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CRYSTALLIZERS

Crystallization is important as an industrial process because of the number of


materials that are and can be marketed in the form of crystals. Crystallization process is
commonly used because of its ability to obtain highly purified and in favorable form of a
chemical solid from relatively impure solutions. Also, crystallization requires much less
energy compared to other purification processes such as distillation. In addition, it can
be performed at relatively low temperatures and on a scale which varies from a few
grams up to a thousand of tons per day.

Crystallizers and evaporators is similar however, designing each vessel depends


primarily on the criteria used in arriving at its sizing. In an evaporator, sizing is done on
the basis of vapor release. On the other hand, sizing a crystallizer is normally done on
the basis of the volume required for crystallization or for special features required to
obtain proper product size.

TYPES OF CRYSTALLIZERS

Mixed Suspension, Mixed Product Removal Crystallizers

This type of equipment is by far the most important in use today. It is also sometimes
called the circulating magma crystallizer. In most commercial equipment of this type,
the uniformity of suspension of product solids within the crystallizer body is sufficient for
the theory (the Randolph Larson general population balance) to apply.

The primary reason for this preference is that the heat transferred through the critical
supersaturating step is through a boiling liquid gas surface, avoiding the
troublesome solid deposits that can form on a metal heat transfer surface.

1. Forced Circulation Evaporator Crystallizer

Forced circulation crystallizers are


evaporative crystallizers. They create a super
saturated solution by evaporating the solvent of
a saturated solution. The solute of this super
saturated solution then cools, forming crystals.
The feed slurry is first heated in a heat
exchanger then pumped to the main body of the
crystallizer. Vaporization occurs at the top of the
slurry while nucleation occurs near the bottom of
the crystallizer body. The crystals are removed
and the vaporized solvent is condensed and returned to the crystallizer body.
ADVANTAGES DISADVANTAGES
Least expensive type of crystallizer Crystal size is difficult to control
Large range of sizes available
High rate of circulation reduces particle
deposits on vessel walls

2. Draft Tube Baffle Evaporator Crystallizer

Draft tube baffle (DTB) crystallizers


are used in applications in which excessive
nucleation occurs. Small, unwanted crystals,
called fines, are removed from larger particles
using gravitational settling and recycled
through the crystallizer again, resulting in
maximum crystal recovery and larger crystals
DTB crystallizers have distinct two
volumes. In the baffled region gravitational
settling separates larger crystals from fines.
The larger crystals settle between the baffle
and the draft tube and are removed in the
product slurry, while the fines are recirculated
after being redissolved in a heat exchanger.
The evaporated solvent is then condensed,
cooled, and returned to the region of active crystallization.
ADVANTAGES DISADVANTAGES
Frequent flushings required to minimize
Crystal size is easy to control
deposits on the crystallizer walls
Cannot effectively handle a high
Economic due to recyclability of fines
density slurry
More energy efficient than forced
circulation crystallizers

3. Surface Cooled Crystallizer

Surface cooled crystallizers combine a draft tube baffle crystallizer


body with a forced circulation heat exchanger. The slurry is drawn from the
crystallizer body and then cooled before being pumped back into the crystallizer
body.
Crystallizers such
as these are the most
useful for operations in
which the solutions
boiling point is extremely
high, or when such low
temperatures are
required that evaporation
by vacuum is not
possible.

4. Direct Contact Refrigeration Crystallizer

When crystallization occurs at such


low temperature that it is impractical to use
surface cooling or when the rapid
crystallization of solids on the tube walls
would foul a conventional surface cooled
crystallizer, a draft tube baffle crystallizer or
a forced circulation unit utilizing the direct
contact refrigeration technique can be
employed.
In this operation, a refrigerant is
mixed with the circulating magma within the
crystallizer body where it absorbs heat and
is vaporized. Refrigerant vapor leaves the
surface of the crystallizer similar to water
vapor in a conventional evaporative
crystallizer. It must be compressed, condensed and circulated to the crystallizer
to maintain continuous operating conditions. Refrigerants must be relatively
insoluble in the solutions processed and have the thermodynamic characteristics
to minimize compressor horsepower.

5. Reaction Type Crystallizer


Reaction type crystallization, or reactive crystallization, is where a solid
phase crystalline material results from the
reaction of two components, can often be
performed more profitably in a crystallizer than
in a separate reactor.
The draft tube baffle crystallizer is
particularly suited for reactive crystallization.
The reactants are mixed in the draft tube of
the DTB unit where a large volume of slurry is
mixed continuously with the materials to
minimize the driving force created by the
reaction. The removal of heat produced by the
reaction is accomplished by vaporizing water
or other solvents as in a conventional
evaporative type of crystallizer
Also, reactive crystallization can be
performed in a forced circulation type
crystallizer, where the reactants are mixed in the circulation piping.

Factors to Consider in Designing a Crystallizer

In designing a crystallizer, many important factors must be put into consideration.


The following are the information that must be known before the crystallizer can be
identified.

1. Materials of Construction
2. Method of supersaturation
3. Mode of operation
4. Solubility curve of solution

Crystallizer Design

Design a crystallizer to produce sodium chloride based on the given data:

Production Rate 20 tons/hr


Medium Product Size 400 500 microns
Coefficient of Variation for the Product 20 25 %
Feed Concentration 320 kg/m3
Feed Concentration (w/w) 0.27 kg/kg
Specific heat of feed 3.29 kJ/kg-K
Density of feed 1185 kg/m3
Feed Temperature 20oC
Evaporator entry temperature 55oC
Boiling point elevation 7oC
Additional Undercooling 2oC
Vapor condensation temperature 46oC
Vapor Pressure 10 kPa
Vapor Density 68.7 x 10-3 kg/m3
Latent heat of vaporization 2400 kJ/kg
Steam saturation temperature 66oC
Product slurry concentration 250 kg/m3
Density of crystals 2115 kg/m3
Dynamic viscosity of slurry 23 x 10-4 Pa-s
Specific heat of solid crystals 0.877 kJ/kg-K
Specific heat of slurry 2.7 kJ/kg-K
Density of slurry 1300 kg/m3

Design Description

Crystallizers are used in industry to achieve liquid-solid separation. They are an


important piece of chemical processing equipment because they are capable of
generating high purity products with a relatively low energy input. Nucleation of solutes
inside the crystallizers occurs in response to the formation of the supersaturated
solution. Supersaturated solutions form by evaporation of the solvent in a saturated
solution.

Design Selection

Since the solution is a mixture of water and sodium chloride wherein the solubility
temperature variation is small, it can be separated by evaporative crystallization
(Tavare, N.S.,1994). The crystal size is not controlled, which best suit for the force
circulation evaporative crystallizer. The material of construction used is 316 L stainless
steel which is best suited for sodium chloride.

Data and Assumptions

1. Reynolds number is equal to 5 x 106 (Newman and Bennett, 1959)


2. Overall Heat Transfer Coefficient is 2 kW/m2-K
3. Volume of cone is 40 m3
4. Volume of external loop is 40 m3
5. Inlet and outlet velocity is equal
6. Assume ideal conditions

Design Considerations

1. Height of the vapor space is 0.75 times the diameter of the evaporator body
(Tavare, N. S.)
Parts of Crystallizer

Design Requirements

1. Energy input requirement


2. Circulation rate
3. Diameter of the vessel body
4. Inlet velocity
5. Crystallizer inlet diameter
6. Crystallizer outlet diameter
7. Inlet temperature of the brine
8. Minimum height required
9. Volume of the vessel
10. Total residence time
11. Heat transfer Area

Design Calculations

Mass Balance

=+

( ) ( ) (20 /)(1.3 3 )
= = = 104 /
0.250 /3

20 /
= = = = 74 /
0.27 /

= = + = 104 + 74 = 178 /

Energy input requirement

= ( ) +


= (178 ) (3290 ) (55 20) + 74 /(2400000 )


= 1.98 = 55000

Circulation rate (temperature rise = 4oC)

1.98 /
= =
1300 /3 (2.7 )(4)

= 14100 3 /

Crystallizer Geometry

=

0.68 0.68 (74 ) (1000)
=
( )0.5 0.5
(0.0687 3 ) (3600)

= 7.3

= = 0.75

5 106 (0.0023 )
= =
1300 /3 (7.3 )

= 1.21 /

3
4 4(14100 )
= =
2
2(1.21 )(3600 )

= 1.43

In order to maintain equal velocities in inlets and outlets

= 2 = 2(1.43 )

= 1.69

= 55 + 2 + 4 = 61

At 61oC, the vapor pressure is 20.86 kPa

= = 20.86 10

= 10.86

At = 1300 /3 , the required static head is,

10.86
=
1.300 /3 (9.8067 / 2 )

= 0.85

= + + + = 0.85 + 1.43 + .75(7.3) + 0.5


= 8.25

= (volume of the vessel)



= ( 2 ) ( + + 0.5) + +
4

= [ (7.3)2 ] [0.85 + 1.43 + 0.5] + 40 + 40
4
= 200 3

0 =

200 3 (0.250 3 )
0 = =

20

0 = 2.5

An axial flow pump should be chosen to achieve 141000 m 3/hr.

61 57
= =
66 57
ln ln 66 61

= 8.5

55000
= =
(2 ) (8.5 )
2
= 3235 2

Design Specifications

CRYSTALLIZER
Identification
Number of Unit 1
Material Handled Sodium chloride solution
Residence Time 2.5 hours
Materials of Construction 316L Stainless Steel
Design Data
Energy input 73 756.215 hp
Circulation rate 14 100 m3/hour
Diameter of the vessel body 7.3 m
Crystallizer inlet diameter 1.43 m
Crystallizer outlet diameter 1.69 m
Inlet temperature 61oC
Height of cylinder 8.25 m
Volume of Crystallizer 200 m3
Heat Transfer Area 3235 m3
Auxiliary Parts
Heat exchanger, Condenser
References:

Green, D.W., Perry, R.H., Perrys Chemical Engineers Handbook 8 Th Edition.


McGrawHill Companies. 2008
Tanave, N.S., Industrial Crystallization: Process Simulation Analysis and Design.
(The Plenum Chemical Engineering Series). Springer Science+Business Media,
LLC. 1995
http://encyclopedia.che.engin.umich.edu/Pages/SeparationsChemical/Crystallizer
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