Mass Transfer 2 CPB 20104

Experiment 4
BATCH EVAPORATIVE CRYSTALLIZATION
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1.0 INTRODUCTION

Crystallization is a separation process where solid particles form within a

homogeneous liquid phase due to supersaturation induced either through cooling or
evaporation. It is essentially a solid-liquid separation techniques and a very important
one at that. An important example is the production of sucrose from sugar beet, where
the sucrose is crystallized out from an aqueous solution. This process can occur in the
freezing of water to form ice, in the formation of snow particle from a vapor, in the
formation of solid particle from a liquid melt, or in the formation of solid crystals from a
liquid solution.

In crystallization, the solution is concentrated and usually cooled until the

solute concentration becomes greater than its solubility at that temperature. Then the
solute comes out of the solution forming crystals of approximately pure solute.

The SOLTEQ-QVF Crystallization Unit (Model: BP 120) has been designed to

demonstrate the basic principles of crystallization and operation of a crystallizer
equipment. The unit consists of mainly a crystallizer vessel, crystallizer pump,
feed/reaction vessel, dosing pump, heat exchanger, condenser, product vessels and
heating/cooling thermostats. This model utilizes both the evaporation and cooling
methods for crystallization. In evaporation, liquid is removed from a saturated feed
solution to generate supersaturation for crystals to form. Similarly in the cooling
method, the solution’s temperature is lowered so that supersaturation can occur.
Figure 1 show the process flow diagram for the crystallization unit.

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Description and Assembly

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

 To perform batch crystallization process utilizing the evaporation method.

 To examine the rate of evaporation and crystallization in a batch process.

3.0 MATERIALS AND ANCILLARY EQUIPMENTS REQUIRED

a) Material required
 Salt
 Water

b) Ancillary Equipments Required:

 10 litres beaker
 Homogenizer

c) Preparation of 7 litres salt solution

Prepare 7 litres of salt solution based on Table 1 a day before the experiment and let
the solution keep overnight.

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

4.0 OPERATING PROCEDURES

4.1 General Start-up:

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.

4.2 Experiment Procedures:

4.2.1 Perform the general start-up procedures as above. For batch

crystallization, thermostat T2 need not be switched on.
4.2.2 Set the circulation flow rate, vacuum pressure and the temperature of
thermostat T1 to a suitable value. Make sure that the feed solution will
boil at the specified temperature and pressure.
4.2.3 Allow the circulation line to heat up until boiling and evaporation
occurs, and condensate starts to appear in the condensate vessel B3.
Start the timer.
4.2.4 Record the circulation flowrate and inlet/outlet temperatures of both feed
solution and thermal fluid through the heat exchanger W1.
4.2.5 Observe the formation of crystals in the circulation line. Once crystals
start to appear, stop the timer and record the time duration.
4.2.6 Measure the amount of condensate accumulated in condensate vessel B3
and drains the condensate vessel. Refer section 4.4. Restart the timer.
NOTE:
If the condensate vessel B3 gets full before any crystals are observed,
drain the vessel when the volume gets to 1000 mL. Remember to note
down the number of times that the vessel has been drained and add to
accumulated amount above.
4.2.7 Perform the following steps at every 15 minutes intervals:
i) Record the circulation flowrate and inlet/outlet temperatures of
both slurry solution and thermal fluid through the heat
exchanger W1.
ii) Measure the amount of condensate accumulated in vessel B3.
iii) Drain the condensate vessel B3 by opening valve V13. Refer
section 4.4.
4.2.8 Carry out step 7 above until the liquid level in the crystallizer vessel B1
has dropped to about halfway below the conical inlet.
4.2.9 Record the total time taken for the crystallization process.
4.2.10 Collect about 2 L of product slurry from the circulation line as explained
in section 4.3.
4.2.11 Determine the amount of crystals obtained and the crystal concentration
in the crystallizer at the end of the batch process.
4.2.12 The entire experiment can be repeated by varying the circulation flow
rate, vacuum pressure and heating rate (temperature at thermostat T1).

4.3 Product Collection

4.3.1 Make sure the product vessel B2 is empty.

4.3.2 If the unit is operating at atmospheric pressure, simply open valve V6
and let the slurry solution flow the circulation line into the product
vessel.

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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 Draining Condensate

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 General Shut-Down Procedures

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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5.0 RESULTS AND DISCUSSION:

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:

Circulation flow rate = ___________________ L/hr

Vacuum pressure = ___________________ bar

Temperature of thermostat (T1) = ___________________ oC

Mass of salt = ___________________kg

Volume of water = ___________________ L

Concentration of feed = ___________________ mg/L

Weight of container = ___________________ g

Weight of crystals obtained + container = ___________________ g

Weight of crystals = ___________________ g

Amount of condensate = ___________________ L

Total time = ___________________ hour

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Table 1: Data of the results

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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