ABSTRACT

Packed distillation column experiment was conducted to study the effect of

operational time on the composition and volume of the product distillate and also to study the
correlation between the volume of the product distillate and the composition of the product
distillate. The experiment was started by preparing ethanol-water mixture for obtaining their
refractive index, after that the packed distillation was conducted and the experimental data
was collected for every 5 minutes, and at the same time the volume of distillate methanol also
been measured. The graph of mole fraction and volume of product versus time was plotted.
From the graph, we can see that the composition of methanol increasing throughout the
experiment, and the mole fraction of methanol remain constant at 30%. Lastly, from the
volume product graph, this shows that when the time increases, the volume of the distillate
will increase.

1.0

INTRODUCTION
1.1 Experimental Background
Distillation is the separation of one substance from another by evaporation and

condensation. The product obtained by distillation is called the distillate. This process is used

for purifying liquids having undesired substances in them, for separating different kinds of
liquids from each other, and for producing chemical changes in solid substances.

Many types of distillation columns have been introduced, each designed to perform
specific types of separations, and each design differs in terms of complexity. One way of
classifying distillation column type is to look at how they are operated. They have batch and
continuous column. Batch column is the feed to the column is introduced batch-wise. That is,
the column is charged with a 'batch' and then the distillation process is carried out. When the
desired task is achieved, a next batch of feed is introduced. While, the continuous column is
process a continuous feed stream. No interruptions occur unless there is a problem with the
column or surrounding process units.

Distillation columns are made up of several components, each of which is used either
to transfer heat energy or enhance material transfer. A typical distillation contains several
major components that are a vertical shell where the separation of liquid components is
carried out, column internals such as trays/plates and/or packings which are used to enhance
component separations, a reboiler to provide the necessary vaporisation for the distillation
process, a condenser to cool and condense the vapour leaving the top of the column and a
reflux drum to hold the condensed vapour from the top of the column so that liquid (reflux)
can be recycled back to the column.

The terms trays and plates are used interchangeably. There are many types of tray
designs, but the most common ones are bubble cap trays, valve trays and sieve trays. Bubble
cap trays have riser or chimney fitted over each hole, and a cap that covers the riser. The cap
is mounted so that there is a space between riser and cap to allow the passage of vapour.
Vapour rises through the chimney and is directed downward by the cap, finally discharging
through slots in the cap, and finally bubbling through the liquid on the tray. In valve trays,
perforations are covered by liftable caps. Vapour flows lifts the caps, thus self creating a flow
area for the passage of vapour. The lifting cap directs the vapour to flow horizontally into the
liquid, thus providing better mixing than is possible in sieve trays. While the sieve trays are
simply metal plates with holes in them. Vapour passes straight upward through the liquid on
the plate. The arrangement, number and size of the holes are design parameters.
1.2 Objective

In this experiment, the objectives of the study are to study the effect of operational
time on the composition and volume of the product distillate and to study the correlation
between the volume of the product distillate and the composition of the product distillate.

1.3 Scope of Study

The scope of this study is distillation process which is using packed distillation
column because of their most commonly is material in the column tray because of their
efficiency, wide operating range, and ease of maintenance and cost factors. This experiment
is carried out in order to give more understanding in the process of distillation.

2.0

LITERATURE REVIEW

Packed column distillation is a common technique used for fractional distillation. Some
advantages of packed column distillation are
Efficiency:

Packed column distillation apparatus have up to 45 theoretical plates at

atmospheric pressure. Packed distillation columns can be stacked for even higher efficiencies.
Scalable: Packed column distillation systems can be scaled up from small laboratory units up
to much larger industrial sizes. B/R produces packed columns with up to 2000 liter boiler
capacities.

High Throughput: Packed column distillation can produce high distillation rates. Our largest
packed distillation column can distill over 100 liters per hour.
All distillations attempt to separate a lower boiling material (A) from a higher boiling
material (B). Packed columns are "packed" with a material that creates a large surface area
within the distillation column. Vapors rise through the column, are condensed by the
condenser and fall back down the column. This material is called the condensate. The
descending condensate "wets" the packing. Ascending vapors rise through the wet packing
and are forced into intimate contact with the condensate. This intimate contact causes the
vapor to become enriched in the lower boiling material. This process is often called
rectification.

Distillation is a commonly used method for purifying liquids and separating mixtures of
liquids into their individual components. Familiar examples include the distillation of crude
fermentation broths into alcoholic spirits such as gin and vodka, and the fractionation of crude
oil into useful products such as gasoline and heating oil. In the organic lab, distillation is used
for purifying solvents and liquid reaction products.

The boiling point of a pure liquid is defined as the temperature at which the vapor pressure of
the liquid exactly equals the pressure exerted on it by the atmosphere and is one of its
characteristic physical properties. The boiling point is used to characterize a new organic
liquid, and knowledge of the boiling point is used to compare one organic liquid with another,
as in the process of identifying an unknown organic substance.
The boiling point of a mixture is a function of the vapor pressures of the various components
in the mixture. Impurities either raise or lower the observed boiling point of a sample,
depending on how the impurity interacts with the compound for which the boiling point is
being measured.
At any temperature, some molecules of a liquid possess enough kinetic energy to escape into
the vapor phase (evaporation) and some of the molecules in the vapor phase return to the
liquid (condensation). Equilibrium is set up, with molecules going back and forth between
liquid and vapor. At higher temperatures, more molecules possess enough kinetic energy to
escape, which results in a greater number of molecules being present in the vapor phase
(McCabe et al. 2005).

Unfortunately, each time of fractional distillation is run, material is lost. Some evaporates into
the air and some is left behind, stuck to the apparatus. Material left behind is known as holdup. We would find that after doing three separate simple distillations, we have lost much
material. Besides obtaining pure compounds we also want to attain high yields, with little loss.
A method exists for carrying out several simple distillations in one apparatus, thereby
resulting in smaller losses. This method is called fractional distillation.

In a simple distillation this is done one time. In a fractional distillation, as the vapor ascends
the column, it encounters a cooler area and condenses. The hot ascending vapors revaporize
the liquid and the vapor travels further up the column, where it encounters a cooler area and
recondenses. Hot ascending vapors revaporize the liquid and it travels a bit further. Each
vaporization-condensation cycle is equivalent to a simple distillation so by the time the vapor
reaches the top of the column, it has undergone several simple distillations, and has thus
undergone further purification than in the simple distillation apparatus. Because it was done
in one apparatus, much less material is lost and the yield is greater than if several separate
simple distillations had been done. Note however that even in a fractional distillation, some
material is lost to evaporation and some is left behind in the apparatus (hold-up).
Distillation is a sacrificial process in that some material is always lost, no matter how careful
or experienced the chemist. Minimizing the loss is an important goal.
The number of vaporization-condensation cycles that can occur within a fractionation column
determines the purity which can be attained. The efficiency of a column depends upon
column length and composition. In the fractionation column used in this lab, the column is
packed with copper sponge. This increases the surface area that the ascending vapor
encounters and results in more vaporization-condensation cycles compared to an empty
column. A measure of efficiency of a column is known as the number of theoretical plates of
that column. One theoretical plate is equivalent to one vaporization-condensation cycle,
which is equivalent to one simple distillation. Thus a fractionation column that can attain the
equivalent of three simple distillations would be said to have three theoretical plates
(Geankoplis C.J, 2003).

The purpose of reflux is to get distillate with higher purity. The reflux ratio can be described
as follow:

There are two cases of reflux, which is maximum reflux and minimum reflux. Maximum
reflux happens when all the vapor returned to the column as reflux, which is no feed going
back and none of the product is produced. In this case also, the number of separation stages
required is minimal. Minimum reflux involves the infinite number of separation stages.
However, this situation is impossible to occur.
To obtain optimal results, a suitable reflux ratio should be selected. The selection of a suitable
reflux depends on the operating costs, especially steam and capital costs associated with the
number of plates used. In theory, the optimum reflux ratio is 1.1Rm <Ropt <1.5 Rm (Gavhane,
2009).

3.0

METHODOLOGY
3.1 Experimental Procedure
Seven ethanol-water mixtures are prepared by using pipette. The refractive indexes of

the mixtures are obtained by using refractometer. 32 litres of methanol-water feed mixture is
prepared with composition of 30% methanol and 70% water. All equipment must be making
sure in place and in good condition before starting the experiment. V2 valve is adjusted to be
open and RCV1 valve, V3 valve and V4 valve are adjusted to be close. The electric heater is
opened simultaneously with the coolant flow pump. The reflux ratio at 2.0 or 3.0 is set up by
slowly opening the reflux control valve, RCV1 and the product distillate will flow to RI 1B.
The rest of the product distillate will flow through RI 1A and return to the reboiler vessel. In
order to collect product distillate which does not return to the reboiler vessel, V2 valve, V3
valve and V4 valve must be adjusted. For V2 valve, it must be closed while V3 valve is
opened but if V4 valve is opened, V3 valve must be closed. Then, V4 valve should be opened.
The volume and refractive index of the collected product distillate are measured. The steps
are repeated for every 5 minutes and the table given is filled up.

3.2 Equipment/Materials
a) Bubble cap distillation column
b) Refractormeter
c) Syringe
d) Measurement cylinder
e) Reagent bottle

f) Stop watch
g) Water
h) Ethanol
From the graph of refractive index versus % mole of methanol(Graph 1), we can use it to
determine the % mole of methanol in Part 2. Based on Graph 1, the result is obtained in
Table 2.
Example calculation for Part 2:
From Graph 1, the equation that relates refractive index and % mole of ethanol is

At t = 10 min, refractive index is x = 1.3291

=>
x = 31.22 %

mole fraction of methanol

mole fraction of methanol versus time

33
31
29
27
25
23
21
19
17
15

y = 0.040x + 24.77

10

20

30

40

50

Time
Graph 2: Mole fraction of methanol versus time

60

70

Volume of Distillate (mL)

400
350
300
y = 1.451x + 250.26

250
200
150
100
50
0
0

10

20

30
40
Time (min)

50

60

70

Graph 3: Volume of distillate versus time

5.0

DISCUSSION

Graph 1: Refractive index versus % Mole of ethanol

Based on Graph 1, the graph shows a curve that represents the relationship between
the refractive index for ethanol-water mixture. The curve shows a maximum point of
refractive index at a certain composition of mixing. This shows that the refractive index for a
mixture will reach a maximum point at some mixing composition. Later, the graph used as
standard graph to determine the composition of methanol by the known value of refractive
index for distillate.

Graph 2: % Mole of distilled methanol versus time

The methanol composition in the distillate is increasing with the time as shown in
Graph 2. Theoretically, methanol has a lower boiling point compared to the water, hence at
early stage of distillation, the composition of methanol is higher than water. Thus, there is an
error occurred during handling the experiment.
Graph 3: Volume of distillate versus time

From graph 3 the volume of distillate increase with time or in the other hand can
conclude that volume of distillate is proportional to time. As refer to the ratio of the reflux,
the ratio of the reflux increase at the end of the experiment. The higher the ratio of reflux
caused more reflux flow back to the column without flow out as the distillate. The graph
gives positive slope shown the exact situation in the system. .

5.1

ADVANTAGES OF THE PACKED COLUMN DISTILLATION

There are a lot of advantages of the packed column distillation that is the larger

supporter of the end of the system can solve the floating problem at the supporter part. The
packed column is make of material ceramic, carbon or material entertain erosion that allow
the acidic solution and erosion material operated with it. For pillar that diameter less than 0.6
meter (2.0ft), packed column is cheaper than other plat pillar except the packed column which
is made of alloy. The properties of low pressure fall allow the usage in distillation process
vacuum critical. Packed column can operate with the large distance of the mixture flow rate
under a constant efficient of equipment. Liquid that form bubbles can be transfer more
effective in packed column because of lower relative disturbance degree of liquid for gas. The
installation of packed column is easier than other plat column that needs a cautious design to
have good performance.

5.2

ERRORS IN THIS EXPERIMENT

Errors is cannot avoided in each experiment. Below are the errors that occurred during
this experiment:

i.

Parallax errors exist when reading from thermometer, reading for reflection index,
reading from the volume of distillate because the eyes is not parallel with the
reference.

ii.

The level fluid in RI 1B is not in the 2.0 and always change because of the difference
in the volume of distillate.

iii.

Systematic errors also occurred when taking the result from stop watch.

iv.

The leakage maybe occurred at the valve V2 and V3 when it closed and opened for
the respective valve and it caused the volume for methanol distillate changed.

v.

The thickness of the layer is difference each time so that it makes the reading not
accurate. The glass of that apparatus in not clean and wet to makes the reading not
accurate.

vi.

The possibility of the distillate volume of methanol is less than the true volume
because some of the methanol is evaporated to the air. This is because when distillate
of methanol takes out from valve V4, where the solution temperature of methanol is
higher than ambient temperature.

vii.

There is dirt at the used apparatus is polluted and after that affect the experiment
result.

viii.

There is some methanol entrapped or pasted at the mouth of the valve that make the
volume not accurate.

5.3

PRECAUTION STEPS
1. The mirror of the refractometer must wash with distill water after every reading of the
deflection index.
2. The mixture of water methanol need to shake to make sure the solution is similarly.
3. The eyes or the observer must always at the erect position to avoid errors.
4. Reflux RI 1B must always at 2.0.
5. All the apparatus must in clean condition.
6. The flow of cooler water must continuous during the experiment to make sure the
system can be cool down and get the distillated product.
7. The operation temperature must at 1000C during the experiment. This is because the
water will boil and evaporate at the temperature.
8. All the valve must be tight enough.

6.0

CONCLUSION
This experiment is lack accuracy as the relationship between mole fraction and time,

volume of distillate and time could not be determined since the graph were not a smooth
curve or straight, they only can be estimated. This may due to some error happened during
experiment.

Graph 1 is used to estimate the composition of methanol in the distillate. Graph 2 is

graph of negative slope, showing that the composition of methanol in the boiler is increasing
as more amount of methanol was distillate. Graph 3 shows that the volume of distillate is
increasing with time.

7.0

RECOMMENDATIONS
All of the errors however, can be reduced or overcome by taking precautionary steps

throughout the experimental procedures. First, it is important to ensure that all the apparatus
needed are rinsed properly and clean enough so that there will be no impurities contained
inside the apparatus. Readings or measurement should be done thoroughly to avoid any
possible errors such as parallax error. Proper handling and storing of volatile compound such
as ethanol may help to maintain its volume throughout the experiment. The refractive index
of the ethanol must be tested two or more times in order to get the best results.

8.0

REFERENCES
1. Geonkoplis, C. J., Transport Process & Separation Processes Principles, 4th Edition.
Prentice Hall, 2003.
2. Mc Cabe, W.L.,Smith, J.C & Harriot, P., Unit Operation of Chemical Engineering,
4th Edition, Mc Graw-Hill, 1985.
3. Treybal, R. E. (1963) Liquid Extraction. McGraw Hill, NY.