BATCH DISTILLATION EXPERIMENT

In Partial Fulfilment of the Requirements for the subject of

ChE Laboratory I

By
Guillermo, Denver
Olangco, Jewel Fe
Rante, Ferlyn Jade
Sia, Patric
Singson, Mariella B.

Engr. Caesar P. Llapitan

Instructor

May 2018
 ABSTRACT

An experiment was conducted using batch distillation process. A 30% ethanol-water mixture
was prepared, the volume, mass and temperature of the samples was collected during the
experiment. It was calculated that the 1st distillate sample, 2nd distillate sample and 3rd distillate
sample have a specific gravity of 0.875, 0.907 and 0.926 respectively. Using bilinear interpolation,
it was determined that the mass fraction in the initial flask mixture, 1st distillate, 2nd distillate, 3rd
distillate and final flask mixture were 30.55, 61.12, 49.005, 39.96 and 21.932 respectively. From the
results that was calculated, it was shown that the first distillate will be more concentrated than the
2nd and 3rd distillate sample since its mass fraction is higher than the two distillate samples. Also,
the generated curve (x-T) is similar to the actual curve of ethanol-water mixture.
 NOMENCLATURE

m Mass of the solution

v Volume of the solution
 Density of the solution
%wt Mass fraction
SG Specific gravity
 TABLE OF CONTENTS

ABSTRACT ......................................................................................................................... 2

NOMENCLATURE ........................................................................................................... 3

I. INTRODUCTION .......................................................................................................1

II. OBJECTIVES................................................................................................................1

III. THEORY .................................................................................................................. 2

IV. APPARATUS ............................................................................................................ 4

V. EXPERIMENTAL PROCEDURE ............................................................................. 6

VI. RESULTS AND DISCUSSIONS ............................................................................. 8

VII. CONCLUSIONS ..................................................................................................... 11

VIII. RECOMMENDATIONS ........................................................................................ 11

IX. REFERENCES ....................................................................................................... 11

X. APPENDICES ............................................................................................................ 12

LISTS OF FIGURES

FIGURE 1: SCHEMATIC OF A BATCH RECTIFIER ..................................................................................... 2

FIGURE 2: SCHEMATIC DIAGRAM ............................................................................................................ 4
FIGURE 3: ACTUAL SET-UP ....................................................................................................................... 5
FIGURE 4: ETHANOL AND WATER CONCENTRATION-TEMPERATURE DIAGRAM ........................... 9

LIST OF TABLE

TABLE 1: RESULTS USING BATCH DISTILLATION................................................................................... 8

I. INTRODUCTION

Distillation is the process of separating the components or substances from a liquid

mixture by selective boiling and condensation. Distillation may result essentially complete
separation (nearly pure component), or it may be a partial separation that increases the
concentration of selected components of the mixture. In either case the process exploits
differences in the volatility of the mixture’s component.
Batch distillation refers to the use of distillation in batches, meaning that a mixture is
distilled to separate it into its component fractions before the distillation still is again charged
with more mixture and the process is repeated. This is in contrast with continuous
distillation where the feedstock is added and the distillate drawn off without interruption.
Batch distillation has always been an important part of the production of seasonal, or low
capacity and high-purity chemicals. The interest in batch distillation has been steadily
increasing in the last few years. This is a natural resection of a change in industrial trends. In
fact, the shift towards the production of high value-added and low volume specialty chemicals
and biochemical has been much more marked in the last decade than in the past.
In this experiment, distillation operated in batch to concentrate the mixture of ethanol-
water having 10% concentration of ethanol. The goal of the experiment is to increase the initial
concentration of ethanol in water till the distillate extracted reach 40 ml in the beaker. Three
40 ml of the distillate was extracted before the distillation ended. The physical and
thermodynamic properties were gathered and was used for the calculation of the concentration
of the distillates.

II. OBJECTIVES

The objective of this experiment is to apply the process of distillation to a mixture of ethanol
and water to obtain a new mixture with an increased concentration of ethanol. Specifically, it
aims to:
1. Calculate the mass fraction of ethanol in the three distillate samples and the final
mixture and,
2. Approximate the x-T curve using the distillate samples in the ethanol-water calculated
value.
3.

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III. THEORY

Batch distillation was used in the experiment, this is due to the several advantage of its
application in small amounts of material or varying product compositions. In batch distillation,
the more volatile component is evaporated from the still which therefore becomes
progressively richer in the less volatile constituent. Distillation is continued, either until the
residue of the still contains a material with an acceptably low content of the volatile material,
or until the distillate is no longer sufficiently pure in respect of the volatile content.
To obtain products with a narrow composition range, a batch rectifying still is commonly
used. The batch rectifier consists of a pot (or reboiler) as in simple distillation, plus a rectifying
column, a condenser, some means of accumulating and splitting off a portion of the condensed
vapor (distillate) for reflux, and one or more product receivers (Fig. 1).

Figure 1: Schematic of a Batch Rectifier

The temperature of the distillate is controlled near the bubble point, and reflux is returned
at or near the upper column temperature to permit a true indication of reflux quantity and to
improve the column operation. A heat exchanger is used to subcool the remainder of the
distillate, which is sent to a product receiver. The column may operate at an elevated pressure
or at vacuum, in which case appropriate additional devices must be included to obtain the
desired pressure. In operation, a batch of liquid is charged to the pot, and the system is first
brought to steady state under total reflux. A portion of the overhead condensate is then
continuously withdrawn in accordance with the established reflux policy. “Cuts” are made by
switching to alternate receivers, at which time the operating conditions, e.g., reflux rate, may
also be altered. The entire column operates as an enriching or rectifying section. As time
proceeds, the composition of the liquid in the pot becomes less rich in the more volatile

2
components, and distillation of a cut is stopped when the accumulated distillate attains the
desired average composition.
Typically, an Equilibrium stage operations are based on principles of phase equilibrium
which is defined as an area in which different phases are brought into close contact so that a
component can be redistributed between the phases to equilibrium concentrations. When the
phases are separated, one is enriched with the solute and the other depleted. This combination
of mixing, approach to equilibrium, and separation is called an equilibrium stage. In the simple
batch distillation setup in this experiment, liquid in the 500-mL flask is in close contact with
the vapor phase that forms as the mixture boils, and this is the only place where this situation
is present in the setup. Therefore, there is one equilibrium stage in this batch distillation.
Assuming everything works ideally, the vapor phase is in equilibrium with the liquid in the
flask at any given time.
The equilibrium information needed for analyzing this separation process is the one that
shows the vapor-liquid equilibrium relationship for an ethanol/water mixture. The most useful
representation of the data is a y versus x graph, where y and x are the vapor and liquid phase
concentrations, respectively, of the more volatile component, ethanol. Points on the curve
depicted in such a graph represent the concentration of ethanol in the vapor and liquid phases
at equilibrium. Along the equilibrium curve, pressure is constant, but temperature is different
at each point.
Batch distillation has always been an important part of the production of seasonal, or low
capacity and high purity chemicals. It is very frequent separation process in the pharmaceutical
industry and in wastewater treatment units.

Temperature-Concentration Diagram
120

100
Temperaure,°C

80

60

40

20

0
0 0.2 0.4 0.6 0.8 1 1.2
% Mass Fraction of Ethanol

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IV. APPARATUS
This experiment involves small-scale batch distillation. The basic setup (actual and schematic
diagram) is shown below.

THERMOMETER

WATER OUTLET

DISTILLING FLASK CONDENSER

MIXTURE

DISTILLATE

COLD WATER INLET

Figure 2: Schematic Diagram

4
Figure 3: Actual Set-up

5
 The apparatus consists of the following:

a) 1000 mL Distilling flask with rubber stopper

b) Thermometer
c) Condenser
d) Copper tubing
e) Latex tubing
f) Gas stove
g) Iron stand
h) Plastic collection bottles, 40 mL

V. EXPERIMENTAL PROCEDURE

First, label the three plastic distillate collection bottles and make a mark to indicate the
level equal to 40mL. Pour 40 mL of the initial 10% ethanol in water solution into a 50 mL
graduated cylinder. Since specific gravity is dependent upon temperature, measure the
temperature of the solution. Once the specific gravity and temperature have been determined,
the solution may be discarded.
Next, determine the weight of an empty 1000-ml flask. Add 500 mL of the initial 10%
ethanol in water solution to the 1000 –mL distilling flask. Determine the weight of the flask
and solution. Be certain that distillation apparatus has been set up correctly and that you
understand how the system operates. Place the rubber stopper (with the copper tubing in it)
on the flask that contains the solution. The tubing should stick out past the stopper
approximately ½” into the flask. Do not force the thermometer or copper tubing into the
rubber stopper. Start water flowing through the cooling jacket of the condenser. Make sure
that the flow is from bottom to top. Otherwise, the coils may not be fully bathed in the cooling
water. The flow should be a gentle, but steady stream. Be certain that the rubber tubing is not
resting on or near the gas stove. The smell of burning rubber is not pleasant.
Then, turn the gas stove setting to medium-high and leave it at this setting for
approximately 10 minutes, or until the solution starts to boil. Turn the heat setting to medium.
The solution should begin to boil within 8-10 minutes. Once the solution begins to boil, it
should be about 3-5 minutes until you observe distillate dripping into the collection bottle.
Throughout the experiment, be sure the boil is very gentle. After the first bottle has collected
40 mL of distillate, quickly replace it with an empty one. This needs to be done as rapidly as
possible so that minimal distillate is lost. Cover and label the bottle containing the first distillate
sample. Record the temperature of the vapor phase above the boiling solution. Also determine

6
the mass of the first distillate sample. Calculate the specific gravity of the first distillate. The
temperature, density, mass fraction correlation chart only goes up to 40°C. Therefore, if the
distillate is warmer than 40°C, you will need to allow it to cool before measuring its specific
gravity. If it is already cool enough, it is a good idea to go ahead and calculate its specific gravity
while collecting the second distillate sample. Pour your distillate into a 50-mL cylinder. (If the
cylinder is too full, some of the liquid can be poured out after the mass is measured since it is
not necessary to have the total sample present to measure specific gravity; specific gravity is
not dependent on sample size.) Recall, the objective is to deduce the number of moles each of
water and ethanol in each of your distillate samples so that you can carry out a final mass
balance.
Repeat the procedure by collecting the second and third distillate sample. Once you are
close to collecting 40 mL of the third distillate, turn the gas stove off and carefully remove the
flask from on top of the gas stove. Do not remove the distillate collection bottle until the
mixture in the flask has stopped boiling for about 5 minutes. This helps to ensure that no
vapors remain in the tubing. After the third distillate collection bottle has been removed, the
flask can be removed from the clamp, and the stopper/tubing apparatus can be detached.
However, be sure to keep the flask covered while it is cooling so that no vapors escape. The
flask mixture will need to cool quite a bit before its specific gravity can be measured. A cool
water bath will help expedite the cooling process of the flask mixture. In addition, gently
swirling the liquid in the flask will help release heat more quickly. Once the solution in the
flask has cooled to below 40°C, determine the mass of the solution that remains in the flask.
Calculate its specific gravity of the solution remaining in the flask using the same method you
used for the initial solution. For each of your samples, use the specific gravity, temperature
and Table of the Densities of ethyl alcohol (C2H5OH in water) (Perry 2008) to determine the
mass percentage of ethanol in each sample. You may need to use bilinear interpolation to
calculate these values.

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VI. RESULTS AND DISCUSSIONS

A. Determining the mass fraction of ethanol in the three distillate samples and the final mixture.

In this experiment, a mixture of 10% ethanol-water was distilled using batch distillation
process. The initial flask mixture, 1st distillate sample, 2nd distillate sample, 3rd distillate sample
and the final flask mixture were weighed using analytical balance to calculate its specific gravity.
The temperature of the samples and also their boiling points were also collected. The mass
fraction of ethanol was calculated using bilinear interpolation. The specific gravity, temperature
and table of the densities of ethyl alcohol (C2H5OH in water) (Perry 2008) was used to
determine the mass percentage of ethanol in each sample.

Volume Temperature of %Mass

Sample and/ or Temperature the vapor space Specific fraction
Mass of sample after each Gravity ethanol
(mL,g) (°C) distillate is (calculated)
collected(°C)
Initial 500
Flask mL/488.7 g 33 °C 88.9 °C 0.9774 10.13
Mixture
1st 40 mL/35 g
distillate 36 °C 91.5 °C 0.875 61.12
sample
2nd 40
distillate mL/36.28 g 33.5 °C 93 °C 0.907 49.005
sample
3rd 40
distillate mL/37.05 g 34 °C 95.9 °C 0.92625 39.96
sample

Final 381
flask mL/373.7 g 40 °C 96 °C 0.9821 5.58
mixture

Table 1: Results using Batch Distillation

All of the vapor produced in the flask travels through the condenser and is collected as
distillate, then the mole fraction of ethanol in the distillate sample is the same as that of the
vapor in the flask. The 40-mL distillate samples were collected over a period of time during
which the concentration of the vapor and distillate continue to change. Thus, the mole
fractions of the distillate samples reflect a sort of time-averaged concentration.

A mixture consisting of two components, ethanol and water, which have boiling points
of 78°C and 100°C, respectively. When the mixture begins to boil, the vapor phase that is

8
 formed will be richer in ethanol than the liquid phase. This is because ethanol has a lower
boiling point and vaporizes more easily than water. Therefore, ethanol has a greater tendency
to enter the vapor phase while water tends to remain in the liquid phase.

As the mixture continues to boil, the compositions of both the vapor and liquid phases
changes with time. Since ethanol enters the vapor phase more quickly than water, the
concentration of ethanol in the liquid phase decreases while that of water increases. Also, as
the temperature of the boiling liquid increases, more water vaporizes as time passes, and the
concentration of water in the vapor phase also increases with time. If some fraction of the
original mixture vaporizes and the vapor is collected and allowed to cool and condense in a
separate container, the new liquid mixture (1st distillate sample) will have a higher concentration
of ethanol than the original did. If the first distillate is distilled by repeating the process, a
second distillate with an even higher concentration of ethanol will be obtained. The first
distillate that was collected will be more concentrated than the 2nd and 3rd distillate sample. The
more volatile component will be the ethanol since its molar mass is higher than the molar mass
of water.

B. Approximation of the concentration-temperature (x-T) curve using the distillate samples in the ethanol-water
calculated value.

Concentration-Temperature Diagram
96.5
96
95.5
95
94.5
Temperature

94
93.5
93
92.5
92
91.5
91
35 40 45 50 55 60 65
%Mass Fraction

Figure 4: Ethanol and Water Concentration-Temperature Diagram for the 3 Distillate

Samples

9
 Figure 5 shows the Concentration-Temperature Curve of ethanol and water mixture for
the 3 distillate samples. As the boiling point temperature decreases, the concentration of
ethanol increases. Because the density increases with temperature dependence. It is based on
the thermodynamic property of ethyl alcohol (Perry 2008). The approximated curve (Figure 5)
is similar to the actual curve of ethanol-water mixture.

C. Approximation of the concentration-temperature (x-T) curve using the initial flask mixture and final flask
mixture in the ethanol-water calculated value.

Concentration-Temperature Diagram
97 96
96
95
94
Temperature

93
92
91
90
88.9
89
88
5 6 7 8 9 10 11
% Mass Fraction

Figure 5: Ethanol and Water Concentration-Temperature Diagram for the Initial and
Final Flask Mixture

Figure 5 shows the Concentration-Temperature Curve of ethanol and water mixture for the initial
and final flask mixture. The boiling point increases

10
 Temperature-Concentration Diagram
100

95
Temperaure,°C

90
Theoretical Values

85
Experimental Values

80

75
0.35 0.45 0.55 0.65 0.75
% Mass Fraction of Ethanol

VII. CONCLUSIONS

Based on the experiment, the initial flask mixture, 1st distillate sample, 2nd distillate sample,
3rd distillate sample and the final flask mixture has a boiling temperatures of 88.9 °C, 91.5 °C,
93 °C, 95.9 °C and 96 °C respectively. The boiling temperature increases whereby the
concentration of ethanol in liquid decreases. The 1st distillate that was collected will be more
concentrated than the 2nd and 3rd distillate sample and will have a higher concentration of
ethanol than the initial. The concentration-temperature (x-T) curve was also generated to
compare it with the actual curve of ethanol-water mixture and the approximated curve is
similar with that actual curve.

VIII. RECOMMENDATIONS

Preparing a 30% solution must be more precise to obtain an accurate mixture of ethanol
and water solution. The apparatus should be calibrated to have accurate result. Also, some of
the evaporated water may be escaped from the process due to the error in settling the apparatus
therefore, the distillation set-up must operate correctly. No broken apparatus used and it must
be free from dirt.

IX. REFERENCES
[1] Mutjaba, I. (n.d.). Batch Distillation Design and Operation (Vol. 3). Imperial College Press.

11
 [2] Wankat, P. C. (2007). Separation Process Engineering Includes Mass Transfer Analysis, Third
Edition.

[3] R.H. Perry, C.H Chilton, and S.O. Kirkpatrick (Eds.), Chemical Engineers Handbook, 8th ed.,
New York, McGraw-Hill, p. 2-117, p. 13, 2008

[4] Liu, S. X., & Ming, P. (2009). The Simulation of Simple Batch Distillation of Multiple
Component Mixtures via Rayleigh's Equation. Wiley Interscience, 7.

X. APPENDICES

A. Calculating the mass fraction of ethanol in the mixture

Using bilinear interpolation formula,

The specific gravity, temperature and Table of the Densities of ethyl alcohol (ethanol –
C2H5OH) are given in Perry’s Chemical Engineering Handbook to determine the mass
percentage of ethanol in each sample.

1. Initial Flask Mixture

At T = 30°C;  =0.97031, %wt = 10
At T = 35°C;  =0.97846, %wt = 10
At T = 30°C;  =0.96723, %wt = 11
At T = 35°C;  =0.96527, %wt = 11

Solving for y,

(x 2  x)(y 2  y) (x  x 1 )(y 2  y) (x 2  x)(y  y 1 ) (x  x 1 )(y  y 1 )

P (Q 11 )  (Q 12 )  (Q 21 )  (Q 22 )
(x 2  x 1 )(y 2  y 1 ) (x 2  x 1 )(y 2  y 1 ) (x 2  x 1 )(y 2  y 1 ) (x 2  x 1 )(y 2  y 1 )

(35 - 33)(11- y) (33  30)(11 y) (35 - 33)(y - 9)

0.9774  (0.97031) (0.96723) (0.97846)
(35  30)(11 9) (35  30)(11 9) (35  30)(11 9)
(33  30)y  9)
 (0.96527)
(35  30)(11 9)

y  30.55%

2. 1st distillate sample

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 At T = 35°C;  =0.87615, %wt = 61
At T = 40°C;  =0.87180, %wt = 61
At T = 35°C;  =0.8739, %wt = 62
At T = 40°C;  =0.86943, %wt = 6

Solving for y,

(x 2  x)(y 2  y) (x  x 1 )(y 2  y) (x 2  x)(y  y 1 ) (x  x 1 )(y  y 1 )

P (Q 11 )  (Q 12 )  (Q 21 )  (Q 22 )
(x 2  x 1 )(y 2  y 1 ) (x 2  x 1 )(y 2  y 1 ) (x 2  x 1 )(y 2  y 1 ) (x 2  x 1 )(y 2  y 1 )

(40 - 36)(62- y) (36  35)(62  y) (40 - 36)(y - 61)

0.875  (0.87615) (0.87180) (0.87390)
(40  35)(62  61) (40  35)(62  61) (40  35)(62  61)
(36  35)y  61)
 (0.86943)
(40  35)(62  61)

y  61.123%
3. 2nd Distillate Sample

At T = 30°C;  =0.90805, %wt = 49

At T = 35°C;  =0.90396, %wt = 49

At T = 30°C;  =0.90580, %wt = 50

At T = 35°C;  =0.90168, %wt = 50

Solving for y,

(x 2  x)(y 2  y) (x  x 1 )(y 2  y) (x 2  x)(y  y 1 ) (x  x 1 )(y  y 1 )

P (Q 11 )  (Q 12 )  (Q 21 )  (Q 22 )
(x 2  x 1 )(y 2  y 1 ) (x 2  x 1 )(y 2  y 1 ) (x 2  x 1 )(y 2  y 1 ) (x 2  x 1 )(y 2  y 1 )

(35 - 33.5)(50- y) (33.5  30)(50  y) (35 - 33.5)(y - 49)

0.875  (0.90805) (0.90396) (0.90580)
(35  30)(50  49) (35  30)(50  49) (435  30)(62  61)
(33.5  30)(y  49)
 (0.90168)
(35  30)(50  49)

y  49.005%
4. 3rd Distillate Sample

At T = 30°C;  =0.92979, %wt = 39

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 At T = 35°C;  =0.91597, %wt = 39

At T = 30°C;  =0.91770, %wt = 40

At T = 35°C;  =0.91385, %wt = 40

Solving for y,

(x 2  x)(y 2  y) (x  x 1 )(y 2  y) (x 2  x)(y  y 1 ) (x  x 1 )(y  y 1 )

P (Q 11 )  (Q 12 )  (Q 21 )  (Q 22 )
(x 2  x 1 )(y 2  y 1 ) (x 2  x 1 )(y 2  y 1 ) (x 2  x 1 )(y 2  y 1 ) (x 2  x 1 )(y 2  y 1 )

(35 - 34)(40- y) (34  30)(40  y) (35 - 34)(y - 39)

0.875  (0.92979) (0.91597) (0.91770)
(35  30)(40  39) (35  30)(40  39) (35  30)(40  39)
(34  30)(y  49)
 (0.91385)
(35  30)(40  39)

y  39.96%
5. Final Flask Mixture

At T = 35°C;  =0.97672, %wt = 5

At T = 40°C;  =0.97485, %wt = 5

At T = 35°C;  =0.97335, %wt = 6

At T = 35°C;  =0.97142, %wt = 6

Solving for y,

( x2  x)( y2  y ) ( x  x1 )( y2  y ) ( x  x)( y  y1 ) ( x  x1 )( y  y1 )
P (Q11 )  (Q12 )  2 (Q21 )  (Q22 )
( x2  x1 )( y2  y1 ) ( x2  x1 )( y2  y1 ) ( x2  x1 )( y2  y1 ) ( x2  x1 )( y2  y1 )

(40 - 39)(6 - y) (39  35)(6  y ) (40 - 39)(y - 4)

0.875  (0.97672)  (0.97335)  (0.97485)
(40  35)(6  5) (40  35)(6  5) (40  35)(6  5)
(39  35)( y  4)
 (0.97142)
(40  35)(6  5)

y  5.58%

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B. Documentation
1. Preparation of the 30% ethanol mixture

2. Weighing the 30% ethanol-water solution

15
3. Distillation Set-Up ( During the experiment)

4. Collection of Three Distillte Samples

16
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