My Distillation Column
My Distillation Column
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.
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 0.162 L/min, the distillate flow-rate was found to be 0.035
L/min and the bottom product was found to be 0.127 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 8.
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 162.5%. 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.
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INTRODUCTION
Distillation is a process of physically separating a mixture into two or more
products that have different boiling points, by partial vapourization 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.
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located at different heights on a fractionating column. The bottoms fraction can
be taken from the bottom of the distillation column or unit, but is often taken
from a reboiler connected to the bottom of the column.
METHOD OF DISTILLATION:
Differential Distillation
Flash or equilibrium distillation
Rectification.
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THEORY
A brief description on the continuous distillation is an ongoing separation
process in which a liquid mixture of two or more miscible components is
continuously fed into the process and physically separated into two or more
products by preferentially boiling the more volatile (i.e., lower boiling point)
components out of the mixture.
To provide for the intimate mixing of the upward flowing vapour and
downward flowing liquid in distillation columns, the columns usually contain a
series of horizontal distillation trays or plates. The distillation trays or plates
are typically separated by about 45 to 75 centimetres of vertical distance.
However, some columns are designed to use beds of packing media rather than
trays or plates.
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Distillation as seen is a separation process method that converts a mixture or
solution of chemical substances into two or more distinct product mixtures. At
least one of results of the separation is enriched in one or more of the source
mixture's constituents. In some cases, a separation may fully divide the mixture
into pure constituents. Separations exploit differences in chemical properties or
physical properties (such as size, shape, mass, density, or chemical affinity)
between the constituents of a mixture.
This process separating mixture into two or more products that consist of
different boiling points through the vapourization of a liquid mixture
components and the recycling of counter-current gas liquid flow in the column.
Therefore, the liquid phase richer is less volatile which has higher boiling point
and the vapour phase is more volatile with the lower boiling point component.
Distillation process is the most of common separation used in industry because
it’s known as 90% efficiency in separation process and significantly user of
energy in the heating process that necessarily involved. The apparatus used in
the distillation process is Distillation Column.
The column of the distillation column has many types of tray such as bubble
cap trays, sieve tray and packed bed column. The principal of bubble cap tray
is not a counter current flow but cross flow on every stage while sieve tray
flow with counter current flow. Furthermore, packing column can have a lower
pressure drop and good for thermally sensitive liquid. To determine the
appropriate tray, it will consider the fouling tendency, allowable of pressure
drop and turndown requirement in the column.
The separation of distillation process that use heating power can separate the
vapour and liquid phase. Heating element installed at the bottom of to ensure
the liquid mixture evapourates in the whole column. The vapour phase will rise
up into the condenser and the product will be entering into the distillate tank,
meanwhile the liquid will go downward as a waste or bottom product. There
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are two heat exchangers above the distillation column. The function of the
second exchanger acts as condenser, which allow the vapour leaving the first
exchanger using cooling water. Then the reflux tank will be filled with the
condensate that flow from condenser. The electromagnetic controlled in the
column by switching of on and off controlled the reflux ratio. The remaining
from the reflux tank then turned back to the top of the column. The separation
behaviour of the column can be analysed by the samples analysed for each
stage. Therefore, the refractive index of every sample analysed by refractor
meter. The rectification is the mass transfer between the two phases in
equilibrium
From the distillation column system, there are two major method that need to
be followed in order to carry out the experiment, which is batch distillation
method and continuous steady state distillation process. Batch distillation
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process is the process when there is no reflux and the vapour that boiling the
liquid mixture to be separated and condensing vapour not allowing any liquid
to return into the top column. Therefore, the continuous distillation process is
vice versa. Some example of continuous distillation is flash distillation (single
stage partial vapourization) and rectification distillation.
INDUSTRIAL APPLICATION
Distillation is one of the unit operations of chemical engineering. Continuous
distillation is used widely in the chemical process industries where large
quantities of liquids have to be distilled. Such industries are the natural gas
processing, petrochemical production, coal tar processing, liquor production,
liquefied air separation, hydrocarbon solvents production, cannabinoid
separation and similar industries, but it finds its widest application in
petroleum refineries. In such refineries, the crude oil feedstock is a very
complex multicomponent mixture that must be separated and yields of pure
chemical compounds are not expected, only groups of compounds within a
relatively small range of boiling points, which are called fractions.
These fractions are the origin of the term fractional
distillation or fractionation. It is often not worthwhile separating the
components in these fractions any further based on product requirements and
economics.
In the industries, there are many categories of products that use distillation for
separation such as petroleum refining, petrochemical, process of natural gas
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and beverage. In generally, the typical aim to remove the light component from
mixture of heavy component. Other example of distillation process is within
the food industries which concentrating essential oils and flavour,
deodorization of fats and oil.
METHOD OF DISTILLATION:
DIFFERENTIAL DISTILLATION
The rate of depletion of liquid is equal to the rate of distillate output. The
instantaneous rate of depletion of a component in the liquid is therefore,
In - out = accumulation
0 − dD = dL
∫ dlL =∫ y∗−f
dX
W xW
This equation can be integrated to get the following form which is called the
Rayleigh’s Equation,
xf
f dX
¿ = ∫
w xW y∗−f
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The integral on the right-hand side of this equation may be solved graphically
if the equilibrium relationship between f and w is available. Thus, if over the
range concerned the equilibrium.
Then;
f 1 ( m−1 ) x +c
¿ = ∈[ ]
w m−1 ( m−1 ) x 0+ c
The feed is usually pumped through fixed heater and enters through a valve
where the pressure is reduced. The still is essentially a separator in which the
liquid and the vapour produced by the reduction in pressure have sufficient
time to reach equilibrium. The vapour is removed from the top of the separator
and usually condensed while the liquid leaves from the bottom.
RECTIFICATION
Rectification is the most important of these methods, and it differs from the
other two methods in that; part of the vapour is condensed as product.
In the two processes considered the vapour leaving the still at any time is in
equilibrium with the liquid remaining, and normally there will be only small
increase in the 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
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still. This is achieved by arrangement by a known fractionating column which
enables successive evapouration or vapourization and condensation to be
accomplished in one unit
REFLUX:
The term reflux is very widely used in industries that utilize large-scale
distillation columns and fractionators such as petroleum refineries,
petrochemical and chemical plants, and natural gas processing plants.
In that context, reflux refers to the portion of the overhead liquid product from
a distillation column or fractionator that is returned to the upper part of the
column as shown in the schematic diagram of a typical industrial distillation
column. Inside the column, the down-flowing reflux liquid provides cooling
and condensation of the up flowing vapour thereby increasing the efficiency of
the distillation column.
The more reflux provided for a given number of theoretical plates, the better is
the column's separation of lower boiling materials from higher boiling
materials. Conversely, for a given desired separation, the more reflux is
provided, the fewer theoretical plates are required
OVERHEAD:
This is the product leaving the top of the column from the condenser as the
reflux has been sent back into the column.it is also referred to as distillate and
represented by D while the composition by Xd
BOTTOM:
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This is the product leaving the bottom of the column near reboiler. The bottom
is rich in the low or less volatile component. It is represented by W and the
composition by Xw.
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Fig 3: Pictorial view of a continuous distillation column
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NUMBER OF PLATES REQUIRED IN A DISTILLATION COLUMN:
Four streams are involved in the transfer of heat and material across a plate, as
shown in figure below in which plate n receives liquid L n+1 from plate n+1
above and vapour Vn-1 from plate n-1 below. Plate n supplies liquid L n to plate
n-1 and vapour Vn to plate n+1.The action of the plate is to bring about mixing
so that the vapour Vn to plate n+1. The action of the plate is to bring about
mixing so that the vapour 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 during the interchange process on the plate, some of the more
volatile component is vapourized from the liquid L n+1, decreasing its
concentration to xn and some of the less volatile component is condensed from
Vn-1, increasing the vapour concentration to yn.
Lewis-Sorel Method
McCabe and Thiele Method
Mathematical Expression for the Top operating Line and Bottom operating
line equation are shown below;
Thus;
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DESCRIPTION OF APPARATUS
1. CONTINOUS DISTILLATION COLUMN:
The Continuous Distillation Column is a self-contained distillation facility
consisting of two interconnected units: a floor standing process unit and a
bench- mounted control console. 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
maneuver the unit into position initially.
The 50mm diameter sieve plate column is made up of two glass sections (3)
and (4) each containing four sieve plates. The columns are separated by a
central feed section and arranged vertically for counter-current vapor/liquid
flow. The column is insulated to minimize heat loss.
Feed mixture from either of the feed tanks is pumped by pump (7) to the base,
center or top of the distillation column at connections (A), (B) or (C)
respectively. The feed pump incorporates a length of Viton rubber tubing. This
tubing is suitable for all of the recommended test mixtures. Where other test
mixtures are being used, the suitability of this material must be checked.
A packed column is supplied loose. This column can be fitted in place of the
sieve plate column where it is required to demonstrate the characteristics of a
packed column.
The reboiler (13) situated at the base of the column is manufactured from
316stainless steel and incorporates a flameproof immersion type heating
element. Either batch or continuous distillation can be carried out using this
reboiler.
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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 (PRV1) to protect the system in the event of a blocked
vent and cooling water failure. Cooling water enters the condenser at a
regulated rate through a variable area flowmeter (FI1) and the flowrate 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.
2. BEAKER:
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
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Fig 4: A beaker
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PROCEDURES
The cooling water valve controller was switched on.
The reboiler was filled with water until the indicator on the power source
turned green.
The power to the control panel was switched on while the valve bringing in
the cooling water was opened and set at 3000ml/min.
The temperature selector was switched to T9 (the temperature in the
reboiler)
The reboiler was filled with about 1.59 litres to have enough feed in the
reboiler for the operation to run perfectly and the power controller was set
to a value of 1Kw. The contents of the reboiler will be observed to heat up.
After the vapour rises up to the column, the feed tank was opened to allow
the feed stream at T5
Before switching on the reflux switch, the reflux ratio was set to 5:1,
meaning 5 would return to the column and 1 will pass on to the top product
column. A click sound would be heard to indicate the reflux valve is
operating once put on.
The whole operation was allowed to go on for long till enough ethanol was
recovered
A sample from the top product stream was taken for testing and used to
calculate the component of the bottom product since the component of the
feed stream is known.
RESULTS
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Experiment title: CONTINUOUS DISTILLATION COLUMN
xi 0.0035 0.0175 0.0585 0.0935 0.2125 0.3615 0.4985 0.64 0.723 0.837 0.888 0.9489 0.9825
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yi 0.0175 0.13150 0.305 0.411 0.5455 0.6060 0.6555 0.72 0.776 0.852 0.893 0.9502 0.9835
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The Equilibrium graphs was drawn. For easy plot, the x i and yi values were
approximated to 2.dp on the graph.
Given;
Volume of Feed = 9.7 Litres
Volume of Distillate = 2.1 Litres
Xf = 0.25 of Ethanol
Xd = 0.89 of Ethanol
Xw =?
Reflux ratio = 5
Thus;
Performing the over balance on the column;
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F=D+W
0.162=0.035+W
W =0.162−0.035
W =0.127 L/mins
Assuming the percentage provided are by volume;
Component balance on Ethanol;
FXf = DXd + WXw
0.162 (0.25) = 0.035 (0.89) + X w (0.127)
0.0405 = 0.03155 + 0.127 X w
−3
9 x 10
0.127
X w = 0.07
Calculating for the operating lines;
Recall that
LN
R=
D
L n = RD = 5 x 0.035 = 0.175 L/min
V n = L n - D = 0.175 + 0.035 = 0.21 L/min
xd
Cordinate for the top operating lines are (Xd, Xd) and (0, R +1 )
Having drawn the lines, the steps are drawn downwards, starting at point X d =
Yd = 0.89 to get the no. of theoretical trays.
The number of theoretical plates was seen to be 13.
Thus;
Computing for our operating line equations;
TOP OPERATING LINE EQUATION
Recall that
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Ln D
yn = x + x
V n n+1 V n d
D
x is our intercept
Vn d
0.175 0.68−0.48
x n+1 = x =0.833 x n+1
0.21 0.64−0.4 n+1
Thus;
The top operating line equation spelt out above can be written as;
yn = 0.833 x n+1 +0.15
Where;
L m = L n + F = 0.175 + 0.162 = 0.337 L/min
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THE EFFICIELCY
Recall that;
Number of theoritical plates
x 100 %
Actual number of plates
13
x 100 %=162.5 %
8
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DISCUSSION
The experiment; “The continuous Distillation Column” was performed using a
mobile distillation column with the aim of trying to measure the efficiency of
the column. This was done at steady state to maximize the efficiency.
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 bottom operating lines were traced on our plot. Finally, drawing
the steps starting from the distillate mole fraction (Xd), 0.89, the number of
theoretical plates was discovered to be 13 plates.
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The efficiency of the plate was computed to be 162.5%. 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 162.5% implies that
the column is over 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;
Constant check for leakage in our column cylinder.
The decanter must be free from impurities..
Constant servicing of the distillation column.
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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 13 plates from the equilibrium curve. The actual number of plates in the
distillation column was 8. This gave an efficiency of 162.5%.
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.
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RECOMMENDATIONS
1. The feed should be introduced with a higher mole fraction for better
efficiency.
2. Supply of heat to the column must be regulated so the efficiency value
does spike up.
3. A decanter must always be provided so that the azeotrope mixture won’t
be formed.
4. The distillation column should contain more plates in order to get a very
pure distillate product.
5. The set up should be free from leakages as the presence of leakage will
lead to loss of fluids and therefore affect experimental results.
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REFERENCES
Azeotrope: https://en.wikipedia.org/wiki/Azeotrope
A distillation column for tray efficiency studies by Michael dean burns
Coulson Richardson’s Chemical Engineering Volume 2 by J. F.
RICHARDSON, J.H. HARKER and J. R. BACKHURST
McCabe – Thiele method
https://en.wikipedia.org/wiki/McCabe
%E2%80%93Thiele_method#:~:text=The%20parameter%20q%20is
%20the,means%20the%20line%20is%20vertical.
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.
“Separation process principles “by Seader J. D, Henley, Ernest J.
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APPENDIX
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