Steady State Distillation of A Binary Mixture Under Continuous Operation

Object of experiment
Steady state distillation of a binary mixture under continuous operation.
Equipment set-up
Flow Diagram
5 litres of liquid mixture of methylcyclohexane and toluene containing 65 mol percent

methylcyclohexane in each of the feed tanks and sufficient 25 mol percent methylcyclohexane and
75 mol percent toluene mixture to reach the overflow (V1) in the reboiler.
Also required is:

1 - 250 ml measuring cylinder graduated in mls.
1 - stop watch
1 - hand held refractometer
calibration curve for the feed pump
calibration graph for refractometer (produced in Experiment B)
equilibrium data for methylcyclohexane/toluene at atmospheric pressure.
Summary of theory
Calculation of Number of Plates using the LEWIS-SOREL method
Material balance of top of column.

Equations (1) and (2) combined with the equilibrium curve can be used to calculate the
composition on the various plates working from the condenser down to the still. The plate which
has a composition nearest to that of the feed should be used as the feed plate. Consequently the
number of theoretical plates and position of entry for the feed can be calculated.
Sample Calculation
Using a feed of a binary mixture of 60 mol percent methylcyclohexane and 40 mol percent
toluene.
Top product required: 75 mol percent methylcyclohexane
Bottom product required: 44 mol percent methylcyclohexane
Reflux ratio 5:1
A material balance on the M.V.C. (most volatile component), methylcyclohexane gives,
Feed = Top product + Bottom product

100 x 0.60 = 0.75D + 0.44W
and D = 100-W
100 x 0.60 = 0.75(100-W) + 0.44W
W = 48.39 and D = 51.61
Procedure
Charge the feed beaker with 5 litres of a mixture of 65 mol percent methylcyclohexane and 35 mol
percent toluene. Required for the mixture are:
1.17 litres of toluene
3.83 litres of methylcyclohexane
Charge the reboiler with 10 litres of a mixture of 25 mol percent methylcyclohexane and 75 mol
percent toluene. Required for the mixture are:
7.15 litres of toluene
2.85 litres of methylcyclohexane
Make sure the filler cap on the top of the reboiler is firmly replaced. Turn on the power to the
control panel. Set the temperature selector switch to T9, 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 litres/min. This rate may be varied according to the temperature of the water. If there is
insufficient water flow, some of the vapour will be uncondensed and emerge from the vent pipe at
the side of the unit in which case increase the water flow rate. If required, admit cooling water to
the bottom product cooler. This is not always necessary as sufficient cooling takes place in the
pipework to reduce the product temperature from the boiling point.
On the control panel turn the power controller for the reboiler heating element fully anti-
clockwise and switch the switch turning on the power to the heating element to “power on”
position. Another red lamp will illuminate indicating the heating element is on. 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.
Eventually, vapour 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 T1. Vapour 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 vapour will return to the column.
The cool distillate is then returning to the top of the column and will cascade down the trays
forming a liquid level on the trays and bubbling of vapour passing through the liquid. The system
will have reached an equilibrium condition when the temperatures T1, T2, T3, T4, T5, T6, T7 and
T8 have reached an average steady temperature (but note cycling due to the intermittent reflux).
Before switching on the reflux switch, set the reflux ratio to 5:1, meaning 5 sec back to column and
1 sec to top product receiver, (see “Operational Procedures”). C- means back to column and C+
means to top product receiver. When this is done, switch the reflux valve on (on the control
panel). You should now hear a click, meaning the reflux valve is working. You should also see
condensed vapour flowing to the top product receiver.
The feed to the column must be admitted at the mid point (onto tray 5).
When the column has stabilised at total reflux (it takes 15 to 30 minutes), the flow of feed and the
reflux can be started at the same time.
It is advisable to set a feed flow of 2 litres/hr (from the feed pump calibration graph).
As the flow into the column becomes established so more vapour 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 litres take a sample of the overheads through valve V3. When doing
that, be careful never to drain the condensate return line ie. partially open valve V3 to leave a
small amount of liquid in the line all the time. Take a further four samples.
Generally, when taking samples, drain a “discarding” sample of approximately 5 to 10 ml before
taking the representative sample in a sample glass. Do not drain too much of the “discarding”
sample because of the disturbance of the mass balance. Discard the “discarding” sample in a safe
way. After the representative sample has been taken, keep the sample glasses in an upright
position. Do not overturn them because of the possibility of evaporation of the sample.
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. CAUTION! THIS SAMPLE WILL BE
HOT. Record the refractive index for this sample, too.
Repeat the sample taking a further nine times during the experiment (before feed runs out).
x = mole fraction of methylcyclohexane in liquid
y = mole fraction of methylcyclohexane in vapour
t = temperature, °C

Steady State Distillation of A Binary Mixture Under Continuous Operation

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Object of experiment

Steady state distillation of a binary mixture under continuous operation.

5 litres of liquid mixture of methylcyclohexane and toluene containing 65 mol percent

Also required is:

Calculation of Number of Plates using the LEWIS-SOREL method

Material balance of top of column.

A material balance on the M.V.C. (most volatile component), methylcyclohexane gives,

Feed = Top product + Bottom product

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