3.

0 METHODOLOGY

3.1 Materials

1. 3 liters of ethanol
2. 4 liters of tap water

3.2 Apparatus

1. 100 ml measuring cylinder

2. 250 ml beaker
3. Thermometer
4. Analytical balance
5. Distillation pilot plant

Figure 1: Distillation pilot plant

Part 1: The feed mixture was loading into the feed tank (TK1)

3 liters of ethanol was mixed with 4 liters of tap water and filled in TK1.

The silicone flexible was connected on the draining valves of the distillate and
bottoms products tank (TK2,TK3).

The silicone flexible was made sure put into the cap.

Part 2: The control panel was activating

The main switch at the control box was turned clockwise to ON the unit.

The emergency stop button was checked whether it was freed by turning the key.

The power indicator turned to white when the power is supplied to the unit.

The GENERAL ON switch was turned on. The power supply was available for
each actuator when green light appeared.
Part 3: The reboiler was loading by feed pump (P1)

Before turning on the P1, V4, V7, V10, V9 and V2 were closed.

The valve V1 was opened.

The 3 ways valve V5 was put in position in order to fill up the reboiler (3 o'clock position).

The 3 ways valve V6 was put in position in order to use the thermal siphon re-boiler (12 o'clock
position).

The outlet flexible tubing of feed pump P1 was made sure to fill with liquid mixture.

The feed pump P1 was activated by turning on the P1 General On switch.

The valve V3 was opened.

The reboiler was loading up to overflow line.

The feed flow rate was set up to 20L/h by adjusting the F14.

Part 4: Water feeding of condenser and refrigerants

 Valve V19 was opened.

Valve V20 was opened and flow rate was set at 60L/h.

The heating was started after the cooling water circulating inside the distillation unit.

Part 5: Heating
 The cooling water was ensured to circulate in the distillation unit before the heating was started.

Electrical heater on the control box was switched on.

The boiler percentage was adjusted to 50% on the touch screen.

The vapours coming up into the distillation column was observed.

Valve V5 was put in position, such that the mixture flows into the middle of the distillation
column when the mixture is boiling.

The column pressure drop was observed, the normal value was 100mm of water.

The boiler percentage was adjusted based on pressure inside the boiler.

The vapors condensed in the condenser was observed.

The boiler percentage and the charge pump flow rate were reduced when the pressure was too
high.

Part 6: Adjustment of reflux ratio

 The vapor was ensured to condense and fills up condenser ECH3.

The reflux flow rate V12 and distillate flow rate V13 were opened.

The pump P2 was switched on.

Air bubble was ensured not inside the flow meter.

Valves V12 and V13 were adjusted to the reflux ratio of 0.5 (2.0 for next experiment).

The system was waited until stable. 100ml of mixture was collected from cooled residue
opening V8, cooled distillate opening V10 and feeding mixture opening V4. The valves
were opened slightly and slowly less than 45°.

V17 and V16 were opened to drain the ethanol and water in TK1 after collected the
mixtures from each reflux ratio.

The density of each samples was measured from each reflux ratio.

The results were recorded in the table.

Part 7: Residue extraction

 P3 from control box was switched on.

Valve V8 was opened.

The extraction flow was adjusted from valve V11 to maintain a constant level into
the reboiler.

The liquid flow into the reboiler was miantained as constant as possible.

Part 8: Stop at the end of the workshop

All the pumps and the boiler heating were stopped.

The cooled water circulation flow rate was kept at 200L/h into the condenser.

The boiler was waited to cool down at least 30°C on Tl1 indicator.

The unit and experimental area were cleaned.

The electric control box was turned off with the main switch. The main switch was
locked.

All the valves were closed.