Batch

Crystallizer

Manufactured by
Rajesh Scientific Industries
6, M. G. Road, Near St. John's college, Agra 282002
Phones: 0562 2850566, 2856011, +91 9837290266
Fax: 0562 2856011, 2850566 email: [email protected]
 Technical Specifications

Crystallizer Double walled jacketed type

MOC SS 304
Capacity Two liter
Dimensions
Outer dimensions 225mmHx200mmD
Inside dimensions 200mmHx150mmD

Stirrer
Drive DC 24V Geared motor
RPM 0-220 Max.
Measurement 7segment LED
Sensor RF Proximity Cylindrical sensor 10-30V DC

Temperature measurement
Display 7Segment LCD
Type Mutiport manual selector
Sensors SS Thermocouple type
Sensor locations Jacket inlet, outlet and Crystallizer

Flow
Measurement Acrylic tube Rotameter
Maximum flow 4LPM
Fittings Push fit interchangeable 8mm fittings
Pipelines 8mm ID PVC flexible pipelines can withstand
temperature upto 120°C, pressure upto
10kg/cm2
Overall dimensions
LxWxH 62x62x124cms
Weight 36kg
 Controls & Position
RPM Indicator
Temp. Indicator
RPM Selector
Cold
Water
In
Rotameter
Drive Cold
Cold water water
Control discharge
Valve
Crystallizer Crystallizer
Temp.
Probe

Bottom Drain Valve Front View

Fuse

Stirring
Unit
Adjustment

Cooling
water
out
probe Cold water in

Rear View
 Crystallization
Objective

To find the yield of batch crystallizer and to verify material balance.

Theory

Crystallization of the substance leads to separation and purification of a substance from

impurities. An understanding of the mechanism by which the crystals form and grow is vital
to any attempt for applying theory in the practical process of crystallization. This operation
involves both heat and mass transfer.
The solubility of the solute in a solvent is function of temperature and is represented by the
equilibrium phase diagram. It is a practical method of obtaining a concentrated chemical
substance in a form that is pure, attractive and convenient for handling. The formation of a
nucleus of the crystal and its growth could be understood through the knowledge of mass
transfer.
If a solution from which crystallization is to occur has no solid particles either of the material
crystallizing out or any foreign particles, then nuclei formation must occur before crystal can
grow. Also nuclei may continue to form while other nuclei are already present and growing.
Nuclei may form spontaneously if conditions are suitable. But in many cases small seed
crystals are added on which the growth takes place to form a large crystal. Refer to the
solubility curve shown in fig.1 The curve CD is the ordinary solubility (equilibrium) curve and
represents the maximum concentration of solutions that can be obtained by bringing solid
solute in equilibrium with the solution. It also represents the ultimate limit towards which
crystallization from supersaturated solution tends.
If a sample of material having the composition and temperature of point E, is cooled in the
direction shown by the arrow, it follows the line EF first crossing the solubility curve and one
could think of start of the crystallization. If pure solution freed from solid particles of the
substance itself and/ or any foreign matter is taken for crystallization, , the solution will not
begin to crystallize until it has super cooled considerably past the cure CD. Somewhere at
the point F crystallization begins according to Miers theory and the concentration of the
substance follows the curve FG. In absence of any solid the curve FG (called the
supersolubility curve) represents the limit at which the nucleus formation begins
spontaneously and consequently point where crystallization can starts. According to the
Miers theory short of this point ( i.e., at any position along the line CD), nuclei can not form
and crystallization can not occur.
Material Balances
If the material crystallizes as a hydrated salt, water of crystallization should be
accounted, since this water separates along with crystals and is removed from the
solution. For the process of crystallization with no evaporative cooling the material
balance equation maybe easily derived as:

F= L + C -------(1)
Fxf = Lxl + Cxc -------(2)

here equation 1 is overall material balance equation and equation 2 represents

component( solute) balance
Where F = feed , kg/hr
L = mother liquor , kg/hr
C = Crystals, kg/hr
X = Weight fraction of solute in liquid and solid phase
 C
A

F E
Concentration

D G

Temperature

Fig. 1: Miers supersaturation Theory

Precautions
1. Ground the instrument to avoid electric shock.
2. Level the instrument before operation.
3. Connect the cold water inlet to the tap having pressure not exceeding
2kg/cm2.
4. After operation clean all the components in contact with mother liquor.
5. To avoid caking due to organic matter development in the jacket, put few
drops of sodium hypochlorite solution in the jacket.
6. Do not use any organic solvent to clean the instrument, Mild detergents
and water shall always be used.
7. Replace fuse of required rating only.
8. Use mother liquors between pH 4.00 to 10.00 for crystallization.
Experimental Setup:

Please refer page 2 for details.

Experimental procedure

1. Prepare a solution of 30%

MgSO4 in water and heat
the solution to 80 -900C.
2. Pour the solution into the
crystallizer and start the
agitator at a Speed on which
no sedimentation of crystals
occurs.
3. Start a cooling water
circulation at a slow rate and
note down the flow rate &
time.
4. Record the temperature Vs
time as the cooling
progresses.
5. Cool the solution until the
temperature reaches 15 0C.
6. Stop the agitator and wait for
25 to 30 min.
7. Open the bottom drain valve
to transfer the magma to the
crystal separator (Sieve) and
collect the mother liquor in
the collecting tank.
8. Dry the crystal collected and
weigh.
9. Take the weigh of mother liquor collected.

Observations and results :

Weight, kg wt. fraction w/w of Solute

Supersaturated liquid taken F =……. XF =

Mother liquor after filtration L = …… XL =

Crystal separated C = …… Xc =
Verify the material balance using equation (1) and (2)
 R
TAP O
T
A
M
E
T
E
R

DRAIN

Flow Diagram for cold water COMMON

+12V
CNT

6 7 8 9

°C RPM

RPM
CONTROLLER

Fluid out
Crystallizer

Fluid in

Electric Circuit