Beruflich Dokumente
Kultur Dokumente
Product
Discharge
Active
Volume
Settling
Zone
Feed
Inlet
Vapor
Skirt
Baffle
Draft
Tube
Agitator
Assembly
Elutriation
Liquid
Mother Liquor
with Fines
Fines Dissolution
and Recirculation Loop
Vapor to
Condenser
Steam
Inlet
Condensate
Outlet
Mother Liquor
with Fines
Fresh
Feed
Mother Liquor
with Fines
Fresh
Feed
Vapor to
Condenser/
Vacuum System
Dissolution
Tank
Dissolution
Liquid
Vapor to
Condenser/
Vacuum System
Mother Liquor
with Fines
Fresh
Feed
Refrigerant
Fresh
Feed
Mother Liquor
with Fines
Refrigerant Vapor
to Condenser
a
b
c
d
I Figure 6. Draft-tube-baffle crystallizers (above) can
employ various options(right): (a) evaporation, (b) adia-
batic evaporative cooling with feed addition for fines
dissolution, (c) adiabatic evaporative cooling with a
fines dissolution tank, or (d) direct-contact cooling.
CEP October 2006 www.aiche.org/cep 35
use only surface cooling to generate
supersaturation
provide a mixed suspension as the active
volume for relieving the supersaturation
employ magma recirculation to control
supersaturation generation
do not provide a mechanism for classi-
fied product removal
provide a mechanism for fines dissolu-
tion when a baffle is present (SCB configu-
rations; SC configurations do not provide a
mechanism for fines dissolution).
Figure 7 illustrates a common SCB con-
figuration. It consists of a shell-and-tube
heat exchanger, a vessel with an internal
skirt baffle, and a recirculation pump. The
baffle is positioned so that it acts as a parti-
tion between a settling zone and the active
crystallization volume. The feed inlet is
located on the recirculation pipe just prior
to the recirculation pump. The settling zone
outside the baffle provides an outlet for the
mother liquor. The recirculating magma is
returned to the crystallizer vessel through a
central tube extending into the active crystallization volume.
The operation of this crystallizer corresponds to the
schematic in Figure 4. The desired supersaturation is generat-
ed by cooling the mixed stream formed by the fresh feed and
the recirculating slurry in the tubes of the shell-and-tube heat
exchanger. The heat exchange surface is the coldest part of
the process and is prone to solids build-up. The heat exchang-
er is therefore operated such that the temperature difference
between the tube-side and the shell-side typically does not
exceed 510C.
The recirculation pump and the external recirculation loop
provide the magma recirculation. The recirculation rates are suf-
ficiently high to ensure that the supersaturation generated in the
heat exchanger is low. Returning the recirculating slurry
through a central tube extending into the baffled volume ensures
thorough mixing inside the active crystallization volume.
Fines dissolution in an SCB crystallizer works in much
the same way as in a DTB crystallizer. Astream is continu-
ously drawn off from the top of the settling zone created by
the baffle. This draw-off induces an upward flow into the set-
tling zone. Fines below a certain size (whose free settling rate
is less than the upward flow) stay in this zone and are
removed in the draw-off. The fines are usually dissolved in a
separate dissolution tank and sent back to the crystallizer.
Because the SC configuration does not have a skirt baffle,
it lacks a fines dissolution mechanism. It is similar to the
SCB configuration in all other respects.
Classified-suspension crystallizers
Also known as Oslo crystallizers, classified-suspension
crystallizers:
use surface cooling, evaporation or adiabatic evaporative
cooling to generate supersaturation
provide a classified suspension as the active volume for
relieving the supersaturation
employ liquor recirculation to control supersaturation
generation
provide a built-in mechanism for fines dissolution
provide a built-in mechanism for classified product
removal.
Figure 8a depicts the Oslo configuration that uses evapo-
ration to generate supersaturation. It consists of a suspension
tank and a vaporizer. Recirculation is provided by recircula-
tion piping and a pump. The recirculating liquor is fed to the
vaporizer. Fresh feed is added to the recirculation leg ahead
of the recirculation pump, and the product slurry is taken off
near the bottom of the suspension tank.
When evaporation is used to generate supersaturation, the
recirculating liquor is passed through a shell-and-tube heat
exchanger (as illustrated). When adiabatic evaporative cooling
is used, the heat exchanger is omitted (this version is not
shown). In both mechanisms, evaporation of solvent from the
recirculating liquor entering the vaporizer generates the super-
saturation. The liquor recirculation rate is high enough to ensure
that the supersaturated liquid in the vaporizer stays in the
I Figure 7. A surface-cooled baffle crystallizer uses an external heat-exchange surface to
generate supersaturation by cooling.
Dissolution Tank
Fresh Feed
Coolant
Outlet
Coolant
Inlet
Product
Discharge
Active
Volume
Dissolution
Liquid
Dissolved Fines Recirculation
Recirculation
Pump
Recirculation
Loop
Central
Feed
Tube
Settling
Zone
Cooler
Skirt
Baffle
Mother Liquor
with Fines
36 www.aiche.org/cep October 2006 CEP
metastable zone and remains stable and near the solubility limit.
The liquid from the vaporizer flows down into the suspen-
sion tank through a downcomer that extends to near the bot-
tom of the tank. The suspension tank provides the active
crystallization volume in the form of fluidized classification
of growing crystals. The classification ensures that the super-
saturated liquid coming from the downcomer comes into con-
tact with the larger crystals first. It also ensures that near the
top of the active volume, the liquid is sufficiently clear and
can be withdrawn for liquor recirculation. In some cases, weir
baffles are included to promote liquor recirculation.
These configurations have built-in mechanisms for fines
dissolution and classified product removal. If the liquor
drawn from the top of the suspension tank contains fines, the
addition of heat (in case of evaporation) or feed (in case of
adiabatic evaporative cooling) dissolves the fines. The prod-
uct slurry is taken off near the bottom of the suspension tank.
Classification inside the tank ensures classified product
removal. As a result, additional provisions for fines dissolu-
tion and classified product removal are usually not needed.
Figure 8b shows the Oslo configuration that uses surface
cooling for supersaturation generation. This system also has a
classified suspension tank. However, it uses a shell-and-tube
heat exchanger instead of a vaporizer to generate supersatura-
tion. This is similar to the SCB/SC configurations. However,
unlike the SCB/SC design, it uses liquor recirculation.
In all Oslo configurations, liquor recirculation ensures that
there will be no (or minimal) attrition and crystal breakage.
However, as noted earlier, the ability to maintain a classified
suspension is sensitive to changes in the recirculation rate.
Summing up
Table 2 summarizes the operating mechanisms
employed in the various crystallizer configurations. This
summary, along with the guidance regarding operating
mechanisms provided in Table 1, provides insights for
selecting the appropriate crystallizer design.
These configurations are the most commonly used in
industrial practice. Several other modifications and combi-
nations employing the basic operating mechanisms dis-
cussed here are used for specific applications. Regardless
of the configuration, engineers designing and operating a
continuous crystallizer for a specific application should
pay attention to the following:
The residence time provided for the liquid phase
should be enough to ensure low supersaturation in the
active crystallization volume.
The impact of possible changes to the residence time
due to future changes in operating conditions should be
taken into account.
Changes in operating conditions that may bring about
significant changes in the residence time should be avoided.
The recirculation rate should be high enough to control
the generation of supersaturation. As a rule of thumb: when
surface cooling is used, the temperature drop in the heat
exchanger should be limited to about 12C; when evapora-
tion is used, the temperature increase in the heat exchanger
should be limited to about 15C; and when direct-contact
cooling or adiabatic evaporative cooling is used, the tempera-
ture drop at the vapor-liquid interface should be about 15C.
The recirculation rate should also be compatible
Solid/Liquid Separations
I Figure 8. A classified-suspension, or Oslo, crystallizer can employ (a) evaporation, adiabatic evaporative cooling (not shown), or (b) surface cooling.
Steam
Inlet
Steam
Outlet
Product
Discharge
Fresh
Feed
Recirculation Pump
Vaporizer
Suspension
Tank
Classified Bed
Active Volume
Vapor to
Condenser
Recirculation
Loop
Weir
Baffles
Heat
Exchanger
(omitted
from
systems
using
Adiabatic
Evaporative
Cooling)
a
Suspension
Tank
Classified Bed
Active Volume
Product
Discharge
Recirculation
Loop
Fresh
Feed
Recirculation
Pump
Coolant
Inlet
Coolant
Outlet
Cooler
b
CEP October 2006 www.aiche.org/cep 37
with the degree of mixedness required to sustain the
recirculation type.
When magma recirculation is used, the recirculation
rates and equipment should not cause severe attrition and
crystal breakage.
When liquor recirculation is used, future changes in
operating conditions that may impact the ability to main-
tain a classified suspension should be evaluated.
When liquor recirculation is used, changes in operat-
ing conditions that may lead to mixed suspension and
change to magma recirculation should be avoided.
Both capital and operating costs must be considered
when designing a crystallizer for a particular application.
In general, rankings based on capital costs, from highest to
lowest, are DTB/DT, Oslo, FC, SCB/SC. This is only a
rough rule of thumb, however, as capital costs depend on
the actual design specifications for the application. In gen-
eral, the operating costs for industrial crystallizers domi-
nate the process economics.
The total cost for the crystallizer that gives higher-qual-
ity product and trouble-free operation over a long period
of time is much lower than for a crystallizer that requires
less capital but produces poorer-quality product and
requires frequent maintenance and cleaning.
It is our hope that the descriptions and insights provided
in this article will be useful for chemical engineers dealing
with continuous crystallization-based processes. The discus-
sion here is by no means comprehensive. Additional details
related to crystallization mechanisms, crystallizer design,
operational issues and auxiliary equipment are found
in sources such as Refs. 16.
Literature Cited
1. Bennett, R. C., Crystallizer Selection and Design, in
Handbook of Industrial Crystallization, 2nd edition,
Myerson, A. S., ed., Butterworth-Heinemann, Boston, MA,
pp. 115140 (2002).
2. Mullin, J. W., Crystallization, 4th edition, Elsevier
Butterworth-Heinemann, Boston, MA (2001).
3. Kwok, K. S., et al., Experimental Determination of Solid-
Liquid Equilibrium Phase Diagrams for Crystallization-
Based Process Synhesis, Ind. Eng. Chem. Res., 44, pp.
37883798 (2005).
4. Bamforth, A. W., Industrial Crystallization, The
Macmillan Co., New York, NY (1966).
5. Jancic, S. J., and P. A. M. Grootscholten, Industrial
Crystallization, University Press, Delft, The Netherlands (1984).
6. Wibowo, C., L. OYoung, and K. M. Ng, Streamlining
Crystallization Process Design, Chem. Eng. Progress, 100
(1), pp. 3039 (Jan. 2004).
KETAN D. SAMANT is a senior engineer and founding member at
ClearWaterBay Technology, Inc. (CWB Tech, 20311 Valley Blvd., Suite C,
Walnut, CA 91789; Phone: (909) 595-8928; Fax: (909) 595-8928; E-mail:
ketan@cwbtech.com). He also acts as product manager for SLEEK, CWB
Techs process-development tool for crystallization. In this role, he is
involved in various technology initiatives and consulting projects dealing
with the synthesis, design and operation of crystallizers and
crystallization-based processes. He received a BTech (Honors) from the
Indian Institute of Technology, Kharagpur, and a PhD from the Univ. of
Massachusetts Amherst, both in chemical engineering.
LIONEL OYOUNG is president and co-founder of CWB Tech (E-mail:
lionel@cwbtech.com). He has more than 15 years of experience in process
synthesis and development in the petrochemical, fine chemicals and
pharmaceuticals industries, and he holds patents for various
petrochemical processes. He earned both BS and PhD degrees in
chemical engineering from the Univ. of Manchester Institute of Science
and Technology (UMIST; Manchester, U.K.) and is a member of AIChE.
CEP
Table 2. Commonly used crystallizer configurations.
Forced- Draft-Tube Surface-Cooled
Mechanism Circulation Baffle Draft Tube Baffle Surface-Cooled Oslo
Supersaturation Generation
Cooling Direct-contact Direct-contact Surface Surface Surface
Evaporation
Adiabatic Evaporative Cooling
Relieving the Supersaturation
Mixed Suspension
Classified Suspension
Control of Supersaturation Generation
Magma Recirculation Internal Internal
Liquor Recirculation
Particle-Size Manipulation
Fines Type based on Type based on Internal
Dissolution supersaturation generation supersaturation generation
Classified Product With With With Internal
Removal elutriation leg elutriation leg elutriation leg