Crystallization

Equipment
NGO. TlONGCO.
Outline of Report
l. Crystallization: Definition and Industrial Importance
ll. Crystallization Equipment
A. Tank and Batch-Type Crystallizers
l. Agitated Batch Crystallizer
2. Swenson-Walker Crystallizer
3. Wulff-Bock Crystallizer
B. Evaporative Crystallizers
C. Vacuum Crystallizers
Crystallization: Definition and
Industrial Importance

lt is a process whereby a solution is supersaturated so

as to cause the formation of crystals.

lt is the removal of a solute such as a salt from a solution

by precipitating the solute from the solution.

Crystallization is an important operation in the chemical

industry as a method of purification and as a method of
providing crystalline materials in the desired size range.
Crystallization Equipment
Crystallizing equipment can be classified according to the
methods used to bring about supersaturation as follows:
1. Tank and Batch-Type Crystallizers supersaturation is
produced by cooling the solution with negligible evaporation.
. Crystallizin! E"aporators supersaturation is produced by
evaporation of the solvent with little or no cooling.
#. $acuum Crystallizers supersaturation is produced by
combined cooling and evaporation in an adiabatic evaporator.
Tank and
Batch-Type
Crystallizers
Agitated
Batch
Crystallizer
Swenson-
Walker
Crystallizer
Wulff-Bock
Crystallizer
Tank and Batch-Type Crystallizers

These are crystallizers which produce supersaturation by

cooling.

The material must have a solubility that varies greatly

with temperature.

3 types:
!itated Batch Crystallizer

Water is circulated
through the cooling
coils and the solution
is agitated by the
propellers mounted
on the central shaft.

See Figure l8-79,

Perry's HB, 8th ed.
!itated Batch Crystallizer

%&'CTI(') (% T*E +,IT+T(-

l. lt increases the rate of heat transfer and keeps the
temperature of the solution more uniform.
2. lt also keeps the fine crystals in suspension, thus it
gives them an opportunity to grow uniformly instead of
forming large crystals or aggregates.
!itated Batch Crystallizer
+D$+'T+,E)
l. Production of more uniform crystals compared to older tanks.
2. The crystals formed are very much finer than that from the
older tanks.
. DI)+D$+'T+,E)
l. lt is a batch or discontinuous crystallizer.
2. The solubility is the least at the surface of the cooling coils.
Therefore, crystal growth is most rapid at this point and the
coils rapidly build up with a mass of crystals that decreases the
rate of heat transfer.
"#enson-$alker Crystallizer
lt consists of an open
trough with a semicircular
bottom having a cooling
water jacket welded
outside.
lt is about 2 ft wide and l0
ft long.
The hot concentrated
solution to be crystallized is
fed at one end of the trough
and cooling water usually
flows through the jacket in
counter current to the
solution.
"#enson-$alker Crystallizer

A slow-speed spiral agitator, set as close as possible to

the bottom of the trough, rotates and suspends the
growing crystals on turning.
Blades pass close to the wall and break off any
deposits of crystals on the cooled wall.

ln order to control crystal size, it is sometimes

desirable to introduce an extra amount of water into
certain sections in the jacket.
A number of units may be joined together to give
increased capacity.
"#enson-$alker Crystallizer

+D$+'T+,E):
l. Large saving in floor space.
2. Large saving in material in process.
3. Saving in labor.
4. Free from inclusions and aggregations.

DI)+D$+'T+,E):
l. The product generally have a somewhat wide crystal-
size distribution.
$ulff-Bock Crystallizer
lt has similar characteristics
as that of the Swenson-
Walker crystallizer,
however, it depends on air
cooling.
lt consists of a shallow
trough set inclined and
mounted on rollers so that it
can be rocked from side to
side.

The slow rate of cooling in

this crystallizer results in low
capacity but it gives uniform
crystals.
$ulff-Bock Crystallizer

+D$+'T+,E:
lt gives more uniform crystals as compared to Swenson-
Walker Crystallizer.
.
DI)+D$+'T+,E:
The slow rate of cooling in this crystallizer results in low
capacity.
E%aporati%e Crystallizers

These are crystallizers which produce supersaturation by

e"aporation of solvent.

The material must have a solubility that changes little

with (or is independent of) temperature.
&acuum Crystallizers

These are crystallizers which produce supersaturation by

adia.atic e"aporation /ith coolin!.

The method of producing supersaturation in these

crystallizers is the most important one for large-scale
production.

Hot solution is introduced into a vacuum where the

solvent evaporates and the solution is cooled
adiabatically.
'orced Circulation Crystallizer

an "active volume" to get both required residence time for

crystal growth and mother liquor desupersaturation

agitation rate
Control the extent of supersaturation arising from the
evaporation,
Control the temperature difference in the heat exchanger

a special design of the liquid-vapor separation area to

avoid the formation of an excessive amount of fines, which
is highly detrimental to crystal growth.
'orced Circulation Crystallizer

These systems can be either single or multiple effects.

Usually operate from low vacuum to atmosphere pressure.

Used for high evaporation rates and when crystal size is

not of the utmost importance.

Almost any material of construction can be considered for

the fabrication of these crystallizers.

Use vacuum cooling or evaporation method

'orced Circulation Crystallizer
Typical products are:

NaCl (food or technical grade)

KNO3Na2

SO4

K2 SO4

NH4Cl

Na2CO3H2O
Citric acid
Draft Tu(e Baffle )DTB*
Crystallizer

AKA Messo-turbulence

Employ magma recirculation to control supersaturation

generation

Use cooling, vacuum cooling and evaporation

The concept is such that if no (or little) heat make-up is

required, it results in a rather compact arrangement;
therefore the initial investment is minimized

operate with a rather low supersaturation so that very

large coarse and uniform crystals can be produced only by
providing extensive and costly dissolving of fines.
Draft Tu(e Baffle )DTB*
Crystallizer

When destruction of fines

not needed or wanted,
baffles are omitted and the
internal circulation rate is set
to have the minimum
nucleating influence on the
suspension
Draft Tu(e Baffle )DTB*
Crystallizer
Typical products are:

boric acid

Na2SO4. l0H20 (Glauber salt)

melamine

citric acid

NaClO3
Induced Circulation Crystallizer

provide additional agitation of the active volume of forced

circulation crystallizers with the use of only one pump.

operates similarly to a Draft Tube Baffle crystallizer but

without the internal agitation device

main applications are for evaporative crystallization cases

produce a narrow crystal size distribution

can be fabricated in almost any material of construction

limited to non-viscous solutions

Induced Circulation Crystallizer
Typical products are:

NaCl

NH4ClO4

NH4Cl
"urface-cooled )"C* Crystallizer

Same with surface-cooled-baffle (SCB) crystallizers

Use only surface cooling to generate supersaturation

Employ magma recirculation to control supersaturation

generation

Do not provide mechanism for classified product removal

provide a mechanism for fines dissolution when baffle is
present (SCB ONLY)

The heat exchanger surface is the coldest part of the process

and is prone to solids build-up so it is operated such that the
tube-side and shell-side does not exceed 5-l0C
Oslo Type Crystallizer
AKA classified-suspension crystallizer
Oldest design for large, coarse crystals
Design Criteria:
Employ liquor recirculation to control supersaturation generation
Use surface cooling, evaporation or adiabatic evaporative cooling
to generate supersaturation
Provide a built-in mechanism for fines dissolution and classified
product removal.
keeping most of the crystals in suspension without contact by a
stirring device, thus enabling the production of large crystals of
narrow size distribution
Oslo Type Crystallizer

classifying crystallization
chamber is the lower part of
the unit
upper part is the liquor-vapor
separation area

Used for reaction-

crystallization and separation-
crystallization when several
chemical species are involved.
Oslo Type Crystallizer
Usually "close type"
the "open" type is to be considered when very large settling areas are
required or when the vessel must be fabricated out of high cost alloys or
metals.
Oslo Type Crystallizer
Typical products are:

(NH4)2 SO4

Na2SO4

AgNO3

hydrated mono sodium glutamate

mono ammonium phosphate (MAP)

Crystallizer Confi!urations
Crystallizer Comparison
Crystallizer Equipment -ou!h Cost
Estimate
011hi!hest2
Forced Circulation
Crystallizer
4
lnduced Circulation
Crystallizer
2
Draft Tube Baffle (DTB)
Crystallizer
l
Surface-cooled (SC)
Crystallizer
5
Oslo Type Crystallizer 3
Crystallizer
Equipment
+d"anta!es Disad"anta!e
Forced Circulation
Crystallizer
Least expensive type of
crystallizer
Large range of sizes
available
High rate of circulation
reduces particle deposits on
vessel walls
Crystal size difficult to
control
Draft Tube Baffle
(DTB) Crystallizer
Crystal size easy to control
Economic due to
recyclability of fines
More energy efficient than
forced-circulation
crystallizers
Frequent flushings
required to minimize
deposits on the
crystallizer wall
Cannot effectively
handle a high density
slurry
Not easily reproduced
in small scale
Surface-cooled (SC)
Crystallizer
Can handle high boiling
point solution
Can handle solution that has
such low temperature boiling
point that evaporation by
vacuum is not possible
Crystallizer Equipment +d"anta!es Disad"anta!e
Oslo Type Crystallizer operating costs of the
Oslo type crystallizer
unit are much lower
than with any other
type when both large
and coarse crystals
are required
Since crystals are not
in contact with any
agitation device, the
amount of fines to be
destroyed is lower
and so is the
corresponding energy
requirement.
allows long cycles of
production between
washing periods.
Not easily reproduced
in small scale
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Crystallization of
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Forced Circulation Crystallizer

C:\Users\Chong\Documents\PARTECH\Crystallization\gea-wiegand-animation-forced-video.mp4
References
Samant, K.D. & O'Young, L. (2006). Understanding
Crystallization and Crystallizer. Clearwaterbay
Technology, lnc.
http://www.niroinc.com/evaporators_crystallizers/crystalliz
ation.asp

http://www.alaquainc.com/Crystalizers.aspx
http://video.geap.com/video/852l92/gea-wiegand-
animation-forced
http://video.geap.com/channel/4l033l9/crystallization

http://www.slideshare.net/saravanamoorthy/crystallization