
=
X ( y−x )
2
dx

PROCEDURE:

A Distillation
i An acetic acid-water solution was prepared in an Erlenmeyer flask.
ii The flask was put on heating mantle. The distillation apparatus was set up as
demonstrated.
iii The tap was gently turned on to let the cooling water into the condenser. The inlet
water was adjusted so that the cooling water enters at a rate sufficiently high enough
to cool and condense the vapor completely.
iv A dry clean beaker was weighed and positioned beneath the distillate outlet spout to
collect the distillate.
v The distillation was started by turning on the heating mantle. The heating mantle
control switch should be positioned at 6 or 7.
vi The heating mantle was turned off after the solution inside the flask was
approximately one-third vaporized.
vii The mantle was cools down and all the vapors were condensed. The distillation
equipment was disassembled. The trapped distillate was collected and added up into
the collecting beaker.
B Titration of distillate
i The collecting beaker including its content was reweighed.

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 ii All the distillate was poured into a 250ml volumetric flask. The remaining distillate
left on the beaker wall was washed with distilled water.
iii Half of the flask was filled with distilled water and was shaken gently a few times. It
then was filled up to the mark. The flask was turned upside down so that the solution
is well-mixed.
iv 100ml of the diluted solution was poured into a clean beaker. 25ml of the diluted
solution each then was pipette into 3 separate conical flasks. 2 drops of
phenolphthalein was added into each flask.
v A burette was filled with 1.0M NaOH solution and the content of each flask was
titrated with NaOH.
C Titration of liquid residue
i The step B(i) to B(v) were repeated for the liquid residue.

Figure #1: Distillation of

acetic acid-water solution

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 Figure # 2: Titration of distillate and liquid residue with NaOH solution

RESULT & DISCUSSION:

Mass of beaker: 62.5558g

Mass of distillate: 81.7911g – 62.5558g = 19.2353g

Mass of liquid residue: 71.8483g – 62.5558g = 9.2925g

Table #1: Result of Titration of the Distillate

Trial Rough I II III

Final reading of the 20.80 20.60 20.30 20.00
burette (ml)
Initial reading of the 0.00 0.00 0.00 0.00
burette (ml)
Volume of NaOH (ml) 20.80 20.60 20.30 20.00
Average volume of NaOH: 20.30ml

Table #2: Result of Titration of the Liquid Residue

Trial Rough I II III

Final reading of the 13.10 12.80 12.50 12.90
burette (ml)
Initial reading of the 0.00 0.00 0.00 0.00
burette (ml)
Volume of NaOH (ml) 13.10 12.70 12.50 12.90
Average volume of NaOH: 12.70ml

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 V = 0.5943 ml

L1 = 0.9052
ml

XA = 0.3863
XB =0.6137

L2 = 0.2199 ml

Figure #3: Schematic Diagram of Distillation

Table #3: Feed Solution Composition

Species Volume(ml) Mass(g) Mole(gmol) Mole fraction Mole %

HC2H3O2 20.0000 20 ×1.049=20.98 20.98 0.3497 38.63%
=0.3497 =0.3863
60 0.9052
H2O 10.0000 10 ×1.000=10.00 10.00 0.5555 61.37%
=0.5555 =0.6137
18 0.9052
Total 30.0000 20.98 0.9052 1.000 100.00%

Molar composition of the feed;

HC2H3O2 = 38.63% = 0.3863
H2O = 61.37% = 0.6137

It could be observed that the volumetric amount of sodium hydroxide used in the titration
of the distillate is higher compared to the utilized amount to titrate the residual liquid. It can also
be noticed that the composition of the distillate was more favored with the presence of water than
acetic acid while in the liquid residue, there were more acetic acid than water based on their
molar composition. Since there was less acetic acid on the distillate and more water was present

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in the distillate mixture, more NaOH solution was needed while less NaOH was used in the
residual liquid due to the abundance of acetic acid and lack of water molecules.

CONCLUSION & RECOMMENDATION:

At the end of the experiment, it could be observed that batch distillation of water-acetic
acid binary mixture could be separated. However, due to the nature of the binary mixture which
deviates the azeotrope, there was difficulty in conducting the separation process. Although the
experiment suggested that component ‘A’ which is more volatile than component ‘B’ is greater
in the distillate and the less volatile ‘B’ is highly present on the residual liquid, by utilizing the
Rayleigh equation to determine the theoretical composition of the distillate and liquid residual, it
can be observed that there is a significant difference on the value. This difference may be caused
by human error during the experimentation procedure.It is advisable to increase the temperature
at 1atm to encourage more distillate to form and more acetic acid would be present in the
residual liquid. Nonetheless, the efficiency and separation of this binary mixture is
recommended to be improved by means of various entrainers. It is also recommended to conduct
another experiment that aims to compare which of the possible entrainers is more suitable and
cost effective for the binary batch distillation of water-acetic acid mixture.

APPENDICES:
Sample Calculation:

1. Calculate the composition of distillate:

Species Mole Mass(g) Mole Fraction Mole

%
Acetic Acid 0.203 0.203 ×60=12.180 0.203/0.594=0.342 34.2
Water 0.391 0.391 ×18=7.038 0.391/0.594=0.658 65.8
Total 0.594 19.218 1.000 100.00

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From the titration data, determine the composition of the liquid residue.

HC2H3O2 + NaOH NaC2H3O3 + H2O

MaVa a
=
MbVb b

Ma = ? Va = ?
Mb = 1.0 M Vb = 20.30ml = 0.0203 L

2. Calculate the composition liquid residue:

Species Mole Mass(g) Mole Fraction Mole

%
Acetic Acid 0.127 0.127 × 60=7.62 0.127 /0.2199=0.5775 57.75
Water 0.0929 0.0929 ×18=1.6722 0.0929/0.2199=0.4225 42.25
Total 0.2199 9.2922 1.000 100.00
MaVa a
=
MbVb b

Ma = ? Va = ?
Mb = 1.0 M Vb = 12.70 ml = 0.0127 L

3. Using Rayleigh Equation

Calculate the theoretical composition of distillate and residual liquid.

By using Raleigh equation,

X1
L1 1
ln
[ ] L2 ∫
=
X ( y−x )
2
dx

0.3497
L1 1
ln
L2
= ∫
X2
( y −x )dx
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 let :
L1
ln =1.4
L2
 To determine the value of X2, we can perform trial and error.
 In order to calculate the value of X2 between 0 and 0.35 that must be equivalent to
1.4 after integration.
 After trial and error, at X2=0.17 the area under the curve is close to 1.4
 Thus, X2 = 0.17

REFERENCE:

Binous, H., & Al-Harthi, M. (2011). Simple Batch Distillation of a Binary Mixture. Simple
Batch Distillation of a Binary Mixture. Retrieved from
https://library.wolfram.com/infocenter/mathsource/8304/binous_al_harthi.pdf
Galli, F., Previtali, D., & Pirola, C. (2017). Simulation of the Water-Acetic Acid Separation via
Distillation Using Different Entrainers: an Economic Comparison. Simulation of the Water-
Acetic Acid Separation via Distillation Using Different Entrainers: an Economic Comparison.
doi: https://doi.org/10.3303/CET1757194
Lei, Z., Li, C., Li, Y., & Chen, B. (2004). Separation of acetic acid and water by complex
extractive distillation. Separation and Purification Technology, 36(2), 131–
138. doi:10.1016/s1383-5866(03)00208-9 
Sorensen, E. (2014). Design and Operation of Batch Distillation. Distillation, 187–
224. doi:10.1016/b978-0-12-386547-2.00005-3 
Xu, Z., Afacan, A., & Chuang, K. T. (1999). Removal of acetic acid from water by catalytic
distillation. Part 1: Experimental studies. The Canadian Journal of Chemical Engineering,
77(4), 676–681. doi:10.1002/cjce.5450770408 

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