Batch Distillation

Concept

Distillation has been described as the “work-horse” of chemical engineering because of its
widespread use in industry. Distillation separates two or more liquid components in a mixture
using the principle of relative volatility or boiling points. The greater the difference in relative
volatility the greater the nonlinearity and the easier it is to separate the mixture using
distillation.

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. In addition, the
results of the experiment will be used to approximate the equilibrium relationship between
ethanol and water. Specifically,

1. Calculate the number of moles of ethanol and water in the initial flask, the three distillate
samples and the final mixture.
2. Perform a mole balance for both the ethanol and water. If necessary, propose explanations
for any discrepancies in the balances.
3. Approximate the equilibrium curve using the distillate samples using x/y ethanol-water
calculated values
4. Compare the generated curve with the actual equilibrium curve for ethanol-water mixture

Theory

Distillation type that is used for this experiment is batch distillation type. 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.

For example, consider a mixture consisting of two components, A and B, which have boiling
points of 70°C and 100°C, respectively. When the mixture begins to boil, the vapor phase that
is formed will be richer in A than the liquid phase. This is because A has a lower boiling point
and vaporizes more easily than B. Therefore, A has a greater tendency to enter the vapor phase
while B tends to remain in the liquid phase. Of course, if the entire mixture could boil away,
the resulting vapor would have the same concentration of A and B as the original liquid
mixture. However, if only a fraction of the liquid can boil, the vapor will contain a higher
concentration of A than the original liquid mixture.

As the mixture continues to boil, the compositions of both the vapor and liquid phases change
with time. Since A enters the vapor phase more quickly than B, the concentration of A in the
liquid phase decreases while that of B increases. Also, as the temperature of the boiling liquid
increases, more B vaporizes as time passes, and the concentration of B 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 (first distillate) will have a
higher concentration of A than the original did. If the first distillate is distilled by repeating the
process, a second distillate with an even higher concentration of A will be obtained. This is
basically how distillation works. It is just a series of vaporization and condensation processes
that continues until a desired concentration is reached.

In general, an equilibrium stage in any type of unit operation process 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. In the simple batch distillation setup in this
experiment, liquid in the 1000-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 type of equilibrium information that is needed for analyzing this separation process is that
which 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. A picture of the ethanol/water y versus x graph follows.
 1

0.9

0.8

0.7

0.6

0.5

0.4

0.3

0.2

0.1

0
0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1

Apparatus

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

Figure 1 Actual Setup Figure 1. 1 Schematic Drawing

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) Hot plate or Bunsen burner with hot plate
g) Iron stand
h) Plastic collection bottles, 40 mL

Procedure

1. Label the three plastic distillate collection bottles and make a mark to indicate the level
equal to 40mL. (Do not trust prior marks if they exist)
2. Pour 40 mL of the initial 10% ethanol in water solution (prepared by instructor) into a 50
mL graduated cylinder.
3. Using the appropriate hydrometer, measure the specific gravity of the solution in the
graduated cylinder. Because specific gravity is dependent upon temperature, you must also
measure the temperature of the solution. Once the specific gravity and temperature have
been determined, this solution may be discarded. You should report the specific gravity to
three significant figures and the temperature to the nearest degree.

Figure 1. 2 Hydrometer Reading

4. Determine the weight of an empty 1000-ml flask.
5. Add 700 mL to 800 mL of the initial 10% ethanol in water solution to the 1000 –mL flask
you weighed in step 3.
6. Determine the weight of the flask and solution.
7. 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.
***SAFETY NOTE*** Do not force the thermometer or copper tubing into the rubber
stopper. If they do not easily slide into the stopper, add a drop or two of glycerin to hole
and try again.

 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 hot plate. The smell of
burning rubber is not pleasant.
8. Turn the hot plate setting to medium-high and leave it at this setting for approximately 10
minutes, or until the solution starts to boil. Then, 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.
9. After the first bottle has collected approximately 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.
10. Determine the mass of the first distillate sample.
11. Measure the specific gravity of the first distillate in the same manner as you did for the
initial solution in steps 2 and 3. 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 measure 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.
12. Repeat steps 9-11 to collect the second distillate sample.
13. Repeat steps 9-11 to collect the third distillate sample. Once you are close to collecting 40
mL of the third distillate, turn the hot plate off and carefully remove the flask from on top
the hot plate. **SAFETY NOTE: Please be cautious as the flask will be very hot. You
must use oven mitts for this step. Ask your instructor for assistance. 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.
14. 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. (In the meantime, finish
measuring the specific gravity of the three distillate samples.) 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.
15. Once the solution in the flask has cooled to below 40°C, determine the mass of the solution
that remains in the flask.
16. Measure the specific gravity of the solution remaining in the flask using the same method
you used for the initial solution in steps 2 and 3.
17. For each of your samples, use the specific gravity, temperature and Table of the Densities
of ethyl alcohol (ethanol - 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.

Calculation

Chemical engineers typically perform mole balance analyses on processes as a means of

checking to see that all material is accounted for. In general, this means checking to see that

Input – Generation – Output – Consumption = Accumulation Eq 1.0

In this lab the mole balance can be thought of in terms of

Moles in original flask mixture = Moles in Distillate 1 – Moles in Distillate 2 + Moles in

Distillate 3 – Moles in the final flask mixture Eq 1. 1

1. Calculate the number of moles of ethanol and water in the initial flask, the three distillate
samples and the final mixture.
2. Perform a mole balance for both the ethanol and water. If necessary, propose explanations
for any discrepancies in the balances.

Post Lab Questions

1. Is there a significant difference in the results between the samples?

2. After performing material balance on ethanol and water, are there any discrepancies?
If there were, what caused it?
3. What will happen to the distillate if the concentration of ethanol is increased from 10%?
Explain.

Batch Distillation Data Sheet

Volume Temperature Temperature of the Specific Mass fraction

and/ or of sample vapor space after Gravity ethanol
Mass each distillate is (calculated)
collected
Initial
Flask
Mixture
1st
distillate
sample
2nd
distillate
sample
3rd
distillate
sample
Final flask
mixture

Supplementary Readings
For further discussion about batch distillation for some azeotropic mixtures, refer to the
following books:

1. Mutjaba, I. (n.d.). Batch Distillation Design and Operation (Vol. 3). Imperial College
Press.
2. R.H. Perry, Chemical Engineers Handbook, 8th ed., New York, McGraw-Hill

References

Mutjaba, I. (n.d.). Batch Distillation Design and Operation (Vol. 3). Imperial College Press.
Wankat, P. C. (2007). Separation Process Engineering Includes Mass Transfer Analysis,
Third Edition.

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