Distillation Report
Distillation Report
FACULTY OF ENGINEERING
UNIVERSITY OF BENIN.
A TECHNICAL REPORT ON
MIXTURE.
(CHE 401)
TITLE PAGE
TITLE OF EXPERIMENT: STEADY STATE DISTILLATION OF A
BINARY MIXTURE.
AIM OF EXPERIMENT:
GROUP NUMBER: B4
DATE: 08/11/2023
i
LIST OF FIGURES
FIGURE 1: FUNCTION OFREBOILER..................................................................4
FIGURE 2: FUNCTION OF REFLUX.....................................................................5
FIGURE 3: SCHEMATIC DIAGRAM FOR RECTIFICATION COLUMN..........6
FIGURE 4:CALCULATION OF NUMBER OF PLATES BY LEWIS SOREL
METHOD..................................................................................................................8
FIGURE 5: CONTINUOUS DISTILLATION COLUMN.......................................9
FIGURE 6: DETAILED VIEW OF THE CONTINUOUS DISTILLATION
COLUMN................................................................................................................10
FIGURE 7: REFRACTOMETER...........................................................................13
FIGURE 8: BEAKER..............................................................................................13
LIST OF TABLES
ii
TABLE OF CONTENT
TITLE PAGE............................................................................................................i
LIST OF FIGURES..................................................................................................ii
TABLE OF CONTENT..........................................................................................iii
ABSTRACT.............................................................................................................1
INTRODUCTION...................................................................................................2
THEORY.................................................................................................................4
DESCRIPTION OF APPARATUS..........................................................................9
PROCEDURE........................................................................................................14
RESULT................................................................................................................ 16
DISCUSSION........................................................................................................22
CONCLUSION......................................................................................................24
RECOMMENDATION.........................................................................................25
REFERENCES...................................................................................................... 26
APPENDIX............................................................................................................27
iii
ABSTRACT
The steady-state distillation of a binary mixture experiment was carried out with
the aim of investigating the steady state distillation of a binary mixture (ethanol &
water) under continuous operation and to determine the efficiency of the trays of
the steady state distillation in a binary mixture as a function of feed stage location
and reflux ratio with the use of both the Lewis Sorel method and the McCabe-
Thiele method. This was done on a binary mixture of Ethanol and water with the
most volatile component as Ethanol. It was observed that for the distillate
compositions attained in this experiment, the McCabe-Thiele graphical method
predicted 4 stages which was fewer than the stages found in the laboratory column
indicating there was an efficiency of 12.5 % in the system. 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 fundamental unit operations of chemical engineering and
is simply defined as a process in which a liquid or vapour mixture of two or more
substances is separated into its component fractions of desired purity, by the
application and removal of heat. The process is based on the fact that the vapour of
a boiling mixture will be richer in the components that have lower boiling points.
Hence, when this vapour is cooled and condensed, the condensate will contain
more volatile components. At the same time, the original mixture will contain
more of the less volatile material. The primary equipment employed in the process
of distillation are distillation columns, which are designed to achieve this
separation efficiently.
Distillation process is the most of common separation used in industry because it’s
known as 90% efficiency in separation process and consumes enormous amounts
of energy, both in terms of cooling and heating requirements. It can contribute to
more than 50% of plant operating costs.
The best way to reduce operating costs of existing units, is to improve their
efficiency and operation via process optimization and control. This requires a
thorough understanding of distillation principles and how distillation systems are
designed is essential.
The term “still” is applied only to the vessel in which liquids are boiled during
distillation, but the term is sometimes applied to the entire apparatus, including the
fractionating column, the condenser, and the receiver in which the distillate is
2
collected. If a water and alcohol distillate is returned from the condenser and made
to drip down through a long column onto a series of plates, and if the vapour, as it
rises to the condenser, is made to bubble through this liquid at each plate, the
vapour and liquid will interact so that some of the water in the vapour condenses
and some of the alcohol in the liquid vaporizes. The interaction at each plate is
equivalent to a re-distillation. This process is referred to by several names in the
industry; namely rectification, fractionation, or fractional distillation.
They are capable of handling high throughputs and are the most common of the
two types.
3
processing of chemical products such as formaldehyde and phenol and the
desalination of sea water.
THEORY
As stated earlier, distillation is the process of separating the components or
substances from a liquid mixture by using selective boiling and condensation.
The liquid mixture that is to be processed is called the feed and can be introduced
through the reboiler, the heat exchangers or can be somewhere near the middle of
the column to a tray known as the feed tray.
Feed to the unit supplied to the still cannot produce a nearly pure product because
the liquid in the still is not subjected to rectification. This limitation is removed by
admiting the feed to a plate on the central portion of the column. The feed tray
divides the column into a top (enriching or rectification) section and a bottom
(stripping) section. The feed flows down the column where it is collected at the
bottom in the reboiler. Since the liquid reaching the reboiler is stripped of one
component, the bottom product can be nearly pure component 2. Heat is supplied
to the reboiler to generate vapor. 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 bottom’s product.
4
The vapour travels up the column, and as it exits the top of the unit, it is cooled by
a condenser. The condensed liquid is stored in a holding vessel known as the reflux
drum. Some of this liquid is recycled back to the top of the column and this is
called the reflux. The condensed liquid that is removed from the system is known
as the distillate or top product.
Thus, there are internal flows of vapour and liquid within the column as well as
external flows of feeds and product streams, into and out of the column.
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:
Differential distillation.
Flash or equilibrium distillation, and
Rectification.
5
FIGURE 3: SCHEMATIC DIAGRAM FOR RECTIFICATION COLUMN
6
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
𝑥𝑓, 𝑥𝑑, and 𝑥𝑤 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
𝑽𝒏=𝑳𝒏+𝟏+𝑫 … equation 1
Expressing this equation for the more volatile component (MVC) gives;
𝒚𝒏=𝑳𝒏+𝟏𝑽𝒏𝑿𝒏+𝟏+𝑫𝑽𝒏𝑿𝒅 … equation 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, 𝑳𝒏 may be replaced by 𝑳𝒏+𝟏
𝒚𝒏=𝑳𝒏𝑽𝒏𝑿𝒏+𝟏+𝑫𝑽𝒏𝑿𝒅 … equation 3
Similarly, taking a material balance for the total streams and for the more volatile
component from the bottom to above plate m,
𝑽𝒎=𝑳𝒎+𝟏−𝒘 … equation 4
7
FIGURE 4:CALCULATION OF NUMBER OF PLATES BY LEWIS SOREL METHOD.
With the two equations and the equilibrium curve, 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 𝑦𝑡 from the top plate must equal that of the product 𝑥 ,
and that of the liquid returned as reflux 𝑥𝑡.
N
η= × 100
NR
8
DESCRIPTION OF APPARATUS
9
FIGURE 6: DETAILED VIEW OF THE CONTINUOUS DISTILLATION COLUMN
FLOOR-STANDING FRAME - The distillation column is mounted on a floor
standing, welded tubular steel framework (1) fitted with four adjustable feet (2).
The frame is designed to allow the use of a fork lift or pallet truck to manoeuvre
the unit into position initially.
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successive stages. The liquid seal on the final plate in each section is achieved by
U-tube (H).
Feed mixture from either of the feed tanks is pumped by pump (7) to the base,
centre or top of the distillation column at connections (A). (B) or (C) respectively.
REBOILER - The reboiler (13) situated at the base of the column is manufactured
from 316 stainless steel and incorporates a flameproof immersion type heating
element. Either batch or continuous distillation can be carried out using this
reboiler.
In continuous operation, valve (VI) is open and bottom product flows from the
reboiler through the bottom product cooler (15) to the bottom product tank (9). It is
possible to preheat the feed to the column by directing the feed through a spiral
coil in the bottom product cooler where heat is transferred from product leaving the
reboiler at the boiling point. When feeding cold feed directly to the column, the
product from the reboiler is cooled in the bottom product cooler by circulating cold
water through the spiral cord.
CONDENSER - Vapour from the top of the column passes to a water-cooled, coil-
in-shell condenser (8), which may be fitted with an insulated jacket to allow heat
balances to be carried out. (The insulated jacket should not be fitted to the
condenser for normal operation.) The shell of the condenser incorporates a
pressure relief valve (PRVI) to protect the system in the event of a blocked vent
and cooling water the condenser at a regulated rate through a variable area flow
meter (FI1) and the ilure. Cooling water enters flow rate is controlled by
diaphragm valve (V5). A cooling water supply is connected to the inlet nozzle (19)
and serves also to operate the vacuum pump (20) when operation at reduced
pressure is required. Water supply to the vacuum pump is controlled by valve
(V14), which must only be operated when valve (V5) is open.
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DECANTER - Condensate is collected in a glass decanter (11) (phase separator)
which is by-passed for normal distillation experiments by opening valve (V10).
When the decanter is in use (separation of two immiscible liquids as condensate),
valve (V10) is closed so that the overflow (25) and underflow (26) pipes inside the
vessel, can take effect.
With valve (V10) open, condensate from the condenser outlet passes directly
through the decanter to the inlet of the reflux ratio control valve (12) which is a 3-
way solenoid operated valve. Depending on the setting of the reflux timers,
condensate is directed by the reflux valve either back to the top of the column or to
the top product collecting vessel (10). When directed to the column, the reflux
passes through a U-seal where a. valve (V3) can be used for measuring boil-up rate
or for draining the U-seal. The contents of the top product tank (10) can be drained
into the reboiler (13) for re-use via valve (V12).
ROTAMETER - This measure the flow rate of the cooling water. The flow rate of
the cooling water is also adjustable.
HEAT EXCHANGER - This transfers heat from the product stream of the bottom
to the feed stream. Bottom Product Receiver: This receives the bottom product of
the process.
12
REFLUX VALVE - It connects the decanter back to the distillation column for
reflux. The reflux ratio is set on the control unit.
FIGURE 7: REFRACTOME
TER
FIGURE 8: BEAKER
13
PROCEDURE
1. The power to the control panel was turned on.
2. The temperature selector switch was set to T9 which was the temperature in
the reboiler, and valve V5 was opened to admit the cooling water to the
condenser at a flow rate on FII of approximately 3 litres/min. This rate was
varied according to the temperature of the water. As a result of insufficient
water flow, some of the vapour were un-condensed and emerged from the
vent pipe at the side of the unit in which case water flow rate was increased.
3. On the control panel, the power controller for the reboiler heating element
(fully anti-clockwise) was turned on and the switch turning on the power to
the heating element to "power on" position was also switched on.
4. The power controller was turned clockwise until a reading of approximately
1.5 kW was obtained on the digital wattmeter. The contents of the reboiler
began to warm up and this was observed on the temperature readout meter.
5. 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.
6. Vapour entered the condenser and reappeared as droplets into the glass
walled distillate receiver vessel. The distillate built up a small level in the
receiver and eventually overflowed to the reflux regulator valve.
7. The experiment was started with total reflux, as the condensed vapour was
observed to return to the column. The cool distillate returned to the top of
the column and cascaded down the trays forming a liquid level on the trays
and bubbled vapour through the liquid. The system reached an equilibrium
condition when the temperatures T1, T2, T3, T4, T5, T6, T7 and T8 have
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reached an average steady temperature (but note cycling due to the
intermittent reflux).
8. Before switching on the reflux switch, the reflux ratio was set to 5:1,
meaning 5 sec back to column and I sec to top product receiver. When this
was done, the reflux valve was switched on (on the control panel). A
clicking sound was observed indicating that the reflux valve was working.
Condensed vapour was also observed to be flowing to the top product
receiver.
9. The feed to the column was admitted at the midpoint (onto tray 5). When the
column stabilised at total reflux (it took 15 to 30 minutes), the flow of feed
and the reflux were started at the same time. The feed flow was set at 2
litres/hr (from the feed pump calibration graph). As the flow into the column
became established, more vapour rose up the column and appeared as
condensate in the distillate receiver, this was allowed to flow to the top
product receiver.
10.After feeding approximately 3 litres, a sample of the overheads was taken
through valve V3. When doing that, careful was taken never to drain the
condensate return line i.e. the valve V3 was partially opened to leave a small
amount of liquid in the line all the time. New four samples were further
taken.
11.Generally, when taking samples, a "discarding" sample of approximately 5
to 10 ml was drained before taking the representative sample in a sample
glass. However, Care was taken not to drain too much of the "discarding"
sample because of the disturbance of the mass balance. The "discarding"
sample was discarded in a safe way.
12.After the representative sample has been taken, the sample glasses was kept
in an upright position and was not overturned because of the possibility of
15
sample evaporation. The refractive index for the taken overhead sample was
taken and recorded.
13. In a similar manner and preferably at the same time a sample of the bottom
was taken through valve V2.
RESULT
3
Volume of feed (F) = 16,240 cm = 16.24 L
Volume of distillate (D) = 7020 cm3 = 7.02 L
Brix number for feed = 38
Brix number for distillate = 71
Reflux Ratio = 5:1 = 5
TABLE 1: DATA OF EQUILIBRIUM CURVE POINTS
S/N X1 Y1
1 0.0035 0.0175
2 0.0175 0.1315
3 0.0585 0.305
4 0.0935 0.411
5 0.2125 0.5455
6 0.3615 0.6060
7 0.4985 0.655
8 0.646 0.729
9 0.723 0.776
10 0.837 0.852
11 0.888 0.893
12 0.9489 0.9502
13 0.9825 0.9835
Brix % Alcohol
30 9.77
40 16.70
60 23.66
16
80 30.61
100 37.55
130 47.97
160 58.39
180 65.34
190 68.81
Interpolating using table 2 to obtain the values of the molar composition for the
feed, distillate and the bottom product.
x f −9.77
= 38-30/40-38
16.70−9.77
xf = 37.49 % = 0.3749
For distillate (xd);
x d−23.66 71−60
=
30.61−23.66 80−60
xd =27.48 % = 0.2748
For bottom product (xw);
Converting the volume of feed and distillate to volumetric flow rates, we divide
both values by time (60mins)
Volumetric flow rate of feed =
16.24/60 = 0.271 L/min
Volumetric flow rate of distillate =
7.02/60 = 0.117 L/min
Thus;
17
Performing the over balance on the column;
F=D+W
16.24 = 7.02 + W
W = 16.24 – 7.02
W = 9.22 Liters.
Lm W
ym = V Xm+1 - V Xw … equation (3) also known as Bottom Operating Line
m m
Equation;
18
Ln = 5 ×7.02 = 35.1
Vn = 35.1 + 7.02 = 42.12
Lm = 35.1 + 16.24 = 51.34
Vm = 51.34 – 9.22 = 42.12
OBSERVATION: Vn = Vm
The values are the same because an azeotropic mixture was formed.
At xn,1 = xd = 0.2748
19
Therefore, yn,1 = (0.833 ×0.2748) + 0.0458 = 0.2748
The next value using the top line equation will give a value lower than that of the
composition of feed (xf) so we use the bottom line equation
Ym+3=0.6188 Xn=3=0.6188
This gave us a value lower than the composition of the bottom product which
should not be so we stop there and count the number of points on the equilibrium
curve.
Fig 9: Graph
20
number of theoretical plates
Efficiency= actual number of plates
21
DISCUSSION
Trying to separate a binary mixture, the experiment was performed using Ethanol
as the most volatile component, mixed with water. The feed volume used was16.24
Litres and the volume of the distillate was 7.02 Litres. Their volumes were
converted to flow rates and the flow rate of the bottom was found to be 0.154
L/min.
The mixture was poured into the column cylinder and the feed was made to pass
through the middle of the column. It should be noted that the position of feed entry
plays a critical role in distillation. The column has two sections, the rectifying and
stripping section. When the feed is passed through the middle, the rectifying
section collects the most volatile component, easily there-by leaving the bottom
with water, which is less volatile. With heat supplied to the column, distillation
took place. The column consists of 8 plates. As the temperature increases, the more
volatile liquid (Ethanol) is gradually vapourized to the condenser, thereafter the
product is being stored in the product tanks. A reflux ratio of 5 was used to get our
desired distillate.
The McCabe – Thiele method was used here in determining the number of
theoretical plates used for the experiment. The equilibrium plot was drawn and our
q-Line (Xf) and Xw was labelled on the graph. The tope operating line (TOLE) and
22
bottom operating lines were traced on our plot. Finally, drawing the steps starting
from the distillate mole fraction (Xd), 0.2748, the number of theoretical plates was
discovered to be 4 plates.
The efficiency of the plate was computed to be 50%. It could be seen that this
high value of theoretical plates was as a result of the formation of an azeotrope
mixture. which is not easy to separate by distillation. To counter this formation, a
desiccant is introduced in the rising vessel.
The value gotten from the calculation of our efficiency at 50% implies that the
column is fairly efficient. This means 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.
Although the efficiency is not supposed to exceed 100%. The value we got as
efficiency was due to different parameters. Some of them include;
The feed mole fraction of the feed
The reflux ratio
The work done by the column
Low supply of heat to the column
The plate of entry for the feed,
Human errors, etc.
This experimental value is applied in the industry to check for the performance of
the distillation column. This will help the engineers to draw conclusion and make
decision to maximize the product required.
Care must be taken when handling the distillation column, this include;
23
Constant check for leakage in our column cylinder.
The decanter must be free from impurities..
Constant servicing of the distillation column.
CONCLUSION
Distillation is one of the most effective separation techniques in both chemical and
petroleum engineering industries and it has its application in petroleum refinery
process. From our evaluations and calculations performed using the McCabe –
Thiele method, the theoretical number of plates was discovered to be 4 plates from
the equilibrium curve. The actual number of plates in the distillation column was 8.
This gave an efficiency of 50%.
With this information, it was safe to conclude that the distillation column was over
efficient as it has violated the law of conservation of energy.
24
RECOMMENDATION
25
REFERENCES
Treybal, Mass Transfer Operations, Third Edition, pp. 185, 342-357, 371-419,
McGraw-Hill Book Co. (1968).
Perry, Green and Maloney, Chemical Engineers' Handbook, Sixth Edition, pp. 18-
37 to 18-19, McGraw-Hill Book Co. (1984).
26
APPENDIX
F = Feed
W = Bottom product
D = Top Product/Distillate
R = Reflux ratio
Ln D
yn = V n Xn+1 + V n Xd = Top Operating Line Equation
Lm W
ym = V m Xm+1 - V m Xw = Bottom Operating Line Equation
27