I.

Executive Summary

The key objective of this practical was to study and understand the principles of distillation
process, the calculation procedures and methods around a distillation unit using the McGabeThiele method to assist with the theoretical plate calculation and to determine the efficiency of
the distillation column. And comparing the theoretical values to the actual values calculated in
this practical and lastly completing an energy balance around the condenser of the distillation
column unit to determine energy dislocation.

The distillation column was operated until steady state was achieved, the reboiler valve was
then closed which practically executing it to a batch distillation. One objective was to calculate
the number of theoretical plates needed for this specific distillation column and was calculated
to 2 which was not relevant since the distillation column had eight actual plates and the
efficiency loss was also accounted for therefore the lower value for theoretical plates makes no
sense
The values for theoretical plates was attained by using the McGabe-Thiele technique by
calculating the molar flow rate of the distillate and using the values to calculate the operating
line. The operating line was then plotted and the steps for estimating the theoretical plats was
done. Other objective was to do an energy Balance around the condenser, and it was done and
carried out and the calculated value of the total energy was found to be 480.3 J/s was lost to
the surroundings and then its from that it was assumed that the reaction was exothermic. The
total amount of heat was gained by the water was 239.1 J/s and the total amount of heat lost by
the distillate was 725.4 J/s It was then concluded that the experiment was carried out
successfully and all objectives was accomplished.
1. Introduction
Distillation is one of the oldest methods to separate liquids based on their volatilities and has
been used for centuries. In the modern day industrial it is mainly used for oil refining and the
manufacture of alcoholic beverages. Distillation is a method of separating the components of a
solution which depends upon the distribution of the substances between a gas and a liquid
phase, applied to cases where all components are present in both phases.
Instead of introducing a new substance into the mixture in order to provide the second phase,
as is done in gas absorption or desorption, the new phase is created from the original solution
by vaporization or condensation. In this experiment, the concern is over the separation of the
components of a liquid solution of ethanol and water. By the application of heat, the solution of
ethanol-water is partially vaporized and thereby creates a gas phase consisting of nothing but
ethanol and water. Since the gas is richer in ethanol than the residual liquid, a certain amount of
separation results. By repeated vaporizations and condensations, it is possible to make as
complete a separation as desired, recovering both components of the mixture in as pure a state
as needed. In the following report, the determination of the number of trays of the distillation
column is the main focus of the experiment. The number of trays will be determined
theoretically. The use of flow rates and temperatures are needed to determine the theoretical
number of trays which will be calculated

2. Aim
a) Acquaint the students with the concept of Continuous Distillation
b) Calculate the number of theoretical plates
c) Perform an energy balance across the condenser

2. Theory
2.1 Basic distillation Principles
2.1.1 Distillation theory
Distillation is the separation of components from a liquid mixture depending on the differences in
boiling points of the individual components. Also, depending on the concentrations of the
components present, the liquid mixture will have different boiling point characteristics.
Distillation processes depends on the vapor pressure characteristics of liquid mixtures.
2.1.2 Vapor Pressure
The vapor pressure of a liquid at a particular temperature is the equilibrium pressure exerted by
molecules leaving and entering the liquid surface interface
2.1.3 Boiling Point Diagrams
The boiling point diagram shows how the equilibrium compositions of the components in a liquid
mixture vary with temperature at a fixed pressure. Consider an example of a liquid mixture
containing 2 components (A and B) a binary mixture. This has the following boiling point
diagram

Figure 1

The boiling point of A is that at which the mole fraction of A is 1. The boiling point of B is that at
which the mole fraction of A is 0. In this example, A is the more volatile component and therefore
has a lower boiling point than B. The upper curve in the diagram is called the dew-point curve
while the lower one is called the bubble-point curve. The region above the dew-point curve
shows the equilibrium composition of the superheated vapor while the region below the bubblepoint curve shows the equilibrium composition of the sub cooled liquid.

Dew-point: the temperature at which the saturated vapor starts to condense.

Bubble-point: the temperature at which the liquid starts to boil.
2.1.4 Relative Volatility
A measure of the differences in volatility between 2 components, and hence their boiling points.
It indicates how easy or difficult a particular separation will be. Thus if the relative volatility
between 2 components is very close to one, it is an indication that they have very similar vapor
pressure characteristics. This means that they have very similar boiling points and therefore, it
will be difficult to separate the two components via distillation.
2.1.5 Efficiency
In order to obtain the column efficiency for both the batch and continuous distillation systems
should be performed at total reflux. The overall column efficiency is defined as: Where Nactual is
the actual number of trays in the column and Ntheoretical is the number of theoretical stages, i.e. the
number of trays that would be required to achieve the experimentally observed separation
2.2 Equilibrium Stage Concept
The equilibrium stage concept is the most important part of distillation since this is where the
most important assumptions are made. In the equilibrium stage the vapor-liquid is assumed in
every stage, the liquid is transported to the stages at the bottom and the vapor to the top stages.
The columns that have trays it is reasonable to describe the actual physics behind the columns,
but it is not used in packed columns. It is said that the calculations from the equilibrium stage
concept it works in all columns very well and even in packed columns. Consider a vapor and a
liquid that are in contact with each other as shown in Figure 2. Liquid molecules are continually
vaporizing, while vapor molecules are continually condensing. If two chemical species are
present, they will generally condense and vaporize at different rates. When not at equilibrium,
the liquid and the vapor can be at different pressures and temperatures and be present in
different mole fractions. At equilibrium the temperatures, pressures, and fractions of the two
phases cease to change. Although molecules continue to evaporate and condense, the rate at
which each species condenses is equal to the rate at which it evaporates. Although on a
molecular scale nothing has stopped, on the macroscopic scale, where we usually observe
processes, there are no further changes in temperature, pressure, or composition.
Daltons law of partial pressures: P=PA
That is the total pressure is equal to the summation of the partial pressures. Since in an ideal
gas or vapor the partial pressure is proportional to the mole fraction of the constituent, then

PA=y A .P for an ideal mixture, the partial pressure is related to the concentration in the liquid
phase by
Raoults law which may be written as: PA=PA0 . xA

Figure 2 Equilibrium Liquid-Vapor interaction

Consider a vapor and a liquid that are in contact with each other as shown in Figure 2. Liquid
molecules are continually vaporizing, while vapor molecules are continually condensing. If two
chemical species are present, they will generally condense and vaporize at different rates.
When not at equilibrium, the liquid and the vapor can be at different pressures and temperatures
and be present in different mole fractions. At equilibrium the temperatures, pressures, and
fractions of the two phases cease to change. Although molecules continue to evaporate and
condense, the rate at which each species condenses is equal to the rate at which it evaporates.
Although on a molecular scale nothing has stopped, on the macroscopic scale, where we
usually observe processes, there are no further changes in temperature, pressure, or
composition.
Daltons law of partial pressures: P=PA
That is the total pressure is equal to the summation of the partial pressures. Since in an ideal
gas or vapor the partial pressure is proportional to the mole fraction of the constituent, then
PA=y A .P for an ideal mixture, the partial pressure is related to the concentration in the liquid
phase by
Raoults law which may be written as: PA=PA0 . x A
Where PA0 is the vapor pressure of pure A at the same temperature. This relation is usually
found to be true only for high values of xA, or correspondingly low values of xB, although
mixtures of organic isomers and some hydrocarbons follow the law closely. For low values of xA,
a linear relation between PA and xA again exists, although the proportionality factor is Henrys
constant H, and not the vapour pressure PA0 of the pure material. For a liquid solute A in a
solvent liquid B,
Henrys law takes the form: PA=H.X A (Backhurst et al., 2002)

2.3 McGabe Thiele Theory

For a binary system, the classic McCabe-Thiele graphical technique can be used to design the
distillation column and to explore the effect of process variables. Although it is quite simple to
use, this simplicity comes with a price. The technique uses a number of assumptions
concerning the operation of the distillation column. It is important to analyze whether these
assumptions are reasonable for the batch distillation unit being used. To use the McCabe-Thiele
analysis, one needs the vapor-liquid equilibrium for the system plotted as a y versus x diagram.
The second part is the operating line for the column which is a formulation of the mass balance
from stage to stage; this requires the overall gas and liquid flows and the selected reflux ratio.
When the distillation is continuous and feed enters the middle of the column, there are separate
operating lines (mass balances) for the column above and below the point of feed introduction.
For batch distillation, there is only one operating line since the molar flows of gas and liquid are
constant throughout the column. The number of stages is determined by moving from
equilibrium to operating curve such as occurs in the column. This generates a step structure
which gives the number of stages. While the method is simple to do in practice, it takes some
analysis to understand the concepts.
Upon inspection of Figure 2 Above the number of trays and the feed tray can easily be
determined by using this method if all compositions are known around the distillation column.
Once all the required values are known the stages can be determined Values needed: XF, q, XD,
XB, and RD (calculated with balances around column)
1. Plot the equilibrium curve.
2. Calculate the slope q/(q-1) of the feed line.
3. Plot the feed line using X=XF and the slope.
4. Calculate the y-intercept of the rectifying line XD/ (RD+1).
5. Plot the rectifying line using (Xd,Xd) and the intercept.
6. Draw the stripping line connecting the intersection of the rectifying and feed lines and
the point (xb, xb).
7. Correct for stage efficiency by drawing the "effective" equilibrium curve between the
equilibrium curve and the operating lines.
8. "Step off" equilibrium stages. (McCabe & Smith, 1976)

2.4 Distillation Methods

2.4.1 Flash Distillation/Equilibrium
This is type of distillation that occurs in a single-stage in which a liquid mixture is partially
vaporized. The vapor is allowed to come to equilibrium with the residual liquid and the resulting
vapor and liquid phases are separated and removed from the apparatus.

2.4.2 Batch Distillation

A Feed is charged to a heated kettle .The liquid charge is boiled slowly and the vapor s are
withdrawn as rapidly as possible to a condenser, where the condensed vapor (distillate) is
collected. The first portion of vapor condensed is richest in the more volatile component. As
vaporization proceeds, the vaporized product becomes leaner in the more volatile component
2.4.3 Fractional Distillation
Fractional distillation is essentially the same as simple batch distillation except that a
fractionating column is placed between the boiling flask and the condenser. The fractionating
column is usually filled with packing or on larger scale like the petroleum industry it will have
trays and bubble caps. Fractional distillation results in better separation between different
compounds due to packing or "theoretical plates" on which the refluxing liquid can condense, reevaporate, and condense again, essentially distilling the compounds over and over. The more
volatile liquids will tend to push towards the top of the fractionating column, while lower boiling
liquids will stay towards the bottom, giving a better separation between the liquids.
2.4.4 Steam Distillation
When a mixture of two practically immiscible liquids is heated while being agitated to expose the
surface of one liquid to the vapor phase, each constituent independently exerts its own vapor
pressure as a function of temperature as if the other constituent were not present.
Consequently, the vapor pressure of the whole system increases. Boiling begins when the sum
of the partial pressures of the two immiscible liquids just exceeds the atmospheric pressure. In
this way, many organic compounds insoluble in water can be purified at a temperature well
below the point at which decomposition occurs
2.4.5 Vacuum Distillation
Vacuum distillation is distillation at a reduced pressure. Since the boiling point of a compound is
lower at a lower external pressure, the compound will not have to be heated to as high a
temperature in order for it to boil. Vacuum distillation is used to distill compounds that have a
high boiling point or any compound which might undergo decomposition on heating at
atmospheric pressure. The vacuum is provided either by a water aspirator or by a mechanical
pump.
2.4.5 Azeotropic Distillation
A process by which a liquid mixture is separated into pure components with the help of an
additional substance or solvent.
2.5 Distillation Column Types
2.5.1 Batch Column
In batch operation, the feed to the column is introduced in batches. 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 with the remainder of feed removed from the
column.
2.5.2 Continuous Column

Continuous columns process a continuous feed stream. No interruptions occur unless there is a
problem with the column or surrounding process units. They are capable of handling high
throughputs and are the more common of the two types.

2.6 Distillation Tray Types

2.6.1 Bubble Cap Trays
A bubble cap tray has 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 vapor.
Vapor 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
2.6.2 Valve Trays
In valve trays, perforations are covered by lift able caps. Vapor flows lifts the caps, thus selfcreating a flow area for the passage of vapor. The lifting cap directs the vapor to flow
horizontally into the liquid, thus providing better mixing than is possible in sieve trays
2.6.3 Sieve Trays
Sieve trays are simply metal plates with holes in them. Vapor passes straight upward through
the liquid on the plate. The arrangement, number and size of the holes are design parameters
Because of their efficiency, wide operating range, ease of maintenance and cost factors, sieve
and valve trays have replaced the once highly thought of bubble cap trays in many
applications(McCabe & Smith, 1976)
3. Methodology
3.1 Apparatus

Refract meter
Stopwatch
Measuring cylinder
Continuous Distillation Unit ( Figure 4)

Figure 4: Computer Controlled Continuous Distillation Unit

3.2 Procedure

The mixture of 50/50% ethanol and water was already present in the reboiler at the
bottom of the distillation column. The volume was checked and ensured to be enough
The tap of the cooling water was then opened.
The heating element was then switched on and it was set to the value higher than the
boiling point temperature of the most volatile component and lower than the temperature
of the least volatile component as the set point.
The system was left to reach steady state and produce a steady flow of distillate.

The temperatures of the cooling water in the inlet and outlet as well as the flow rate and
reflux time was then recorded.
The valve that allows the flow of the distillate back to the column was then closed and
the time it takes to fill 50ml of the tank was then recorded.
The distillate and bottoms was collected and measured with the refract meter to
determine its composition.
The system was shut down after the necessary values and measurements were
recorded.
The recorded values was processed and calculation was performed for the distillation
column, from the results conclusions were drawn.

Variables
Coolant In
Coolant out
Coolant flow rate

Values
13.5
14.6
0.31

Units
C
C
l/min

Volume Distillate
Distillate Time

300
1236

ml
s

Volumetric Fraction Bottoms

Volumetric Fraction Distillate
Pressure

32.3
74.9
-0.03

%
%
bar

Table 2: Calculated Values

Calculated variables Value units
Composition of ethanol in distillate (XD)
Composition of ethanol ii bottoms (Xw)
Moles of ethanol in distillate
Mole s of ethanol in bottoms
Composition of water in the distillate
Composition of water in the bottom
Moles of water in distillate
Moles of water in bottom
Reflux ratio
Heat gained by coolant
Heat lost by distillate
Heat lost from system

0.47
0.13
0.12
0.54
0.53
0.87
1.39
3.76
1
239.1
726.4
487.3

/
/
Mol
Mol
/
/
Mol
Mol
mol/mol
J/s
J/s
J/s

Figure 4: Vapor-liquid in equilibrium curve of water and ethanol__

2
4

5
6

XW

XD

5. Discussion
The objective of the practical was to determine the number of theoretical plates in the column
and perform an energy balance around the condenser. To start with looking at the number of
theoretical plates that were determined in this practical shown in figure 4 that 2 theoretical
plates were calculated this value does not corresponds to the number of actual plates the
column has, which is 8 plates.
Normal in theory more actual plates are always required than that of the theoretical plates. That
might be due to physical plates not being 100% efficient at equilibrium phase and that should
always be kept in mind when planning or designing a distillation column unit. Concerning the
energy balance calculation it was calculated that the total energy lost was about 486.3 J/s which
makes sense since the condenser was not insulated as insulation would have defeated the aim

of the condenser, as which is to remove energy in a form of heat from the distillate to condense
it. It can also be seen that more heat was given off by the distillate 725.4 J/s due to the heat lost
to the atmosphere, than the amount of heat gained by the coolant 238.1 J/s in the column.
That indicated that the heat that was lost to the environment which is useful to the condenser as
it helps and used for cooling , as well as the column as this contributed to a decrease in column
efficiency and heat losses which works against the distillation process When looking at column
efficiency, it was calculated the this distillation column had an efficiency of around 76.5% which
is considerably to low and a bad overall efficiency for ethanol distillation as it resulted in a low
estimation of the number of plates estimated using the Vapor-liquid equilibrium curve, more over
considering the mole fraction that were obtained it can obviously be seen that the fraction of the
lighter key which is ethanol is dominant in the distillate process which indicate that the
distillation was successful in separating the ethanol from the water but determining the
theoretical number of plates was not a success.
6. Conclusion
The experimentation was carried out successfully and the theory behind of distillation, the
theoretical plates and the flow of energy was understood. The number of theoretical plates
determined and to have value of 7, compared to the amount of actual plates the value obtained
makes sense taking into consideration the column efficiency The energy balance was carried
out and it was noticed that energy was in fact gained by the water almost double the amount
was lost by the distillate which means that the process is exothermic and heat was given off by
the distillate to the coolant and the surroundings. Recommendations: although time is of the
essence in practicals it would be easier if the whole process, from start to finish, was carried out
by the students to eliminate misconceptions and the need for assumptions after the practical.
Especially have the students prepare the ethanol water mixture instead having it in the column
on arrival.

7. References

Backhurst, J., Harker, J., Richardson, J. & Coulson, J. 2002. Coulson & Richardson's
chemical engineering, J.M. Coulson and J.F. Richardson. Oxford: ButterworthHeinemann.
Cheremisinoff, N. 2000. Handbook of chemical processing equipment. Boston:
Butterworth-Heinemann.

McCabe, W. & Smith, J. 1976. Unit operations of chemical engineering. New York:
McGraw-Hill.