MSMPR Crystalliza-
tion equipment
Department Editor: Scott Jenkins
C
rystallization is a key purification technique
for various sectors of the chemical process
industries (CPI). Several approaches for
industrial crystallization have evolved over time
and highly specialized crystallizer designs have
been developed, especially in long-established
industries. Solution crystallization is an impor-
tant unit operation because the
process can generate high-purity
products from solutions contain- Recirculation
pipe
ing significant levels of impurities
with relatively low energy input.
One scheme for classifying
this equipment is according to
Steam
the method used to suspend the inlet
growing crystals. In this scheme,
a class of equipment known as Heat
mixed-suspension, mixed-prod- exchanger
uct-removal (MSMPR) crystalliz-
ers is most important for the CPI. Condensate
outlet
MSMPR
Circulation
pipe
MSMPR crystallizers, also
known as magma-circulation
crystallizers, have found
widespread application in the
CPI for continuous crystalliza- Forced-circulation (evaporative) crystallizer
tion. In this configuration, a feed
solution is continuously introduced
into the crystallizer, which is equipped with
a mechanism to create supersaturation. An
agitation device allows mixing of the feed
with the contents of the crystallizer and also
maintains a uniform suspension in the mother
liquor inside the crystallizer. A stream of slurry
is continuously removed from the crystallizer in
such a way that the fractions of solid particles
and the particle size distribution in the slurry
inside the equipment equals that of the slurry
removed from the crystallizer.
Examples
Among the group of MSMPR-type crystallizers,
some of the most common are the forced-circu-
lation (FC), draft-tube (DT) and draft-tube-baffle
(DTB) crystallizers.
Forced-circulation crystallizers
This type of MSMPR crystallizer consists of a
body through which a slurry of growing crys-
tals flows, and a tube-and-shell heat exchanger,
which increases temperatures without vaporiza-
tion (diagram, left). Heated slurry returns to the
body via a recirculation line, where it mixes
with the body slurry and raises the temperature
locally, near the point of entry. During the con-
sequent cooling and vaporization to achieve
equilibrium between liquid and vapor, the
supersaturation created causes deposits on the
swirling body of suspended crystals until they
leave again through the circulating pipe. The
lower limit for economic continuous operation
of forced-circulation crystallizers is 1–4 ton/d
of crystals, and the upper limit for a single
vessel is 100–300 ton/d of crystals. Units in
parallel can reach higher capacities.
DTB and DT evaporator-crystallizers
A number of designs have been developed
with circulators located within the body of
the crystallizer in an effort to reduce the head
Cooling
water
Propeller
drive
Cooling Non-condensable
water inlet gas outlet
Air
ejector
Barometric Barometric
condenser condenser
Boiling Body
surface
Skirt baffle
Draft Slurry
Body
tube
Clarified
mother
liquor
Settling Settler
zone
Circulating
Propeller pipe
Source for
Swirl breaker diagrams:
Perry’s Chemical
Circulating pipe Engineers'
Elutriation leg Handbook,
Swenson Process
Equipment
Heating element Steam
Expansion Feed
inlet
joint Product Product
discharge discharge
Feed
inlet
Condensate
Draft-tube-baffle (DTB) crystallizer
against which the circulator must pump. supersaturation by the deposition of solute.
Internal circulators reduce the power input and Crystallizers should operate with a minimum
circulator tip speed, and thereby reduce the 10 wt.% suspended crystals (slurry density)
rate of nucleation, which is influenced signifi- • Contact the supersaturated liquor quickly with
cantly by mechanical circulation. The DTB is an crystals to avoid losses due to time decay
example (diagram, right). In this type, a large, • Destroy excess nuclei via fines destruction
slow-moving propeller is surrounded by a draft configurations. Seeding the crystallizer with
tube within the body that directs the slurry to fines will lower crystal size
the liquid surface to prevent solids from short- • Minimize secondary nucleation by keeping
circuiting the zone of most intense supersatura- mechanical energy input and crystal attrition
tion. Slurry that has been cooled is returned as low as possible
to the bottom of the vessel and recirculated • Maintain high slurry densities. In general,
through the propeller, where heated solution is high densities can produce larger average
mixed with the recirculating slurry. A fines- crystal size as long as crystal attrition is not
destruction feature is common, where a heating a negative influence
element is used to raise the temperature of the • Minimize solids buildup by eliminating local-
solution removed from a settler to destroy the ized heat- and mass-transfer gradients
small crystalline particles that are withdrawn. • Ensure adequate velocities and operation
The baffle can be omitted in cases where fines at low temperature gradients across heat-
destruction is not needed or wanted. exchange equipment
In DT and DTB crystallizers, the circula- • Avoid fluctuations in operating conditions,
tion rate is generally much greater than that such as vacuum, residence time and con-
achieved in a forced circulation device. There- centrations. Employ wash nozzles at liquid
fore, DT and DTB crystallizers are applied interfaces
when it is necessary to circulate large quanti- • Provide a chemical environment (impurities
ties of slurry and minimize supersaturation and additives) that favors the desired crystal
levels within the equipment. These types are shape, purity and size distribution
commonly used in the production of granular • Maintain longer crystal retention times,
materials, such as ammonium sulfate, potas- which can result in less liquor occlusions in
sium chloride and other inorganic and organic the crystals
crystals for which product in the range of 8 to • Keep the feed to the crystallizer slightly
30 mesh is required. unsaturated
Operating Principles References
1. Sutradhar, B.C. Coping with Crystallization Problems.
Basic good-operating principles for solution Chem. Eng., March 2004, pp. 46–52.
crystallization apply regardless of what type 2. S  chweitzer, P.A. “Handbook of Separation Techniques
of crystallization equipment is used. The follow- for Chemical Engineers,” 3rd ed. McGraw-Hill, New
ing represent some of these concepts: York, 1997.
• Control the level of supersaturation to ensure 3. Perry’s Chemical Engineer’s Handbook, 7th ed.
McGraw-Hill, New York, 1997.
low nucleation rates
4. Couper, James. “Chemical Process Equipment:
• Maintain an adequate slurry density to Selection and Design,” Gulf Professional Publishing,
provide sufficient surface area to relieve Houston, 2010.