ABSTRACT

This experiment was carried out to determine the efficiency of a distillation process using an
alcohol/water solution. Distillation, which is the separation of components of a mixture by
continuous evaporation and condensation exploiting their difference in volatility was carried out
using the armfield continuous distillation column.

The experiment was performed at steady state by setting the reboiler to a constant heating
temperature. In order to achieve high purity of product a reflux ratio of 5:1 was used; this implies
that for every 6 moles of condensate at the overhead product, 5 moles is returned as reflux while
just 1 mole is collected as product. This is because the presence of a component with very close
volatility will cause another component to behave differently.

The experiment also employed the use of the Lewis Sorel Method for calculating the number of
theoretical plate. This method involves plotting a graph of an equilibrium data and using the Top
operating line equation and bottom operating line equation to deduce the theoretical number of
plate. From the graph, the theoretical number of plates was 4. The distillation process was then
determined to be 25% efficient. Possible source of error could have resulted from the system
deviating from steady state. The method adopted is recommended for further experiment on
binary state distillation

1
 INTRODUCTION

Distillation is one of the separation process in chemical engineering. A separation process is a

method that converts a mixture or solution of chemical substances into two or more distinct
product mixtures. At least one product mixture of the separation is enriched in one or more of the
source mixture's constituents.

Distillation process involves the conversion of a liquid into vapor that is subsequently condensed
back to liquid form. Distillation is used to separate liquids from non-volatile solids, as in the
separation of alcoholic liquors from fermented materials, or the separation of two or more liquids
having different boiling points, as in the separation of gasoline, kerosene, and lubricating oil
from crude oil. Other industrial applications include the processing of chemical products such as
formaldehyde and phenol and the desalination of seawater. . Distillation process is the most of
common separation used in industry because it is known as 90% efficiency in separation process
and significantly user of energy in the heating process that necessarily involved. A distillation
column is used to carry out the separation process, a distillation column is a tube that provides
surfaces on which condensations and vaporizations can occur before the gas enters the condenser
in order to concentrate the more volatile liquid in the first fractions and the less volatile
components in the later fractions.

Fig.1.0 Schematic of a Distillation Column

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In a petroleum distillation unit, the feedstock liquid mixture is usually introduced near the middle
of the column, to a tray known as the feed tray. This tray divides the column into a top
(enriching, rectification) section and a bottom (stripping) section. The feed flows down the
column where it is collected at the bottom in the reboiler. Heat is supplied to the reboiler to
generate vapor. The source of heat input can be any suitable fluid. In most chemical plants it is
normally steam, and the heating source may be the output streams of other columns. The vapor
raised in the reboiler is re-introduced into the unit at the bottom of the column. The liquid
removed from the reboiler is known as the bottoms.

Rectification section; at the rectifying section, the more volatile component is removed
through contacting the rising vapor with the down-flowing liquid
Stripping section; at the stripping section, the down-flowing liquid is stripped of the
more volatile component by the rising vapor.
Distillation is a core process that is fundamental to the economic operation of any process
plant. Successful outcomes depend on quality distillation monitoring and troubleshooting since
just about every operation uses some form of distillation equipment or fractionating Columns.
The purpose of the Experiment was to determine the efficiency of the Distillation column in
separating Binary Mixtures of near Volatility, which in this Case was Ethanol and Water.

3
 THEORY

Distillation is the process of separating the components or substances from a liquid mixture by
using selective boiling and condensation. It uses the differences in the volatility of the different
components to separate the mixture. Distillation is used for many commercial processes, such as
the production of gasoline, distilled water, xylene, alcohol, paraffin, kerosene, and many other
liquids. Gas may be liquefied and separate. For example: nitrogen, oxygen, and argon are
distilled from air.

There exist various method for carrying out distillation process. it is seen that, for a binary
mixture with a normal y −x curve, the vapour is always richer in the more volatile component
than the liquid from which it is formed. There are three main methods used in distillation
practice which all rely on this basic fact. These are:

o Differential distillation.

o Flash or equilibrium distillation, and

o Rectification.

THE FRACTIONATING COLUMN

Fig 2.0
The distillation column is made up of a series of stacked plates. A liquid feed containing the
mixture of two or more liquids enters the column at one or more points. The liquid flows over
the plates,

4
and vapor bubbles up through the liquid via holes in the plates. As liquid travels down the
column, the vapor comes in contact with it several times due to the multiple plates – a critical
process in distillation columns. The liquid and vapor phases are brought into contact because as
one molecule of higher boiling material converts from vapor to liquid phase by energy release,
another molecule of the low boiling material utilizes the free energy to convert from liquid to
vapor phase.

The base of the distillation column contains a large volume of liquid consisting mostly of the
liquid with higher boiling point (in our example, this would be water). Out of the base flows
some of this liquid, some of which is heated in the re boiler and returned to the column.

DETERMINATION OF NUMBER OF PLATES

A binary feed F is distilled to give a top product D and a bottom product W, with , , and
as the corresponding mole fractions of the more volatile component, and the vapour Vt rising
from the top plate is condensed, and part is run back as liquid at its boiling point to the column as
reflux, the remainder being withdrawn as product, then a material balance above plate n gives;

F=D+W ………………………. (1)

Expressing this equation for the more volatile component (MVC) gives;
F.Xf = D.Xd + W.Xw ……………………………(2)
This equation relates the composition of the vapour rising to the plate to the composition
of the liquid on any plate above the feed plate. Since the molar liquid overflow is constant, may
be replaced by
V n=L n+1 + D
doing the component balance of ethanol for the rectification section
V n y n=Ln +1 x n+1 + D x d
Ln +1 D
yn= x n+1 + x d … … … … … … … ..(3)
Vn Vn

Similarly, taking a material balance for the total streams and for the more volatile component
from the bottom to above plate m,
Lm=V m+ W

Vm = L m – W

Doing the component balance of Ethanol in the stripping Section

y m V m=Lm x m+1 −W x w

5
 Lm W
y m= x − x … … … … … … … ..(4)
V m m +1 V m w

Fig.3.0 Calculation of number of plates by Lewis Sorel method.

With the two equations and the equilibrium curve (Which was Obtained from plotting the
Equilibrium Curve from the given Equilibrium Data , the composition on the various plates may
be calculated by working either from the still up to the condenser, or in the reverse direction.
Since all the vapour from the column is condensed, the composition of the vapour from the top
plate must equal that of the product , and that of the liquid returned as reflux .
number of Actual plate
The efficiency of the system = × 100 … … … … … .(5)
number of Theoretical plate

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 DESCRIPTION OF APPARATUS

CONICAL FLASK: An Erlenmeyer flask, also known as a conical flask (BrE) or a

titration flask, is a type of laboratory flask which features a flat bottom, a conical body, and a
cylindrical neck and is used for making solutions or for holding, containing, collecting, or sometimes
volumetrically measuring chemicals, samples, solutions, etc. for chemical reactions or other processes
such as mixing, heating, cooling, dissolving, precipitation, boiling (as in distillation), or analysis. The
conical flask was used to mix the solutions and starch indicator which were used for titration during the
experiment.

Fig 1: conical flask

MEASURING CYLINDER: A graduated cylinder, measuring cylinder or mixing cylinder is
a common piece of laboratory equipment used to measure the volume of a liquid. It has a narrow
cylindrical shape. Each marked line on the graduated cylinder represents the amount of liquid that has
been measured. It was used to measure the volume of the potassium iodide solution and potassium
persulphate solution required during the experiment.

Fig 2: measuring cylinder

REFRACTOMETER: Refractometer is a special tool designed for the measuring of the liquid
characteristics using the light refraction.

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 Fig 3: refractometer

Condenser

Rotameter

Re-boiler

Control

Fig 4: chemical engineering fractional distillation set-up

The Armfield continuous distillation column consists of two units. The process unit and the control
unit (also known as control console). The process unit is where the entire distillation process is
carried out while the control unit is where the various parameters and properties for process is set.
Various parts of the process unit include:

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The Reflux Valve: It connects the decanter back to the distillation column for reflux. The reflux
ratio is set on the control unit.
The Decanter: which is the vessel collecting condensate, equipped with double overflow weirs and
exit pipes. The decanter is connected to the reflux valve and the top product receives.
Feed Tanks: This is where the feed mixture was introduced into the apparatus.
Reboiler: This is where the boiling of the feed occurs. It has a heater attached to it. The heater supplies
the heat energy.
Feed Peristatic Pump: which pumps the feed from the feed tanks.
Heat Exchanger: which transfer heat from the product stream of the bottom to the feed stream.
Bottom Product Receives: This receives the bottom product of the process.
The Column: This consists of 8 trays where the distillation occurs. The feed enters the column at a
point called the column feed point.
The Condenser: This is where the vapor from the distillation column turns back into liquid. The
condenser has cooling water flowing around and on it.
The Rotameter: This measures the flowrate of the cooling water. The flowrate of the cooling water is
also adjustable.
The Top Product Receiver: It contains the final distillate.
Dosing Vessel: It is used in cases of azeotropes. It contains desiccants used to strip the unwanted
components.

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 PROCEDURE

o The Turn power to the control panel was turn on .

o The temperature selector switch was set to T9, the temperature in the re-boiler, and open valve
V5 admitting the cooling water to the condenser at a flow rate on FI1 of Approximately 3
liters/min. This rate was varied according to the temperature of the water. If there is insufficient
water flow, some of the vapour will be uncondensed and emerge from the vent pipe at the side of
the unit in which case increase the water flow rate. If required, admit cooling water to the bottom
product cooler. This is not always necessary sufficient cooling takes place in the pipework to
reduce the product temperature from the boiling point.

o On the control panel the power controller was turned on, for the re-boiler heating element fully
anti-clockwise and the switch turning on the power to the heating element was changed to
“power on” position. The power controller was turned on clockwise until a reading of
approximately 1.5 kW is obtained on the digital wattmeter.

The contents of the re-boiler began to warm up and this was observed on the temperature readout
meter.

o Eventually, vapour began to rise up the column and the progress of this was clearly observed as
well as detected by the increasing temperatures when switching the temperature selector on T8,
T7, T6, T5, T4, T3, T2 and T1. Vapour enters the condenser and reappears as droplets into the
glass walled distillate receiver vessel. The distillate builds up a small level in the receiver and
eventually overflows to the reflux regulator valve.

o The cool distillate was then returned to the top of the column and cascade down the trays
forming a liquid level on the trays and bubbling of vapour passing through the liquid. The system
reached an equilibrium condition when the temperatures T1, T2, T3, T4, T5, T6, T7 and T8 have
reached an average steady temperature (but note cycling due to the intermittent reflux).

o Before the reflux switch was switched on, reflux ratio was set to 5:1, meaning 5 part was set
back to column and 1 set to the top product receiver, (see Operational section). C- means back to
column and C+ means to top product receiver. When this was completed, the reflux valve was
switched on (on the control panel).

o The feed to the column was admitted at the mid point (onto tray 5). When the column had
stabilised at total reflux (it took 15 to 30 minutes), the flow of feed and the reflux started at the
same time. The feed flow was set to 2 litres/hr (from the feed pump calibration graph).

o As the flow into the column becomes established so more vapour rose up the column and appear
as condensate in the distillate receiver, allowing this to flow to the top product receiver. After
feeding approximately 3 litres a sample of the overheads was taken through valve V3.

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 RESULT

Table 1.0 Correlation data between actual reading and brix reading

Brix %Alcohol (Ethanol)

30 9.77

40 16.70

60 23.66

80 30.61

100 37.55

130 47.97

Table 1.0 From Interpolation of table 1.0

Feed 0.2388

Distillate 0.782

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 Table 3.0 Equilibrium data used

x 0.0035 0.0175 0.0585 0.0935 0.2125 0.3615 0.4985 0.6460 0.723 0.837 0.888 0.9489 0.9835

y 0.0175 0.1315 0.305 0.411 0.5455 0.6060 0.655 0.729 0.776 0.852 0.893 0.9502 0.9835

Table 4.0 Composition of Streams

FEED DISTILLATE BOTTOM PRODUCT

Volume (cm3) 10000 1825 8175

Material Balance (VOLUME BALANCE)

F=D+W ………………(6)

10000 = 1825 + W
W = 8175cm3

Component Balance (Ethanol) Xd

From the refractometer the Value of Xf which is the composition of Ethanol in the Feed =
0.2
Also after the experiment the value of Xd is the Composition of Ethanol in the distillate = 1

Carrying out a Material Balance to get Xw ( the Composition of Ethanol in the Bottom)
F.Xf = D.Xd + W.Xw …………
(7)

Substituting for F = 10000cm3, W = 1435cm3 & D = 8565cm3 into the equation (1)

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((10000)*0.2) = (1825*1) + (8175*Xw)

2000 =1825 + 8175Xw

Xw = 0.021

Using McCabe thiele Method to get the Actual number of Plates

Using the Equilibrium data given in table 3.0 we obtain the Equilibrium curve which is
plotted in the graph attached to the report

To draw the rectifying operations line (ROL) we first of all use the formula below to obtain
the y-intercept for the ROL

xd
y−intersect = ………………………….(8)
R+ 1

Where Xd = the component of Ethanol in the distillate

R= the part of the product refluxed back to the column

1
y= =0.17
5+1

From the y-intersect we draw a straight line to meet Xd , and from Xd we took steps off to
meet at Xf to obtain the number of actual plate to be 4

number of Actual plate

The efficiency of the system = × 100 … … … … … … ..(9)
number of Theoretical plate

2
× 100=25 %
8

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 DISCUSSION

Distillation is the process of purifying a Liquid by successive Evaporation and Condensation

of the components of a mixture to separate out its components. In distillation we can achieve
either partial or total separation of the components of the mixture. However, in this
experiment we were able to achieve partial separation of the components of the ethanol/water
solution.The experiment also used a reflux ratio of 5:1, which indicates that for every 6
moles of condensate at the overhead product, 5 moles is returned as reflux while just 1 mole
is collected as product. The reason for introducing a reflux ratio is to ensure high purity of
product because of the close Volatility of the components which is in these case Ethanol and
Water
The higher the reflux ratio, the more vapor/liquid contact can occur in the distillation column.
So higher reflux ratio helps to achieve higher purity of the distillate. It also indicates that the
collection rate of the distillate will be slower.
Concerning the Efficiency of the Distillation Column, we must first of all determine the
number of theoretical plate. It was carried out using the Lewis Sorel’s & McCabe thiele
Method. This method assumes equimolar overflow in the rectifying section and in the
stripping section. The rectifying section consist of 2 number of plates/trays while the
stripping section consist of 4 number of plates, making a total of 8 number of plates. In order
to get the number of active plates, a plot of equilibrium data in the result Section was made.
The equilibrium data was used because in distillation it is assumed that the rate of
evaporation equals the rate of condensation, and at equilibrium no further vapour can be
boiled off to rise higher in the column.
To get the theoretical number of plates, after plotting the Equilibrum Curve the value of the
gotten from the experiment by first of all drawing the operational line of the Rectification
Section and stripping Section in the graph. We first of all trace the Xb , Xf and Xd to the 45o
line(base line) drawn in the graph. Then using the equation to get the Value of the y-
intercept of the Rectification operating line which was gotten to be 0.13 , from there a line
was drawn to join at Xd then from there we trace of Steps to determine the theoretical number
of plates which was gotten to be 2 from which the efficiency was calculated to be 25%.

Possible source of error could have resulted from deviation of the system from steady state
due to fluctuation of reboiler temperature. Another source of error could have resulted from
leakage of vapour out of the system, thereby causing the system to shift out of equilibrium.
Other sources of error could have resulted from Weeping, this is a situation which gives
lower contact surface between vapour and liquid phase. This will result in a lower mole
fraction of ethanol in the distillate. Also, when undissolved solution mixes with the distillate
it causes a wrong volume of ethanol to be recorded (flooding).

CONCLUSION

The Whole aim of the Experiment was to determine the efficiency of the Distillation column.
And after carrying out The distillation process and the necessary Calculations we got 25%
efficiency , which means that the distillation column was fairly enough to separate the

14
components of the binary mixture. This process can however be improved upon to get higher
efficiency; by introducing higher reflux ratio. The Lewis Sorel & McCabe Thiele Method for
calculating the number of theoretical plate is effective and is recommended for future
experiment on steady state binary distillation.

RECOMMENDATION

Although the experiment was proven a success, here are several recommendations students
could apply in order to increase the quality of an experiment. Students/users should ensure
that all apparatuses are in place and are functioning as they are intended to be. All electrical
appliances should be switched off after use. The reading of the vacuum gauge should be at
the eye-level to avoid errors due to parallax while taking reading. The Distillation column
should be of good quality in order to have high efficiency value.

15
 APPENDIX

GRAPH

Fig xi: Graph of yi against xi

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CALCULATIONS

Volume of feed, F = 10 L

Volume of distillate, D = 1.825 L

Concentration of feed, Xf = 30o Brix = 0.0977

Concentration of distillate, Xd = 100o Brix = 0.3755

Reflux Ratio= 5:1

Converting Litres to cm3

1 L = 1,000 cm3

F = 10 L = 10*1,000= 10,000 cm3

D = 1.825 L = 1.825*1,000 = 1,825 cm3

Overall material balance

F=D+W
W=F–D
W = 10,000 - 1,825 = 8,175 cm3

Component Balance (Ethanol)

Fxf = Dxd + Wxw
10,000*0.0977= 1,825*0.3755 + 8,175xw
977 = 685.2875 + 8,175xw
8,175xw = 977 – 685.2875
8,175xw = 291.7125
xw = 291.7125/8,175
xw = 0.0357

From theory, Top operating line equation:

ln D
yn= x n+1 + x d
Vn Vn

L
R= ; L = RD
D

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V = L + D = RD + D = D(R+1)

RD D
yn = x n+1+ x
D( R+1) D( R+ 1) d

R xd
yn = x n+1 +
R +1 R+ 1

Since reflux ration is 5 : 1

5 0.3755
yn = x + = 0.833xn + 0.0626
5+1 n+1 5+1

yn = 0.833xn + 1 + 0.0626………. (i)

Bottom operating line equation:

Lm W
ym = x m+1− x w
vm vm

Lm = Ln + F = RD + F = (5*1,825) + 10,000 = 19,125

Lm = 19,125

Lm = Vm + W;

Vm = L m - W

Vm = 19,125 - 8,175 = 10,950;

Vm= 10,950

19,125 8,175
ym = x m+1− (0.0357) = 1.7466 x m+1−0.0267
10,950 10,950

ym= 1.7466 x m+1−0.0267……… (ii)

Using Lewis-Sorel method

Top plate is found from the equilibrium curve and, since it

is in equilibrium with vapour of composition, yt = 0.3755, xt = xt−1 = 0.08

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This value of composition is sufficiently near to that of the feed, for the feed to be introduced
on plate (t − 1). For the lower part of the column, the operating line equation (ii) will be used.

Thus:

yt−2 = (1.7466 × 0.08) − 0.0160 = 0.12

from the equilibrium curve xt−2 < 0.035

This liquid xt−2 is slightly weaker than the minimum required and it may be withdrawn as the
bottom product. Thus, xt−2 will correspond to the reboiler. Therefore, theoretically, there will
be two (2) plates in the column.

Theoretical number of plates

Efficiency = x 100
Actual number of plates

Theoretical number of plates = 2

Actual number of plates = 8

2
Efficiency = x 100 = 25 %
8

Therefore, Efficiency = 25 %

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