Experiment No. 5

EXPERIMENT NO: 4
Steady state distillation of a binary mixture under continuous operation.
ABSTRACT:
This experiment was performed to understand and implement the knowledge of distillation of
binary mixture of ethanol and water. Continuous distillation of ethanol-water mixture was
studied and the efficiency of the column was estimated. Apart from that, top and bottom product
concentrations were determined by using a refractometer. The efficiency was calculated on the
basis of number of theoretical stages by McCabe Thiele method.
INTRODUCTION:
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 components out of the mixture. Large
scale, continuous distillation is very commonly used in the chemical process industries where
large quantities of liquids have to be distilled. The assembly is very much similar to the batch
distillation apparatus [1].
WORKING PRINCIPLE:
The principle for continuous distillation is same as for the normal distillation process. A mixture
is heated up, and routed into the distillation column. On entering the column, the feed starts
flowing down but part of it, the components with lower boiling points vaporize and rise.
However, as it rises, it cools and while part of it continues up as vapor, some of it (enriched in
less volatile component) begins to descend again. In a continuous distillation column, the system
is kept in a steady-state. Feed rate and feed composition are kept constant therefore, product rate
quality are also constant [2].
APPLICATIONS:
It is widely used in petroleum refining, natural gas processing, petrochemical production, coal tar
processing and hydrocarbon solvents production.
APPARATUS:
Continuous distillation apparatus, hand held refractometer, measuring cylinder 250 ml, stop
watch.
REAGENTS:
Ethanol, water.
Manometer
Steel
framework
Stripping
column
Control panel
Figure 1: Labelled diagram of continuous distillation

column
PROCEDURE:
 Charge 10 liters feed mixture of 65 mole percent Ethanol and 35 mole percent Water to feed
tank. Volume of individual components required is calculated first.
 Charge the reboiler with 10 liters of a mixture of 25 mole percent Ethanol and 75 mole
percent Water.
 Turn on the power to the control panel. Set the temperature selector switch to T9, that is the
temperature in the reboiler, and open valve V5 admitting the cooling water to the condenser
at a flow rate on FI1 of approximately 3 liters/min. This rate may be varied according to the
temperature of the water.
 On the control panel turn the power controller for the reboiler heating element fully anti-
clockwise and turn on the power to the heating element. Turn the power controller clockwise
until a reading of approximately 1.5 kW is obtained on the digital wattmeter. The contents of
the reboiler will begin to warm up and this can be observed on the temperature readout
meter.
 Vapor will begin to rise up the column and the progress of this can be clearly observed as
well as detected by the increasing temperatures when switching the temperature selector on
T8, T7, T6, T5, T4, T3, T2 and Tl. Vapor will enter the condenser and reappear as droplets
into the glass walled distillate receiver vessel. The distillate will build up a small level in the
receiver and eventually overflow to the reflux regulator valve. Start the experiment with total
reflux, meaning the condensed vapor will return to the column.
 The cool distillate is then returning to the top of the column, will cascade down the trays
forming a liquid level on the trays and bubbling of vapor passing through the liquid. The
system will have reached an equilibrium condition when the temperatures Tl to T8 have
reached an average steady temperature.
 Set the reflux ratio to 5:1 which means 5 sec back to column and 1 sec to top product
receiver. Now the reflux switch is turned ON.
 The feed to the column is admitted on the tray 5. Let the column has stabilized at total reflux
for 15 to 30 min, then start the flow of feed and the reflux at the same time. It is advisable to
set a feed flow of 2 liters/hr. As the flow into the column becomes established so more vapor
will rise up the column and appear as condensate in the distillate receiver, allow this to flow
to the top product receiver.
 After feeding approximately 3 liters take a sample of the overheads through valve V3. Open
V3 only partially to not drain condensate return line completely.
 Take approx. 5 to 10 ml discarding sample before taking the representative sample. After the
representative sample, has been taken, keep the sample glasses in an upright position.
 Record the refractive index for the taken overhead sample. In a similar manner and
preferably at the same time take a sample of the bottom through valve V2. Record the
refractive index for this sample.
OBSERVATIONS & CALCULATIONS:

 Calculations for required concentration solutions:
Volume required = 3.5L

Molecular Weight=M=0.65(46) +0.35(18) =36.25kg/kmol
Density=D=0.65(789) +0.35(1000) =862.8kg/m3
Concentration=C=D/M=862.85/ (36.2 x 1000) = 0.0238kmol/L
nA=xACV= (0.65) (0.0238) (3.5) =0.054
For nA=0.054, m=2.484g and VA=3.14L
nB=xBCV= (0.35) (0.0238) (3.5) =0.0029
For nB=0.029, m=0.522g and VB=0.522L
So 3.14L ethanol is mixed with 0.52L water to make required solution. Similarly, calculations
are done for 25 mole percent ethanol in water solution.
TABLE # 1: TOP AND BOTTOM PRODUCT COMPOSITIONS:
Top Product Top Product Bottom Product Bottom Product
Refractive Composition (Mole refractive index n Composition (Mole
index n Fraction of Ethanol) Fraction of Ethanol)
1.342 0.19 1.341 0.13
1.354 0.20 1.343 0.15
1.363 0.60 1.361 0.49
TABLE # 2: REFRACTIVE INDEX AND MOLE FRACTIONS:

Mole Fraction xA Refractive Index (n)
0 1.331
0.2 1.355
0.4 1.360
0.6 1.362
0.8 1.365
1 1.361
Average Efficiency = E = Number of Theoretical Plates/ Number of Actual Plates X100

= (3 x 100)/8
= 37.5%
GRAPH # 1: REFRACTIVE INDEX VERSUS MOLE FRACTION OF ETHANOL:
GRAPH # 2: MOLE FRACTIONS OF ETHANOL IN LIQUID AND VAPOR STATES:

X-axis: mole fraction of
ethanol in liquid
Y-axis: mole fraction of
ethanol in vapors
DISCUSSION & CONCLUSION:

As it is evident from the second graph that we can calculate the theoretical number of plates from
which average efficiency is calculated, that comes out to be 37%. The low value of efficiency
means that we cannot achieve a high purity level.
REFERENCES:
1. Seader J.D and Ernest J. Henley, Separation Process Principles. John Wiley & Sons, Inc.
255-265. (2006).
2. Tham Ming T. Distillation, An Introduction. Chemical and Process Engineering at the
University of Newcastle, Tyne, UK.

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EXPERIMENT NO: 4

Steady state distillation of a binary mixture under continuous operation.

Figure 1: Labelled diagram of continuous distillation

OBSERVATIONS & CALCULATIONS:

Volume required = 3.5L

TABLE # 2: REFRACTIVE INDEX AND MOLE FRACTIONS:

Average Efficiency = E = Number of Theoretical Plates/ Number of Actual Plates X100

GRAPH # 2: MOLE FRACTIONS OF ETHANOL IN LIQUID AND VAPOR STATES:

DISCUSSION & CONCLUSION:

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