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Experiment 4
BATCH EVAPORATIVE CRYSTALLIZATION
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1.0 INTRODUCTION
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R1 Feed/reaction vessel
B4 Dosing vessel
P2 Dosing pump
B1 Crystallizer vessel
P1 Crystallizer pump
P3 Vacuum pump
W1 Heat exchanger
W2 & W3 Condensers
T1 Heating thermostat
T2 Heating and cooling thermostat
B2 Product vessel
B3 Condensate vessel
B5 Sampling bottle
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2.0 OBJECTIVES
a) Material required
Salt
Water
Table 1:
Solution Mass of salt (kg) Volume of water (L)
A 3.5 7.0
B 2.5 7.0
C 1.5 7.0
4.1.1 Ensure all valves are closed except the ventilation valve V12.
4.1.2 Check that the product vessel B2 is empty of liquid.
4.1.3 Prepare about 7 litres saturated salt solution by dissolving the
appropriate amount of salt in water.
4.1.4 Pour the saturated salt solution into the crystallizer vessel B1 through
valve V10 until the liquid overflows at the conical inlet. Close valve V10.
4.1.5 Pour the remaining solution into the feed/reaction vessel R1 through the
charge port.
4.1.6 Switch on the stirrer M1 and adjust the speed to mid-range.
4.1.7 Switch on the crystallizer pump P1 and set the circulation flow rate to
200L/hr. Observe the liquid solution flowing from the crystallizer vessel
B1 through the pump to the heat exchanger W1 and then overflowing at
the conical inlet back to the crystallizer vessel.
4.1.8 Turn on the cooling water flow by opening valves V14 and V15.
4.1.9 Ensure that the thermostat T1 contain sufficient heat transfer fluid while
thermostat T2 contain sufficient water. Refill as necessary.
4.1.10 Switch on both thermostats T1 and T2. Set the temperature of
thermostat T1 (containing thermal-oil fluid) to 110oC and thermostat T2
(containing glycol-water) to 80oC. Set the pump speed for both
thermostats to a value of 8.
4.1.11 To operate the crystallization process under vacuum, close valve V12.
Switch on the vacuum pump P3 and set vacuum pressure at 0.3 bar on
the controller.
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It is advisable to set the vacuum level to allow the feed solution to boil at a
temperature of less than 80oC.
4.1.11.1 Observe the temperature rise in the feed/reaction vessel until it has
reached a constant value.
4.1.12 Allow the circulation line to heat up until boiling and evaporation occurs
and condensate starts to appear in the condensate vessel B4.
4.1.13 The unit is now ready for experiments.
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4.3.3 If the unit is operating under vacuum, slowly open vent valve V7 and V8
to release the vacuum.
4.3.4 Open valve V6 to collect the required amount of slurry solution and close
valve V6.
4.3.5 Carefully open the quick removable connections at product vessel B2 and
remove the vessel. Pour the slurry solution into a collection bottle.
4.3.6 Clean the product vessel before placing it back into the unit.
4.3.7 From the collection bottle, pour the slurry solution through a filter to
obtain the crystallized solid. Dry the solid by putting it under the sun or
in an oven.
4.4.1 If the unit is operating at atmospheric pressure, simply open valve V13 to
drain the condensate vessel B3.
4.4.2 If the unit is operating under vacuum, isolate the vessel from the
vacuum system by closing valve V11.
4.4.3 Slowly open vent valve V12 to release the vacuum.
4.4.4 Open valve V13 to fully drain the vessel. Close valve V13.
4.4.5 To return the condensate vessel B3 to vacuum, close vent valve V12 and
slowly open valve V11.
4.5.1 Reduce the temperature set point for both thermostats T1 and T2 to
below room temperature and allow the liquid in the thermostats to cool
down to room temperature.
4.5.2 Keep the cooling water running through condensers W2 and W3.
4.5.3 Switch off the stirrer M1 and dosing pump P2.
4.5.4 Set the circulation flow rate of pump O1 to 200 L/hr and allow the liquid
to cool down to room temperature.
4.5.5 Turn off the circulation pump P1.
4.5.6 Close valves V14 and V15 to stop the cooling water flow.
4.5.7 Carefully open the quick removable connections at product vessel B2 and
remove the vessel. Discard and clean any remaining liquid or solid
residue in the vessel.
4.5.8 Remove the sampling bottle B5 and open valve V5 to drain all liquid from
the circulation line.
4.5.9 To clean the solid residue in the circulation line, attach a hose to valve
V9 and flush the pipelines with tap water. Drain the water through
valves V5 and V6.
4.5.10 Drain the condensate vessel B4 by opening valve V13.
4.5.11 If required, drain the liquid in the feed/reaction vessel by opening valves
V1, V2 and V3.
4.5.12 Place the product vessel B2 and sampling bottle B5 back into the unit.
Close valves V5 and V6.
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Discuss all your results. The questions below only serve as a guideline. Your discussion
should not only limit to these questions.
1. Compare the yield of crystals obtained from the experiment with the yield of
crystals obtained from the calculation based on material balances.
2. Discuss the factors which influenced the yield of crystals.
3. Discuss the relationship between rates of evaporation with the crystallization
process.
4. Compare the batch crystallization process using cooling and evaporation
method.
REFERENCES
1. Perry, R.H., Green, D.W. and Maloney, J.O., “Perry’s Chemical Engineering
Handbook”. 6th edition, McGraw Hill, 1984.
2. Geankoplis, Transport process and unit operation 3rd Edition, Prentice Hall
(1993).
3. McCabe, Smith and Harriott, Unit operations of Chemical Engineering,
McGraw Hill 6th edition (2000).
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Table of Results:
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Circulation Thermal Vent Heat Heat Feed/reaction Feed Thermal oil Thermal oil Volume of
flow rate oil flow pressure exchanger exchanger vessel temperature inlet outlet condensate
Time
rate inlet outlet temperature temperature temperature
temperature temperature
F1301 F1302 PIC201 TI101 TI102 TI103 TI104 TI105 TI106 B3
L/hr L/hr bar oC oC oC oC oC oC mL
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20104
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