Experiment No.

4
DISTILLATION
1. Objective:
To determine the amount of distillate that can be obtained by batch distillation of a feed of 50% weight
methanol-water mixture.
2. Intended Learning Outcomes (ILOs):
The students shall be able to:
2.1 understand the principles of reflux and reflux ratio.
2.2 understand the effect of vacuum conditions on the separation of a binary mixture of methanol.
3. Discussion:
The unit operation distillation is a method used to separate the components of a liquid solution, which depends
upon the distribution of these various components between a vapor and a liquid phase. All components are
present in both phases. The vapor phase is created from the liquid phase by vaporization at the boiling point.
The basic requirement for the separation of the components by distillation is that the composition of the vapor
be different from the composition of the liquid with which it is in equilibrium at the boiling point of the liquid.
Distillation is concerned with solutions where all components are appreciably volatile, such as in ammonia-water or
ethanol-water solutions, where both components will be in vapor phase. In evaporation, however, of a solution of
salt and wtaer, the water is vaporized but the salt is not. The process of absorption differs from distillation in that
one of the components in absorption is essentially insoluble in the liquid phase. An example is absorption of
ammonia from air by water, where air is insoluble in the water-air ammonia solution.
Batch Distillation
In a batch distillation, it is invariably the overhead product or a cut of it that is required and there are generally
two methods of operation by which the top product or products are obtained.
1. Varying Reflux. This is used to obtain an overhead product of constant composition. As the top product
composition becomes richer in heavier components due to the removal of the lighter fractions, the reflux
ratio is increased to maintain a constant composition. This is continued until there is so little top product
that the still is virtually running at total reflux and the operation becomes uneconomic to proceed further.
2. Constant Reflux. Under these conditions the overhead product composition continually changes, gradually
becoming richer in the less volatile components. One or more cuts can be taken at various intervals to give
top products of required composition.
For the system as shown in Fig. 4.1, a simple still is shown. Originally, a charge of L1 moles of components A
and B with a composition of x1 mole fraction of A is placed in the still. At any given time, there are L moles of liquid
left in the still with composition x and the composition of the vapor leaving in equilibrium is y. A differential amount
of dL is vaporized.
The composition in the still pot changes with time. For deriving the equation for this process, we assume that a
small amount of dL is vaporized. The composition of the liquid changes from x to x-dx and the amount of liquid
from L to L-dL. A material balance on A can be made where the original amount equals the mount left in th eliquid
plus the amount of vapor.

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Fig. 4.1 Simple batch distillation.

Multiplying out the right side,

Neglecting the term dx dL and rearranging,

Integrating,

where L1 is the original moles charged, L2 the moles left in the still, x1 the original composition, and x2 the final
comosition of the liquid.
The integration of this equation can be done graphically by plotting 1/ (y-x) versus x and getting the area under
the curve between x1 and x2. The equilibrium curve gives the relationship between y and x. This equation is known
as the Rayleigh equation. The average composition of the material distilled, yave, can be obtained by a material
balance.

This experiment demonstrates the use of constant reflux to obtain a top product of a specified average
composition (0.95 mole fraction of methanol) by batch distillation of a binary mixture of methanol and water of
composition 50% w/w.
Reflux Ratio
In large scale and industrial operations, the reflux ratio plays an important part, both economically and
practically in the design and operation of such units. The reflux ratio can be defined as the weight of the top
product removed as product. At total reflux, infinite reflux ratio, the separation achieved is maximum. However this
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is the least economic method of operation because the amount of product is minumum and large supply of energy
are required in heating the mantle.
At the other end of the scale, working at zero reflux, all top products are removed, the separation achieved is a
minimum. In this case, to achieve a desired top product a column of maximum height is required.
Therefore, a balance has to be found to minimize the cost of the column, in terms of height, diamter, running
costs, compatible with a specified top product, by using the optimum reflux ratio to achieve this.
This experiment demonstrates the variations in top product, which can be achieved, in a column of fixed
dimensions, solely through variation of the reflux ratio.
Vacuum Distillation
The relative ease of separation of a binary mixture can be readily determined by inspecting the vapor-liquid
composition/temperature curve (commonly known as lens diagram due to its shape). Separation will be easy if the
lens is a flat one and more difficult if it is a thin one, providing no complications occur e.g. presence of azeotropes.
This diagram varies with pressure in several ways.
Decreasing the total pressure on the system lowers the whole diagram, thus boiling points are obviously
reduced under reduced pressure. Conversely, increasing the total system pressure decrease the relative volatility
of the components with respect to each other and this shows as a thinning in the lens diagram making separation
more difficult. Due to the increased pressure, boiling points will also be increased. However, if the total pressure of
the system is increased to the critical pressure of one of the components, complete separation becomes possible.
It can be seen therefore that operation under vacuum should lead to a more efficient separation of the feedstock
mixture. In the following experiments, the effects of vacuum on the binary system of methanol / water are
investigated.
4. Resources:
Equipment: Distilling Column

Materials: Methanol-Water Solution

5. Procedure:
I.

Batch Distillation
1. Check the unit or set-up (instrumentation panel, glass connection specially the glass shopper
on the glass vessel and thermometer probe connection in the unit).
2. Fill up the vessel with 50% w/w methanol / water solution. The height of the liquid should be 1
2 above the heating mantle.
3. Switch ON the instrumentation panel, voltmeter, and the red light function. If not, see to it that
the circuit breaker found on the wall near the unit is turned ON.
4. Switch ON the heating mantle.
5. Turn ON the gate valve of the condenser when the liquid starts to boil.
6. Close the stopcock of the glass receiver.
7. When the distillate start to fall on the glass receiver, measure time and the volume by opening
the stopcock. This enables you to get the total reflux.
8. During frequent interval, simultaneously take a sample of the distillate and a sample from the
glass vessel; measure temperature and specific gravity for each sample.
9. Continue until the distillate composition falls to approximately 0.95 mole fraction methanol.
10. Stop the operation by turning OFF the power and circuit breaker.
11. Turn OFF the gate valve of the condenser when boiling has stopped.

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II.

Reflux Ratio
1. Operate the unit as per Procedure I.
2. Vary and measure the reflux ratio between zero and total reflux.
3. For each value of reflux ratio, determine the top product composition by measuring the
specific gravity and temperature of a sample.
4. Draw the McCabe-Thiele diagram for the various reflux ratio and top products. Plot top
product composition against reflux ratio. In the absence of economic factors, estimate the
optimum reflux ratio to obtain product of specific composition.

III.

Vacuum Distillation
1. Operate the unit as per Procedure I.
2. Fill up the vessel with 30% w/w methanol/water solution instead of 50% w/w methanol/water
solution.
3. Turn ON the vacuum pump and maintain at 200 mmHg.
4. Measure the temperature at the TOP and BOTTOM of the glass column.
5. Get the reflux ratio by measuring the time and volume of the distillate.
6. Measure the specific gravity and temperature of the samples (distillate and solution).
7. Repeat for different reflux ratio, taking a sample at each value of reflux ratio.
8. If time permits, repeat the experiment at atmospheric pressure.
9. Stop the operation by turning OFF the power and the circuit breaker.
10. Turn off the gate valve of the condenser when the boiling has stopped.
11. From the temperature measurements and the vapor-liquid composition vs temperature curve
at 200 mmHg, the composition at the top and bottom of the column can be found. McCabeThiele diagram can be drawn as the number of theoretical stages present in the column can
be found for each other reflux ratio under both atmospheric and vacuum conditions. Construct
graphs of number of theoretical plates vs reflux ratio for vacuum and atmospheric conditions.
12. For various reflux ratio, calculate the percent change in number of theoretical plates from
values at atmospheric pressure.

NOTE:
The reflux ratio may be calculated from the expression

where: R reflux ratio

t1 time taken to half fill product receiver on total off-take
t2 time taken to half product receiver when set to a particular reflux ratio

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6. Data and Results:

Course:
Group No:
Group Members:

Expeiment No:
Section:
Date Performed:
Date Submitted:
Instructor:

Batch Distillation
Sample

Time

Volume

Temperature

Composition of Distillate

1
2
3
4
5
6
7
8

Reflux Ratio
Sample

Time

Volume

Reflux Ratio

Temperature

Composition of
Distillate

Time

Volume

Reflux Ratio

Temperature

Composition of
Distillate

1
2
3
4
5
6
7
8

Vacuum Distillation
Sample
1
2
3
4
5
6
7
8

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Graphs:

29

7. Calculations:

30

8. Concusion:

9. Questions/Problems:
1. Discuss the different distillation methods?
2. What is relative volatility?
3. Derive the equations for enriching section, stripping section and feed line.
4. Differentiate total and minimum reflux ratio.
5. A mixture of 100 kgmol which contains 60 mol% n-pentane and 40 mol% n-heptane is vaporized at 101.32
kPa under differential conditions until 40 kgmol are distilled. Using equilibrium data:
a. What is the average composition of the total vapor distilled and the composition of the remaining
liquid?
b. If this same vaporization is done in an equlibrium or flash distillation and 40 kgmol are distilled,
what is the composition of the vapor distilled and of the remaining liquid?
6. Calculate the approximate minimum number of stages for a binary system with relative volatility of 2.35,
fractionally distilled to yield compositions of 0.98 in the distillate and 0.045 in the bottoms.
7. A rectification column is fed 100 kgmol/h of a mixture of 50 mol% benzene and 50 mol% toluene at 101.32
kPa abs pressure. The feed is liquid at the boiling point. The distillate is to contain 90 mol% benzene and
the bottoms 10 mol% benzene. The reflux ratio is 4.52:1. Calculate the kgmol/h distillate, kgmol/h bottoms,
and the number of theoretical trays needed using the McCabe-Thiele method.
10. Answers:

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11. Further Readings:

Cao, E. (2010). Heat transfer in process engineering. Boston: McGraw-Hill Professional.
Cussler, E. L. (2009). Diffusion: mass transfer in fluid systems (3rd ed. United Kingdom: Cambridge University
Press.
Koenig, D. (2009). Practical control engineering: a guide for engineers, managers and practitioners. New York:
McGraw-Hill Professional.
Mann, U. (2009). Principles of chemical reactor analysis and design. New Jersey: John Wiley & Sons.
Johnson, W. (2009). Practical heating technology. Australia: Delmar Cengage Learning.

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12. Assessment (Rubric for Laboratory Performance):

BEGINNER
1

CRITERIA

ACCEPTABLE
2

PROFICIENT
3

I. Laboratory Skills
Manipulative
Skills

Members do not
demonstrate needed
skills.

Experimental
Set-up

Members are unable to

set-up the materials.

Process Skills

Members do not
demonstrate targeted
process skills.

Safety
Precautions

Members do not follow

safety precautions.

Members occasionally
demonstrate needed
skills.
Members are able to
set-up the materials with
supervision.
Members occasionally
demonstrate targeted
process skills.
Members follow safety
precautions most of the
time.

Members always
demonstrate needed
skills.
Members are able to
set-up the material with
minimum supervision.
Members always
demonstrate targeted
process skills.
Members follow safety
precautions at all times.

II. Work Habits

Time
Management /
Conduct of
Experiment

Members do not finish

on time with incomplete
data.

Cooperative
and
Teamwork

Members do not know

their tasks and have no
defined responsibilities.
Group conflicts have to
be settled by the
teacher.

Neatness and
Orderliness
Ability to do
independent
work

Members finish on time

with incomplete data.

Members have defined

responsibilities most of
the time. Group conflicts
are cooperatively
managed most of the
time.
Clean and orderly
workplace with
Messy workplace during
occasional mess during
and after the experiment.
and after the
experiment.
Members require
Members require
supervision by the
occasional supervision
teacher.
by the teacher.

Other Comments / Observations:

Members finish ahead of

time with complete data
and time to revise data.
Members are on tasks
and have defined
responsibilities at all
times. Group conflicts
are cooperatively
managed at all times.
Clean and orderly
workplace at all times
during and after the
experiment.
Members do not need to
be supervised by the
teacher.
TOTAL SCORE

RATING = ( TotalScore ) x 100%

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SCORE