3.

0 AIMS

To determine the pressure drop of the distillation column for various

boil-up rates in batch distillation.

To observe the degree of forming on trays for each power increment
To plot the curve relating pressure drop and boil-up rate
To determine the refractive index for unknown concentration of
methyl cyclohexane/toluene from the distillation column for each
power increment.

5.0 APPARATUS

Continuous Distillation Column (Model UOP3CC)

Automatic Digital Refractometer RX-5000

6.0 METHODOLOGY
The general start-up of the experiment was performed before starting the
experiment. The electrical power at control console was switched on. This
is achieved by moving the ELCB switch to the up position. The Low Level
lamp in the reboiler heater section of the console will be illuminated. The
reboiler

power,

reflux

timer,

column

temperature,

and

process

temperature digital displays will also be illuminated. All valves V1 and V5

were ensure in the closed position. Laboratory cold water supply was
turned on. Flow control valve V5 is opened to give maximum flow into the
condenser via flowmeter F11. The leaks were checked. The manometer
tube was filled until an equal level is visible about halfway up the scale
close valves V6 and V7. Reboiler heat power is switched on at the console
and power was adjusted to the heater 1.5kW. The water in the reboiler will

begin to heat up and this can be observed by selecting T9 on the process

temperature digital display. V6 and V7 were opened and the pressure
difference was observed in the manometer. V6 and V7 were closed.
After completion of the general start-up procedure, the distillation
column for mixing of methyl cyclohexane and toluene was prepared as
first experiment. 10 liter of methyl cyclohexane and toluene were added
to the feed tank. Reboiler heat power was switched on at the console and
power was adjusted to the heater 0.5kW. The water in the reboiler will
begin to heat up and this can be observed by selecting T9 on the process
temperature digital display. The procedure was continued till reflux in the
decanter is stable. Then, the degree foaming is observed either it is gently
or flooding. V6 and V7 were opened and the pressure drop was observed
in the manometer. The pressure drop was recorded. The V6 and V7 were
closed and V3 was opened to get the reflux about 90mL. The time was set
when taking the reflux to get the boil up rate. The reflux was checked for
the refractive index by using refractometer. The curve was plotted relating
pressure drop and boil-up rate. The step was repeated with different heat
power, 0.75kW, 1.0kW, and 1.5kW.
Non-distillation mixing of methyl cyclohexane and toluene was
prepared as second experiment. The 10ml of solution was assumed equal
to 10 mol%. Let say sample A, mix 0 mol% methyl cyclohexane with 100
mol% toluene using conical flask. The solution was stirred carefully. Steps
2 until 3 were repeated for; B (20 mol% methyl cyclohexane, 80 mol%
toluene), C (40 mol% methyl cyclohexane, 60 mol% toluene), D (60 mol%

methyl cyclohexane, 40 mol% toluene), E (80 mol% methyl cyclohexane,

20 mol% toluene), and F (100 mol% methyl cyclohexane, 0 mol%
toluene). The refractive index values for all sample automatic digital
refractometer were recorded.
The refractive index was found using refractometer. Refractive index
value was taken using automatic digital refractometer for each power
sample of product at each power increment. The automatic digital
refractometer was running. The surface was clean using distilled water
then the power was switch on. Zero setting was pressed and the sample
was placed then the Start was pressed. The refractive index value was
recorded. The refractometer was clean and switched off.
The pressure drop versus boil up rate graph was plotted. The
unknown concentration from refractive index versus percentage of methyl
cyclohexane graph was determined.
The general shut-down procedures was performed after completing
the experiment. The heater power, feed pump motor and reflux valve at
console were switched off. The equipment was disconnected from the
electrical supply when the equipment is not used. All of the water was
drained from the system using drain valves V2, V3, V4, V11 and by
breaking pipe connections of the bottom product cooler and the feed
pump.