TITLE PAGE

TITLE OF EXPERIMENT: STEADY STATE DISTILLATION OF A

BINARY MIXTURE
AIM OF EXPERIMENT:
 TO DEMONSTRATE THE EFFECT OF RECYCLE ON THE TOTAL
MASS FLOW RATE OF A SYSTEM

DATE OF EXPERIMENT: 20th September, 2021

DATE OF SUBMISSION: 27th September, 2021
NAME: EMONBEIFO EFOSA ENOCH
MATRICULATION NUMBER: ENG1708883
SERIAL NUMBER: 029
GROUP NUMBER: A3
EXPERIMENT NUMBER: 05
LEVEL: 400LEVEL
COURSE CODE: CHE401
INSTRUCTOR’S NAME: MR. AGBONGHILE COLLINS

i
 TABLE OF CONTENTS

TITLE PAGE.......................................................................................................i
TABLE OF CONTENTS...................................................................................ii
LIST OF TABLES, EQUATIONS, FIGURES AND GRAPHS....................iv
LIST OF TABLES.........................................................................................iv
LIST OF FIGURES.......................................................................................iv
ABSTRACT/SUMMARY..................................................................................v
CHAPTER ONE.................................................................................................1
1.1 INTRODUCTION....................................................................................1
1.1.1 METHODS OF DISTILLATION OF BINARY MIXTURES..............2
1.1.2 CLASSIFICATION OF DISTILLATION..............................................3
1.1.3 APPLICATIONS OF DISTILLATION..................................................7
1.2.1 NUMBER OF PLATES REQUIRED IN A DISTILLATION
COLUMN............................................................................................................8
PLATE EFFICIENCY.....................................................................................12
1.2.1 THE FRACTIONATING PROCESSES:..........................................12
CHAPTER TWO..........................................................................................15
2.1 DESCRIPTION OF APPARATUS.......................................................15
2.2 EXPERIMENTAL PROCEDURE.......................................................19
CHAPTER THREE..........................................................................................20
3.1 EXPERIMENT READINGS AND RESULTS....................................20
3.1.1 CALCULATIONS:..............................................................................21
Component balance on Ethanol;.....................................................................21
Top operating line equation:............................................................................21
Using Lewis-Sorel method...............................................................................22
Efficiency...........................................................................................................23
3.1.2 GRAPH.....................................................................................................24
3.2 DISCUSSION..............................................................................................25
CHAPTER FOUR............................................................................................27
4.1 CONCLUSION AND RECOMMENDATION....................................27
ii
REFERENCES.................................................................................................28
APPENDIX........................................................................................................29

iii
LIST OF TABLES, EQUATIONS, FIGURES AND GRAPHS

LIST OF TABLES
Table 1: Data showing equilibrium curve points................................................20
Table 2: BRISK READING COMPARISON TABLE......................................20
Table 3: List of symbols and their meaning.......................................................29

LIST OF FIGURES
Figure 1: Flash distillation system........................................................................3
Figure 2: Batch distillation diagram.....................................................................4
Figure 3: Schematic of a trayed distillation column.............................................6
Figure 4: Material balance over a plate..............................................................10
Figure 5: Material balances at top and bottom of column..................................11
Figure 6: Continuous fractionating column with rectifying and stripping
sections...............................................................................................................14
Figure 7: Refractometer......................................................................................17
Figure 8: Beaker.................................................................................................17
Figure 9: Schematics for the UO3PCC continuous distillation column.............18
Figure 10: GRAPH OF LIQUID COMPOSITION AGAINST VAPOUR
COMPOSITION.................................................................................................24

iv
 ABSTRACT/SUMMARY
The Experiment, the Continuous Distillation Column was carried out to check
for the efficiency of a distillation column. This was done on a binary mixture of
Ethanol and water with the most volatile component as Ethanol.
The experiment was performed using the Armfield UOP3CC Distillation
column, with the power of the control panel set to 1KW for heating of the
mixture in the reboiler. The reflux ratio was set to 5:1 in other words, for every
6 moles of the condensate, 1 mole entered the top product receiver and 5 moles
returned back to the distillation column.
From the experiment the composition of ethanol in feed and distillates were
measured using the refractometer---which gives the refractive index of the
component of ethanol in terms of composition present in the ethanol—water
mixture whose value was referred to as the brisk readings. From interpolation
using the brisk reading table the percentage composition was gotten as 23.88%
in the feed and 78.2% in the distillate. The composition of ethanol in the feed
23.88% shows how extremely dilute ethanol was in the binary mixture.

In the course of the experiment, the feed was made to enter the column from the
middle. This was to get the best desired product. The volumetric flow-rates was
found to be 0.167 L/min, the distillate flow-rate was found to be 0.025 L/min
and the bottom product was found to be 0.142 L/min. The McCabe – Thiele
Equilibrium plot was drawn and the top and bottom operating lines were drawn.
The steps in determining the number of theoretical plates was drawn and this
was found to be 13 trays; with the actual number of trays as 4. From the plot,
we could see the point at which an azeotrope mixture was formed. To avoid
this, a desiccant is introduced to the rising vessel.

Efficiency was computed and found to be 50%. This implies that the heat
energy given off by the column (i.e Work) is more than the heat supplies to the
column. This result violate the law of conservation of energy since energy is
being created. Also, it could be that that the level of purity of our distilled
products was high.

It was safe to conclude from the values gotten that our column was over
efficient and as such, the heat supplied to the column must be double checked
so the column does not over work itself.

v
vi
 CHAPTER ONE
1.1 INTRODUCTION

The separation of liquid mixtures into their various components is one of the
major operations in the process industries, and distillation, the most widely used
method of achieving this end, is the key operation in any oil refinery. In
processing, the demand for purer products, coupled with the need for greater
efficiency, has promoted continued research into the techniques of distillation.
In engineering terms, distillation columns have to be designed with a larger
range in capacity than any other types of processing equipment, with single
columns 0.3–10 m in diameter and 3–75 m in height. Designers are required to
achieve the desired product quality at minimum cost and also to provide
constant purity of product even though there may be variations in feed
composition. A distillation unit should be considered together with its
associated control system, and it is often operated in association with several
other separate units. The vertical cylindrical column provides, in a compact
form and with the minimum of ground requirements, a large number of separate
stages of vaporization and condensation.
In process industries the basic problems of design are considered and it may be
seen that not only the physical and chemical properties, but also the fluid
dynamics inside the unit, determine the number of stages required and the
overall layout of the unit.

Distillation is a process of physically separating a mixture into two or more

products that have different boiling points, by partial vaporization of a liquid
mixture and/or by partial condensation of a gas mixture thereby rendering liquid
phase richer in less volatile (with higher boiling point) component and the
vapour phase is richer in more volatile (with lower boiling point) component.

Dry distillation is the heating of solid materials to produce gaseous products

(which may condense into liquids or solids). Dry distillation may involve
chemical changes such as destructive distillation or cracking and is not
discussed under this article. Distillation may result in essentially complete
separation (nearly pure components), or it may be a partial separation that
increases the concentration of selected components in the mixture. In either
case, the process exploits differences in the relative volatility of the mixture's
components. In industrial applications, distillation is a unit operation of
1
practically universal importance, but it is a physical separation process, not
a chemical reaction.
Continuous distillation is a form of distillation in which a mixture is
continuously (without interruption) fed into the process and separated fractions
are removed continuously as output streams. Having already established the
definition of distillation as the separation or partial separation of a liquid feed
mixture into components or fractions by selective boiling (or evaporation)
and condensation. The process produces at least two output fractions. These
fractions include at least one volatile distillate fraction, which has boiled and
been separately captured as a vapour condensed to a liquid, and practically
always a bottoms (or residuum) fraction, which is the least volatile residue that
has not been separately captured as a condensed vapour.

1.1.1 METHODS OF DISTILLATION OF BINARY MIXTURES.

 Differential distillation: The simplest example of batch distillation is a
single stage, differential distillation, starting with a still pot, initially full,
heated at a constant rate. In this process the vapor formed on boiling the
liquid is removed at once from the system. Since this vapor is richer in
the more volatile component than the liquid, it follows that the liquid
remaining becomes steadily weaker in this component, with the result
that the composition of the product progressively alters. Thus, whilst the
vapor formed over a short period is in equilibrium with the liquid, the
total vapor formed is not in equilibrium with the residual liquid. At the
end of the process the liquid which has not been vaporized is removed as
the bottom product. The analysis of this process was first proposed by
RAYLEIGH.
 Flash or equilibrium distillation: Flash or equilibrium distillation,
frequently carried out as a continuous process, consists of vaporizing a
definite fraction of the liquid feed in such a way that the vapor evolved is
in equilibrium with the residual liquid. The feed is usually pumped
through a fired heater and enters the still through a valve where the
pressure is reduced. The still is essentially a separator in which the liquid
and vapor produced by the reduction in pressure have sufficient time to
reach equilibrium. The vapor is removed from the top of the separator
and is then usually condensed, while the liquid leaves from the bottom.

2
 Figure 1: Flash distillation system.

F = L + V ……………. (1)
Fzi = Lxi + Vyi ……….. (2)

 Rectification: In the two processes considered above, the vapor leaving

the still at any time is in equilibrium with the liquid remaining, and
normally there will be only a small increase in concentration of the more
volatile component. The essential merit of rectification is that it enables a
vapour to be obtained that is substantially richer in the more volatile
component than is the liquid left in the still. This is achieved by an
arrangement known as a fractionating column which enables successive
vaporization and condensation to be accomplished in one unit.

Of these, rectification is much the most important, and it differs from the
other methods in that part of the vapor is condensed and returned as liquid to
the still, whereas, in the other methods, all the vapor is either removed as
such, or is condensed as product. For the sake of this report our focus is
mainly on rectification.

1.1.2 CLASSIFICATION OF DISTILLATION

1. Batch distillation: Batch distillation is commonly used when a
continuous process is not practicable owing to process restrictions, the
requirement to distil other process streams, or the low frequency of usage
of distillation does not merit a unit dedicated entirely to a single product.
Batch distillation in a pot or tank can provide a somewhat efficient
separation of two or more components. Despite the fact that the purity of

3
 the distilled product fluctuates during batch distillation, it is nevertheless
used in industry.

Figure 2: Batch distillation diagram.

A feed is initially fed to a tank, and the vapour created by boiling the
liquid is removed and passed through a condenser, as illustrated in Fig. 2.
The distillate, D, has a composition of xD, while the liquid left in the pot,
W, has a composition of xW. The following are the total and
componential material balances surrounding a batch distillation unit:

F = W + D………………….. (3)
FxF= WxW + DxD…….… (4)

Note that W, xW, D and xD all vary throughout the distillation.

2. Continuous distillation with reflux: Operation and equipment

Continuous distillation is nearly always more cost-effective than batch
distillation for large-scale operations, especially when a consistent supply
of feed is available. One of the drawbacks of both batch and flash
distillation is the numerous consecutive distillations required to
accomplish something resembling "complete" separation of the
components. 13 Batch distillation also allows for the production of an
extremely pure product. However, the liquid residue must be redistilled
many times in order to get a high recovery. A continuous distillation
column is similar to a succession of tiny flash units in that it eliminates
the need for numerous units. Indeed, a product stream of any required
purity can potentially be produced unless a combination contains an
4
 azeotrope. In actuality, in order to get a 100 percent pure product, a large
number of trays or a very high reflux ratio would be necessary; these
physical restrictions on the system design limit the actual recovery
feasible.For the subsequent discussion regarding continuous distillation, a
binary (2-component) feed will be assumed. In the case of a binary feed,
the more volatile (lower boiling) component will be referred to as the
light component, whereas the less volatile (higher boiling) component is
referred to as the heavy component. As is standard practice in binary
distillation, all mole fractions (i.e., xD, xB, xF) will be representative of
the light component only.
3. Reflux and Boil-up: The reflux ratio, R, is defined as the molar flow
ratio of reflux returned to collected distillate product. The rising vapor
gradually removes the light element from the liquid/reflux stream as it
falls. The vapor stream tends to evaporate the low-boiling ingredient from
the liquid, while the liquid stream prefers to condense the heavy element
from the vapor as a consequence of both heat and mass transfer
processes. The heavy component of this liquid stream progressively
increases from the top tray to the bottom of the column. The liquid is then
collected at the bottom of the column by a pump, transported to a
reboiler, where it is partially vaporized (steam is generally used as the
heating medium), and then returned to the column to produce a rising
vapor stream in the area of the column below the feed plate. The boil-up
refers to the vapor produced by the reboiler. As the bottoms product, the
remaining reboiler liquid is removed. The boil-up ratio, RB, is defined as
the molar flow ratio of vapor created by the reboiler to the bottoms
product, similar to the reflux ratio.

5
 Figure 3: Schematic of a trayed distillation column

The following are some popular distillation terms:

1. Reflux: This is the liquid that is returned to the column after the above
product has been condensed. It is usually done in order to improve the
purity of the overhead product.
2. Rectification: This is a distillation application that involves fractionating
crude oil into its constituents. As the vapour stream travels through the
column and comes into touch with the reflux, it gets enriched.
3. Overhead: This is the product that exits the column from the condenser
after the reflux has been returned to it. Usually, the desired product or
fractions are involved. It's also known as distillate, and it's denoted by
the letter D and the percentage xD.
4. Bottom: here is the product that has passed through the reboiler and is
leaving the column. It's also known as the trash stream since it's where
products that can't be separated further by the distillation column exit. It
contains a large amount of the less volatile component (s). The letter W
and the fraction xW are used to symbolize it.
5. Vapor- liquid equilibrium: distillation columns are designed based on
the boiling points of the component in the mixture to be separated. Thus
the height of the column are designed with the VLE in mind as from
these the theoretical tray number and size can be estimated.
6
1.1.3 APPLICATIONS OF DISTILLATION

- Distillation of fermented foodstuffs yields high-alcohol distilled drinks or

isolates other commercially valuable fermentation products.
- Distillation is a reliable and time-honoured method of desalination.
- Oil stabilization is a type of partial distillation used in the petroleum
industry to lower the vapour pressure of crude oil, making it safer to store
and transport while also lowering volatile hydrocarbon emissions into the
atmosphere. Fractional distillation is a common operation in oil refineries'
midstream operations for converting crude oil into fuels and chemical
feedstock’s.
- For industrial application, cryogenic distillation separates air into its
constituents, most notably oxygen, nitrogen, and argon.
- Large volumes of crude liquid products of chemical synthesis are distilled
in the chemical industry to separate them from other products,
contaminants, or unreacted starting ingredients.

7
1.2 THEORY
When mixtures (mostly in liquid form) must be separated, distillation columns
are utilized throughout industry. The petroleum business is one such example.
Crude oil is fed into a huge distillation column, and various fractions (oil mixes
of varied composition and volatility) are extracted at different heights in the
column in this application. Each fraction, such as jet fuel, home heating oil,
gasoline, and so on, is utilized in a number of ways by both industry and
consumers. The relative volatilities of the components to be separated, the
number of contacting trays (plates) or packing height, and the ratio of liquid and
vapour flow rates all have a role in the separation accomplished in a distillation
column.
This section explains the theoretical background of the fractionating column,
which serves as the foundation for the distillation process, which allows for
consecutive vaporization and condensation in one unit, as mentioned before
under rectification.

1.2.1 NUMBER OF PLATES REQUIRED IN A DISTILLATION

COLUMN
The transmission of heat and material across a plate involves four streams, as
illustrated in the diagram below, where plate n receives liquid Ln+1 from plate
n+1 above and vapor Vn-1 from plate n-1 below. Plate n-1 receives liquid Ln
from Plate n, whereas Plate n+1 receives vapor Vn from Plate n. The plate's
function is to mix the vapor Vn so that it can reach plate n+1. The plate's action
is to cause mixing so that the vapor Vn, of composition yn, approaches
equilibrium with the liquid Ln, of composition xn. The streams Ln+1 and Vn-1
cannot be in equilibrium, and some of the more volatile component is vaporized
from the liquid Ln+1 during the interchange process on the plate, decreasing its
concentration to xn and some of the less volatile component is condensed from
Vn-1, increasing the vapour concentration to yn.
There two basic method of determining the number of plates required:

 Lewis-Sorel Method

 McCabe and Thiele Method

8
When performing theoretical calculations, it is assumed the system is ideal.
Among this assumption, the system has the following characteristics:

- Column is operating in steady state

- Constant molar overflow
- Column is insulated with minimal heat loss.
- Column pressure is uniform.
- All vapour and liquids are saturated
- Heats of vaporization are equal.
Mathematical Expression for the Top operating Line and Bottom operating
line equation are shown below;

Thus;

9
 Figure 4: Material balance over a plate.

Heat balance over a plate

A heat balance across plate n may be written as:

Ln+1HLn+1+ Vn−1HVn−1= VnHVn+ LnHLn+ losses + heat of mixing

where: HLn is the enthalpy per mole of the liquid on plate n, and
HVn is the enthalpy per mole of the vapour rising from plate n.
This equation is difficult to handle for the majority of mixtures, and some
simplifying assumptions are usually made. Thus, with good lagging, the heat
losses will be small and may be neglected, and for an ideal system the heat of
mixing is zero. For such mixtures, the molar heat of vaporisation may be taken
as constant and independent of the composition. Thus, one mole of vapour Vn−1
on condensing releases sufficient heat to liberate one mole of vapour Vn. It
follows that Vn = Vn−1, so that the molar vapour flow is constant up the column
unless material enters or is withdrawn from the section. The temperature change
from one plate to the next will be small, and HLn may be taken as equal to
HLn+1.
Applying these simplifications to equation above, it is seen that Ln = Ln+1,
so that the moles of liquid reflux are also constant in this section of the column.
Thus, Vn and Ln are constant over the rectifying section, and Vm and Lm are
constant over the stripping section. For these conditions there are two basic
methods for determining the number of plates
required. The first is due to SOREL and later modified by LEWIS, and the
second is due to MCCABE and THIELE. The Lewis method is used here for
binary systems, and also for calculations involving multicomponent mixtures.

10
This method is also the basis of modern computerized methods. The McCabe–
Thiele method is particularly important since it introduces the idea of the
operating line which is an important common concept in multistage operations.
The best assessment of these methods and their various applications is given by
UNDERWOOD.
When the molar heat of vaporization varies appreciably and the heat of mixing
is
no longer negligible, these methods have to be modified, and alternative
techniques are to be used.

Calculation of number of plates using the Lewis–Sorel method

If a unit operation is setup so that a binary feed F is distilled to give a top
product D and a bottom product W with x F, xD and xw as the corresponding mole
fractions of the more volatile component, 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 the plate n is;
Vn=Ln+1 + D
Similarly, taking a material balance for the total streams and for the more
volatile component from the bottom to the above plate m gives:
L m = Vm + W
Ymvm = Lmxm+1 - Wxw
Lm x m +1 Wx w
Ym = Vm
- V
m

Where ym is the mole fraction of the bottom product.

11
 Figure 5: Material balances at top and bottom of column

McCabe-Thiele method:
The McCabe-Thiele method is considered to be the simplest and perhaps the
most instructive method for analysis of binary distillation. It uses the fact that
the composition at each theoretical tray is completely determined by the mole
fraction of one of the components and assumes a complete molar overflow
which requires that:
The molar heats of vaporization of the feed components are equal
For every mole of liquid vaporized there is a mole of vapor that is condensed
Heat effects such as heats of solution are negligible
The method was first published by Warren McCabe and Ernest Thiele in 1925
who were both working in the Massachusetts institute of technology (MIT) at
the time. It requires the Vapor-liquid equilibrium graph.

PLATE EFFICIENCY
The number of ideal stages required for a desired separation may be calculated
by one of the methods discussed previously, although in practice more trays are
required than ideal stages. The ratio n/np of the number of ideal stages n to the
number of actual trays np represents the overall efficiency E of the column,
which may be 30–100 percent. The main reason for loss in efficiency is that the
kinetics for the rate of approach to equilibrium, and the flow pattern on the
plate, may not permit an equilibrium between the vapor and liquid to be
attained.
To calculate the efficiency:
number of theoretical plates
n= ×100
number of experimental plates
N
n= × 100
NR

12
1.2.1 THE FRACTIONATING PROCESSES:
The column is made up of a cylindrical structure that is split into parts by a
series of ventilated trays that allow vapour to move upward. The liquid reflux
travels over each tray, over a weir, and into the tray below through a down
comer. The vapour rising from the top tray goes via a condenser, an
accumulator or reflux drum, and a reflux divider, where some of it is extracted
as overhead product D and the rest is returned to the top tray as reflux R.
The liquid in the column's base is typically heated, either by condensing steam
or a hot oil stream, and the vapour rises to the bottom tray through the
perforations.
The liquid from the still enters the external reboiler, runs over the tubes and
weir, and exits as the bottom product via a bottom's cooler, which preheats the
incoming feed. The reboiler vapour is returned to the bottom of the column with
a composition ys and enters the bottom tray, where it is partly condensed and
then revaporized to provide vapour of composition y1. On each tray, the partial
condensation of rising vapour and partial vaporization of the reflux liquid is
repeated. The top product is made from the condensation of composition yt
from the top tray. Both the D and the R have the same yt makeup. The feed
stream is placed into an intermediary tray with a liquid that is almost identical to
the feed. The rectifying section of the column is located above the feed point,
while the stripping section is located below it. In an ideal tray, the vapour rising
from the tray will be in equilibrium with the liquid leaving, however in
actuality, there will be a lesser degree of enrichment.
When looking at the operation on each tray, keep in mind that the vapour
ascending to it and the reflux pouring down to it are not in balance, thus
appropriate mass and heat transfer rates are required for the proper functioning
of the tray. The tray as described is known as a sieve tray and it has perforations
of up to about 12 mm diameter, although there are several alternative
arrangements for promoting mass transfer on the tray, such as valve units,
bubble caps and other devices.
In all cases the aim is to promote good mixing of vapor and liquid with a low
drop in pressure across the tray.
On each tray the system tends to reach equilibrium because:
(a) Some of the less volatile component condenses from the rising vapor into
the liquid thus increasing the concentration of the more volatile component
(MVC) in the vapor.

13
(b) Some of the MVC is vaporized from the liquid on the tray thus decreasing
the concentration of the MVC in the liquid.

Figure 6: Continuous fractionating column with rectifying and stripping sections

14
 CHAPTER TWO
2.1 DESCRIPTION OF APPARATUS
Below are the apparatus and equipment used to carry out this experiment.
 CONTINOUS DISTILLATION COLUMN:

The UOP3CCContinuous Distillation Column is a self-contained distillation

system made up of two linked units: a floor-standing process unit and a 30
bench-mounted control panel. The distillation column is supported by a welded
tubular steel framework (1) with four adjustable feet that stands on the floor (2).

15
The structure is intended to allow the unit to be moved into place using a
forklift or pallet truck at first.
The sieve plate column has a diameter of 50mm and is made up of two glass
sections (3) and (4), each with four sieve plates. A central feed portion separates
the columns, which are positioned vertically for counter-current vapor/liquid
flow. The column is insulated to keep out the cold and minimize heat loss.
Pump (7) pumps feed mixture from any of the feed tanks to the base, middle, or
top of the distillation column, respectively, at connections (A), (B), or (C). A
length of Viton rubber tubing is included with the feed pump. All of the
approved test mixes (see "Operational Procedures") can be used with this
tubing. The appropriateness of this substance must be evaluated when additional
test combinations are employed.
A loosely packed column is delivered. When demonstrating the features of a
packed column, this column might be used in place of the sieve plate column.
The reboiler (13) at the bottom of the column is made of 316 stainless steel and
has a flameproof immersion type heating element. This reboiler may be used for
either batch or continuous distillation.
Vapor from the top of the column is directed to a water-cooled, coil-in-shell
condenser (8), which may be equipped with an insulated jacket to allow for heat
balancing. (For regular operation, the insulated jacket should not be attached to
the condenser.) A pressure relief valve (PRV1) is included into the condenser
shell to safeguard the system in the case of a blocked vent and cooling water
failure. A variable area flowmeter (FI1) regulates the flowrate of cooling water
into the condenser, which is controlled by a diaphragm valve (V5). When
operation at lower pressure is necessary, a cooling water supply is attached to
the input nozzle (19) and also serves to drive the vacuum pump (20). The
vacuum pump's water supply is regulated by valve (V14), which can only be
turned on when valve (V5) is open.
The system's temperatures are monitored by fourteen thermocouple sensors (T1
to T14), which are strategically placed throughout the system. The temperature
of the liquid on each sieve plate is measured by T1 to T8 in the column. There
are seventeen temperature sensor sites, three of which do not have sensors
installed but may be equipped with sensors relocated from less relevant places if
necessary.
The total pressure drop across the column is measured using a U-tube
manometer (P1) and isolating valves (V6) in the column (V7).

16
  A REFRACTROMETER:
Standard refractometers measure the extent of light refraction (as part of a
refractive index) of transparent substances in either a liquid or solid-state; this is
then used in order to identify a liquid sample, analyze the sample's purity, and
determine the amount or concentration of dissolved substances within the
sample. As light passes through the liquid from the air it will slow down and
create a ‘bending’ illusion, the severity of the ‘bend’ will depend on the amount
of substance dissolved in the liquid. For example, the amount of sugar in a glass
of water.

Figure 7: Refractometer

 Beaker: are made up of tempered glass and have wide mouth for pouring
the solutions easily a beaker is a simple container, which is used for
heating and stirring

Figure 8: Beaker

17
\

18
Figure 9: Schematics for the UO3PCC continuous distillation column

19
2.2 EXPERIMENTAL PROCEDURE
The following procedure was carried out during the performance of the
experiments.
 The controller for the cooling water valve was turned on.
 Water was poured into the reboiler until the power source's indication
turned green.
 The electricity to the control panel was turned on, and the cooling water
inlet valve was opened and set at 3000ml/min.
 T9 was selected on the temperature selector (the temperature in the
reboiler)
 The reboiler was filled with about 1.59 litres of feed to ensure that the
process ran smoothly, and the power controller was set to 1Kw. The
reboiler's contents will be watched as they heat up.
 The feed tank was opened to let the feed stream at T5 after the vapour
rose up to the column.
 The reflux ratio was adjusted at 5:1 before turning on the reflux switch,
meaning 5 would return to the column and 1 would pass to the top
product column. Once the reflux valve is turned on, a click sound will be
heard to signal that it is working.
 The process was permitted to continue for as long as it took to recover
enough ethanol.
 Since the component of the feed stream is known, a sample from the top
product stream was obtained for testing and utilized to determine the
component of the bottom product.

20
 CHAPTER THREE
3.1 EXPERIMENT READINGS AND RESULTS

Table 1: Data showing equilibrium curve points

xi 0.0035 0.0175 0.0585 0.0935 0.2125 0.3615 0.4985 0.64 0.723 0.837 0.88 0.9489 0.9825
6 8
yi 0.0175 0.13150 0.305 0.411 0.5455 0.6060 0.6555 0.72 0.776 0.852 0.89 0.9502 0.9835
9 3

The Equilibrium graphs was drawn. For easy plot, the x i and yi values were
approximated to 2.dp on the graph.

Table 2: BRISK READING COMPARISON TABLE

Brisk 30 40 60 80 100 130 160 180 190

% alcohol 9.77 16.78 23.66 30.61 37.55 47.97 58.59 65.34 68.81

Given;
From the experiment
Volume of feed, F = 10 L
Volume of distillate, D = 1.52 L
Concentration of feed, Xf = 0.2388
Concentration of distillate, Xd = 0.7812
Reflux Ratio = 5:1

21
3.1.1 CALCULATIONS:
Converting the volume of feed and distillate to volumetric flow rates, we divide
both values by time (60mins)
 Volumetric flow rate of feed =
10
=0.167 L/min
60

 Volumetric flow rate of distillate =

1.52
=0.025 L /min
60

Thus;
Performing the over balance on the column;
F=D+W
0.167=0.025+W
W =0.167−0.025
W =0.142 L /mins
Assuming the percentage provided are by volume;

Component balance on Ethanol;

FX f = DX d + WX w
0.167 (0.2388) = 0.025 (0.782) + X w (0.142 )
0.0398 = 0.0196 + 0.142 X w
0.0398−0.0196
0.142
X w = 0.142

Top operating line equation:

ln D
yn= Vn ( Xn+1 ) + Vn Xd

L= RD
V= D(R+1)
RD D
yn= D ( R+1 ) ( Xn+ 1 )+ D ( R+1 ) Xd

22
 R Xd
yn= R +1 ( Xn+1 ) + R +1

Since reflux ration is 5:1

5 0.782
yn= 5+1 ( Xn+1 ) + 5+1 = 0.833Xn + 0.1303

yn = 0.833Xn + 0.1303 ………. (i)

Bottom operating line equation:

Lm W
ym= Vm ( Xm+1 )− Vm Xw

Lm = Ln+F = RD+F = (5*1520) + 10000= 17600

Lm = 17600
Lm= Vm+W
Lm-W= Vm
Vm= 17600 - 8480= 9120
Vm= 7920
17600 8480
ym= 7920
( Xm+ 1 )−
7920
(0.142)

ym= 1.8434 ( Xm +1 )−0.152

ym= 1.8434 Xm +1.6914 ……… (ii)

Using Lewis-Sorel method

Top plate is found from the equilibrium curve and, since it
is in equilibrium with vapour of composition,
Yt = 0.782, Xt = 0.74.
We substitute the value of Xt into eqn (i):
yt−1 = (0.833 × 0.74) + 0.1303 = 0.75
23
xt−1 is obtained from the equilibrium curve as 0.7
yt−2 = (0.75 × 0.7) + 0.1303 = 0.7134
xt−2 from equilibrium curve = 0.62
yt−3 = (0.75 × 0.62) + 0.1303 = 0.60
xt−3 from the equilibrium curve = 0.36
This last value of composition is sufficiently near to that of the feed for the feed
to be introduced on plate (t − 3). For the lower part of the column, the operating
line equation (ii) will be used.
Thus: yt−4 = (1.8434 × 0.36) − 0.075 = 0.58
xt−4 from the equilibrium curve = 0.29
yt−5 = (1.8434 × 0.29) − 0.075= 0.46
xt−5 from the equilibrium curve = 0.12
Since xt-5 (=0.12) is close to Xw (=0.0889). Therefore, theoretically, there will
be five (5) plates in the column.

Efficiency
Theoretical number of plates
Efficiency = X 100
Actual number of plates

Theoretical number of plates = 4

Actual number of plates = 8
4
Efficiency = 8 X 100 = 50%

Therefore, Efficiency = 50%

24
3.1.2 GRAPH

Figure 10: GRAPH OF LIQUID COMPOSITION AGAINST VAPOUR COMPOSITION

25
3.2 DISCUSSION
The goals of this experiment are to identify the number of theoretical plates
needed for experimental distillation and the efficiency of the continuous
distillation column, which are the experiment's experimental capabilities. The
continuous distillation column was used for this. The continuous distillation
column has been constructed in such a manner that it may be used to distil a
binary as well as a multicomponent combination. In this experiment, we're
interested in the binary mixture. We can accomplish partial separation or total
separation in distillation, with partial separation aiming to simply raise the
concentration of the product. The industrial distillation column is essentially a
series of units that perform both partial vaporization and partial condensation at
the same time.
The refractometer was used to determine the composition of ethanol in feed and
distillates, which gave the refractive index of the component of ethanol in terms
of composition present in the ethanol—water combination, whose value was
referred to as the brisk readings. The percentage composition was calculated as
23.88% in the feed and 78.2% in the distillate using interpolation and the brisk
reading table. The 23.88% ethanol content in the feed demonstrates how dilute
ethanol was in the binary combination. That is, 78.2% of the feed was made up
of water. The binary mixture is contained in a feed with an initial capacity of 10
litres. Even though the initial composition ratio of ethanol to water in the feed
was 23.88:78.2, the volume of the distillate was given as 1.52litres at the end of
the experiment. This indicates that the entire procedure was extremely efficient
and tolerable. As can be seen from the figures obtained following the rough
material balancing, the bottom product was 10 litres with a lower ethanol
content.
The experiment was conducted under steady state conditions, which meant that
no specialization in the column component fraction was expected, and a reflux
rate was specified. The continuous distillation column was powered by 1 kW
and had a 5:1 reflux ratio. 5moles of condensate were returned for every 6moles
of condensate at the top overhead, whereas 1mole went to the top product
receiver. The final readings reveal that the ethanol content in the top and bottom
products was 80 percent and 11.2 percent, respectively, indicating a reasonable
range of distillation capability.
The top and bottom line equations were obtained from the graph displayed
using the Lewis Sorel technique. The gas phase composition of the more
volatile component, ethanol, was plotted versus the liquid phase composition.
26
The graph demonstrates that the combination has some azeotropic properties.
The y x curve in the graph illustrates this situation, with the equilibrium curve
crossing the diagonal, indicating the presence of an azeotrope. Here, the issue of
non-ideality arises. Because the activity coefficient is larger than unity, a
positive departure from Raoult's rule exists, and the molecules of the system's
components resist one another other and exert a higher partial pressure than if
their behavior were ideal. This leads to the formation of a “minimum boiling”
azeotrope shown in the graph.
Considering the calculation, we can see that while stepping off plates down the
top operating line AB, the bottom operating line CE cannot be utilized until the
value of Xn on any plate is less than Xe. By the time Xn = Xb, you must have
passed to the bottom line CE. The optimal circumstances are when the least
amount of plates are utilized. The biggest steps in the enrichment section,
according to the geometry of the figure, occur down to the point of intersection
of the operating lines at x = xq. On the bottom working line, the steps are bigger
below this value of x. Although the column will function with a feed
composition between xe and xb, if xf = xq, the smallest number of plates will be
required. This is comparable to making xf equal to the composition of the liquid
on the feed plate for a binary mixture at its boiling point.
The theoretical number of plates is represented by the number of steps obtained
from the VLE curve. According to this experiment curve, the theoretical
number of plates in the distillation column is 4, as opposed to the actual number
of plates in the column, which is 8. (4 in the stripping the section and 4 the
rectification section).
The average effectiveness of the distillation was 50%, which is the ratio of the
theoretical plate to the actual plate multiplied by 100%. The major cause of
efficiency loss is that the kinetics for the pace of approach to equilibrium, as
well as the flow pattern on the plate, may not allow for a vapour-liquid
equilibrium to be achieved.

27
 CHAPTER FOUR
4.1 CONCLUSION AND RECOMMENDATION

Generally, the experiment yielded results that are consistent with the governing
theories. The continuous distillation column used in this experiment has an
average efficiency for complete separation, and it can be seen that the number
of stages required and the overall layout of the unit are determined not only by
physical and chemical properties, but also by fluid dynamics inside the unit. At
steady state distillation operation, the expected composition of the selected
component depends on the initial concentration in the feed, reflux ratio and the
efficiency of the column.
There are several recommendations that should be followed while conducting
this experiment in order to get more accurate data. Firstly, each time after
collecting the sample, immediately close the vial to prevent unnecessary
evaporation of ethanol. Secondly, it is recommended to use glove while
collecting the sample as the sample is still hot. Thirdly, each time to measure
the refractive index of the samples, clean the surface of refractometer using
distilled water. Lastly, for the following experiment after measuring the
refractive index of the sample, make sure to put the mixture back into the inlet
for reuse.

28
 REFERENCES
- Tham, M. T. (October, 1997). Basic Distillatrion Equipment and
Operation. Retrieved 28 March, 2018, from COSTELLO:
http://www.rccostello.com/distil/distileqp.htm Tham, M. T. (October,
1997).
- Column Internals. (I. R. C. Costello & Associates, Producer) Retrieved
28 March, 2018, from COSTELLO:
http://www.rccostello.com/distil/distilint.htm
- Coulson and Richardson’s CHEMICAL ENGINEERING VOLUME 2
FIFTH EDITION Particle Technology and Separation Processes
-  Himmelblau, David M. (1967).  Basic Principles and Calculations in
Chemical Engineering (2nd ed.).  Prentice Hall.
- McCabe W.L., Smith J.C. & Harriott P., Unit Operations in Chemical
Engineering,
- McGraw Hill. Coulson J.M. & Richardson J.F., Chemical Engineering,
Volume 2, fifth edition, ELBS, Pergamon Press. 2002
- 4. Rousseau R.W., Handbook of Separation Process Technology, John
Wiley
- Distillation Project. (15 July, 2017). Retrieved 29 March, 2018, from
NTNU Det Skapende Universitet:
http://folk.ntnu.no/skoge/diplom/prosjekt09/mar/Distillation
%20project.pdf
- A distillation column for tray efficiency studies by Michael dean burns
- “Unit Operations of Chemical Engineering” by Warren L. McCabe
- “Perry’s chemical engineering handbook” (6th edition) by Perry, Robert
H., Green Don W.
- Geankoplis, C. J. (1993). Simple Distillation Methods. In Transport
Procesess and Unit Operations (3rd Edition ed., p. 644). Minnesota:
Prentice Hall.
- Geankoplis, C. J. (1993). Types of Separation Processes and Methods. In
Transport Processes and Unit Operations (3rd Edition ed., p. 585).
Minnesota: Prentice Hall.

29
 APPENDIX
Table 3: List of symbols and their meaning

S/N SYMBOL MEANING UNIT

1 F Feed L/min
2 W Bottom product L/min
3 D Distillate L/min
4 R Reflux ratio Unit-less
5 Ln Mass or molar flow-rate of the liquid reflux L/min
retuned to the column from the condenser.
6 Vn Mass or molar flow-rate of the vapour leaving L/min
the top of the column and entering the
condenser.
7 Xf Mole fraction of the most volatile component in Unit-less
the feed
8 Xd Mole fraction of the most volatile component in Unit-less
the distillate
9 Xw Mole fraction of the most volatile component in Unit-less
the bottom
10 Vm Mass or molar flow-rate of the gaseous boil-up L/min
retuned to the column from the reboiler
11 Lm Mass or molar flow-rate of the liquid leaving L/min
the bottom of the column and entering the
reboiler.
12 Xn Mass or mole fraction of the most volatile Unit-less
component in the liquid leaving state n
13 yn Mass or mole fraction of the most volatile Unit-less
component in the vapour leaving state n

30