8.
18 Crystallizer Controls
C. J. SANTHANAM (1970, 1985) B. G. LIPTÁK
B. G. LAKATOS (2005)
INTRODUCTION
This section describes the control of industrial crystallizers.
Crystallization requires supersaturation, which can be
achieved by cooling, evaporation, vacuum cooling, dilution,
and chemical reaction. The control of multiple-effect crys-
tallizers is also covered.
Crystallization is a widely used technique in the process
industry and is used for the purpose of purification and
separation of substances, as well as for the production of
good-quality crystals. It is a practical method to obtain con-
centrated chemical substances in particulate solid form that
have desirable properties such as good flow characteristics,
handling convenience, suitability for packaging, and pleasant
appearance.
Crystallization can be carried out from solution, vapor,
or melt. Here, only solution crystallization is discussed. The
most commonly used methods for creating supersaturation
in the solution phase include cooling, evaporation, vacuum
cooling, dilution, or chemical reaction. The choice of the
method depends on the solubility of the solute, feed solution
composition, product specifications, and other engineering
considerations.
Most crystallizers in industrial use operate on a continuous
basis, but batch and semibatch crystallizers are also widely
used to produce fine chemicals and special-effect high-added-
value materials such as pharmaceuticals, pigment, agrochem-
icals, or catalysts.
This section is devoted to the subject of controlling basic
continuous crystallizers. It will describe the basic crystalli-
zation techniques, while focusing on the measurement and
control practices used in this industry.
THE CRYSTALLIZATION PROCESS
The fundamental driving force for crystallization is the differ-
ence in chemical potential between the crystallization substance
in the solid and liquid phases, but the common engineering
© 2006 by Béla Lipták
Vacuum
(1995)
Product
Feed
Flow sheet symbol
practice is to use supersaturation as the driving force of
concentration. The crystallization process has three basic
steps: (1) generation of supersaturation, (2) formation of
nuclei, and (3) growth of nuclei into crystals.
Supersaturation is usually expressed as the supersatura-
tion ratio
c
S= 8.18(1)
c′
or the concentration difference
∆c = c − c′ 8.18(2)
where
c = concentration of the crystallizing substance in the
solution
c′ = equilibrium concentration (solubility) of the crystal-
lizing substance in the solution
In most cases, the solubility c′ of a solute increases with
the increase of temperature, but there are a few exceptions
to this rule. The concept of supersolubility and the existence
of the metastable zone are useful in understanding the
behavior of the crystallization process. Figure 8.18a shows
a temperature-solubility plot for a typical salt; the plot is
divided into three zones: (1) stable under saturated zone, where
crystallization is not possible; (2) metastable (supersaturated)
zone between the solubility and supersolubility, where spon-
taneous crystallization is not possible; and (3) labile (super-
saturated) zone, where spontaneous crystallization is probable.
The rate of nucleation and the crystal growth rate are
controlled by supersaturation. The ideal process would be a
stepwise procedure, but nucleation (i.e., formation of new
crystals), because of the secondary nucleation, cannot be
eliminated in a growing mass of crystals. The influence of
supersaturation on nucleation and growth rates is shown in
Figure 8.18b. Whereas the dependence of growth rate on
supersaturation is linear or moderately nonlinear, the nucle-
ation rate increases exponentially with supersaturation.
1811
1812 Control and Optimization of Unit Operations

Concentration by customer specifications. Because very small crystals are

difficult to filtrate, dry, or handle, crystallizer design and
Supersolubility
curve
control usually are directed toward reasonably large crystals
by minimizing nucleation.
B Usual industrial practice involves sufficiently low super-
Labile saturation to minimize supersaturation while being adequate
supersaturated C Solubility for reasonable growth. At the same time, among others in the
zone curve
pharmaceutical industry, there is also an increasing need to
A – Cooling
produce high specific-surface micro particles. Therefore,
A
B – Isothermal because the desirable properties of the crystalline product
Metastable evaporation may change within wide limits, the main purpose is to control
zone C – Vacuum the crystal size distribution.
Stable cooling
The CSD, determined by the rates of nucleation and
undersaturated
zone growth, is influenced by the supersaturation, thus control of
supersaturation becomes the basic element of crystallizer
Temperature
system control. Unfortunately, the workable degree of super-
FIG. 8.18a saturation is usually 0.5–1% so that it is so small that it is
The zones of saturation and solubility plots and the methods by hard to measure directly. Besides, the on-line measurement
which the state of supersaturation can be achieved. of CSD, although it is also possible by laser diffraction, is
restricted to slurries that contain solids at low concentration.
As a consequence, the vast majority of crystallizers use indi-
Figure 8.18b shows three regions of supersaturation, cor- rect means of control.
responding, in principle, to the zones in Figure 8.18a: (1) An important exception to this rule is sugar, in the case
metastable, where nucleation is very low and growth predom- of which the level of supersaturation can be greater than usual
inates; (2) intermediate, where nucleation becomes larger, but in industrial crystallizers, and correlations can be used to
growth is still significant; and (3) labile, where nucleation measure supersaturation directly. Estimations of sugar super-
predominates. solubilities are based on these empirical correlations.
Crystal Size Distribution
Degrees of Freedom
Industrial crystallizers usually yield a crystalline product that
has a wide crystal size distribution (CSD). This CSD affects To define the maximum number of controllers, we consider
the behavior of the product in succeeding operations such as the degrees of freedom for a crystallization system. The vari-
filtration, drying, transport, and storage, and is also defined ables are

1. Temperature and flow of the process fluid

Growth or nucleation rate 2. Temperature and flow of the cooling or heating medium
3. Level of supersaturation
Metastable Intermediate 4. Ratio of mother liquor to crystals, which can be changed
region region by varying recycles of mother liquor to feed stream
Nucleation 5. Removal and dissolution rate of fine crystals
rate
The first principles-based governing equations are

Labile 1. Energy balance equation

region 2. Mass balance equation for the crystallizing substance
3. Balance equation for fines

Growth Because the system has seven variables and three equa-
rate
tions, it has four degrees of freedom. Thus, the maximum
Supersaturation
number of automatic controllers permissible in a crystallizer
Range of system, without overdefining it, is four. The exceptions are
ratio (S)
crystallizer
operation
the dilution and reaction crystallizers, where the flow of the
diluent and ratio of reactants form additional degrees of free-
FIG. 8.18b dom.
The influence of level of supersaturation on nucleation and the The amount of fines can be estimated by using density
crystal growth. measurement. In crystallization operations, the density sensor

© 2006 by Béla Lipták

 8.18 Crystallizer Controls 1813

(differential pressure or any other type), which gives an indi-
cation of the amount of crystals in the crystal slurry, appears
to be an important instrument. This measurement is based on
the fact that the density of the clear liquor is constant. Hence,
the measurement of the differential pressure between two
points in the vessel is a measure of the amount of crystals in
the suspension, because any change in density is caused by
a change in the amount of crystals in the crystal slurry.
EVAPORATIVE CRYSTALLIZERS
occur, producing a large amount of fines and causing build-
up of solids on the walls of the crystallizer.
In general, recirculation rates aim at restricting the flash-
ing at the crystallizer walls or at other boiling surfaces to
approximately 1.7–4.5°C (3–8°F) whereas a magma-density
range of 15–25% is typical, even though the exact optimum
depends on the particular crystal system.
Various designs of crystallizers are available, but the
approaches of controlling the processes are similar. A possi-
ble control system is shown in Figure 8.18c where four con-
trol loops are involved:

This type of crystallizer produces supersaturation and, hence, 1. Feed clear liquor is fed on level control to a feed tank.
crystals, by loss of solvents induced by one of the three Here it is mixed with the mother liquor from the centri-
methods: (1) indirect heating, (2) submerged combustion, and fuge of the crystalline product.
(3) spray evaporation. The first two are the dominant types 2. The mixed liquor is fed to the suction side of the
and will be discussed here. crystallizer recirculating pump. This feed is adjusted
by a level controller. (For methods of protecting the
Indirectly Heated Crystallizers level sensor from plugging and material build-up, refer
to Chapter 3 of the first volume of this handbook.)
Circulating-magma crystallizers with indirect heating are by
3. The steam flow to the heat exchanger is on flow con-
far the most important type of crystallizers in use today: The
trol. Once the steam rate is fixed, the production rate
forced-circulation (FC) and the draft-tube baffle (DTB)
is also fixed, provided that the feed composition does
designs belong to this class.
not change.
A typical FC crystallizer is shown in Figure 8.18c. In
4. Temperature control in the vessel may be achieved by
this design the feed is introduced into the recirculation loop.
controlling the evaporator chamber pressure by an air
The critical design parameters in FC crystallizers are the
bleed.
internal recirculation rate and velocity, the crystallizer hold
volume, and the speed of the circulating pump. At internal
Refinements to this basic system are possible, as an inter-
circulation less than the optimum, excessive flashing can
lock between the steam and circulating pump, or the addition
occur at the boiling surface, causing a high level of super-
of a density recorder. The magma density can also be used
saturation. If this supersaturation cannot be reduced by dep-
for control, rather than just for monitoring. In the control
osition of the solute because of the lack of adequate crystal
configuration shown in Figure 8.18d, the density controller
surface area in the suspension, intensive nucleation will

PRC Vacuum
PRC Vacuum system
system PT
PT Air
Air
LT
LT
Steam
DR PDT
Steam PDT
LIC
FT
LIC SP
FIC DIC
FT
Centrifuge
FRC Centrifuge FSL
Product
FSL Mother
Product
Mother liquor
Feed Feed
liquor
Feed Feed tank
LT LIC
tank
LT LIC
FIG. 8.18d
FIG. 8.18c Cascade control of crystal concentration (measured by density) by
The control of an indirectly heated circulating-magma-type crystallizer. throttling heat input.

© 2006 by Béla Lipták

1814 Control and Optimization of Unit Operations

PRC Vacuum
system
PT
Air

X LT

PDT DIC
FT PT 3
L/L % X
LIC Ratio
Steam SP
FIC VPC < FIC
1 4 2
SP Centrifuge FB FB
FB Product
Mother DT
liquor FT
Feed FC Feed
tank FCV
Non- LT 2
LIC linear

FIG. 8.18e
In this control system, feedforward, dynamic compensation and selective control of the feed are added to the basic controls of a circulating-
magma crystallizer.

serves as the cascade master of the steam flow controller, and
it varies the heat input in order to keep the crystal concen-
tration constant.
Advanced Controls
Figure 8.18e illustrates how a number of additional features
and flexibilities can be incorporated into the controls of a
circulating-magma crystallizer. In this configuration the steam
flow is measured and controlled on a mass basis (FIC-1) so
that it might be directly related to the feed flow (FIC-2). The
density of the feed stream is used to estimate the concentra-
tion of the solute. It can also be used to signal the need to
increase the steam-to-feed ratio in a feedforward whenever
the solvent content of the feed stream rises, i.e., when it
becomes more dilute. The steam-to-feed ratio is trimmed by
the feedback controller DIC-3 so as to guarantee consistent
product concentration in the crystallizer.
In Figure 8.18e, in order to take full advantage of the
surge capacity of the feed tank, its level is not held constant
but is allowed to float up and down. This level variation
slowly adjusts the steam flow rate (FIC-1), which in turn
changes the feed flow set point, and thereby keeps the feed
tank level within limits.
The lead-lag relay (L/L) provides dynamic compensation
for the time constants of the process. The valve position con-
troller (VPC-4) serves to guarantee that the crystallizer will
not be starved for steam. Therefore, whenever the steam valve
opening approaches 100%, the low-signal selector on the feed
valve (FCV-2) blocks the control signal from FIC-2 and allows
VPC-4 to reduce the feed flow as required to match the avail-
ability of the steam. Because VPC-4 and FIC-2 control the
FCV-2 valve in a selective manner, they are both provided
with external feedback (FB) to make sure that their integrals
will not wind up when the other controller is manipulating
the valve.
Draft-Tube Baffle Crystallizer
The draft-tube baffle produces larger crystals than the FC
crystallizers under equivalent conditions. It consists of a
closed vessel with an inner baffle forming a partitioned set-
tling area, inside which a tapered vertical-draft tube sur-
rounds the agitator, which enters from the top or the bottom.
The agitator is of the axial-flow type and operates at low
speeds. If additional classification of the crystals is desired,
an elutriating leg can be fitted to the bottom cone. The draft
tube is centered by support vanes to prevent body swirl and
to minimize turbulence in the circulating magma. Supersat-
uration may be generated by either evaporation, cooling, or
vacuum cooling.
The baffle controls the crystal size by permitting the
separation of unwanted fine crystals. Figure 8.18f shows the
control of the crystal size distribution in a draft-tube baffle-
type crystallizer using fines removal and their dissolution.
Multiple-Effect Operation
Evaporative crystallizers are often used as multiple-effect
systems, because such configurations improve the product
size distribution because of the narrow residence time distri-
butions. Different strategies can be employed to improve the
product CSD. A successful strategy is, for instance, to permit
nucleation in the first stage and only growth in the subsequent

© 2006 by Béla Lipták

 8.18 Crystallizer Controls 1815

PRC
PT

M
Vacuum system

Air FDS – Fines

density sensor
SDS – Slurry
density sensor
LT

Fines removal

TT
FDS
LIC
SDS
Steam
Centrifuge
Fines
FT dissolution Crystalline
FRC product

TIC
FSL Feed
Set point
tank
LT LIC

FIG. 8.18f
The crystal size in a draft-tube-type baffle crystallizer can be controlled by removing and redissolving the fines.

stages. A simplified control scheme on a triple-effect unit is In developing the overall control system, both auxiliaries
shown in Figure 8.18g. and safety interlocks must be included and designed to meet
This complex system has three important features: the requirements of the Fire Insurance Association (FIA).

1. Level in each unit is an important process variable, PIC

because it determines the residence time. Level is usu-
ally controlled by throttling the makeup of the mixed PT Vacuum
Air system
liquor.
2. Steam flow to the first unit is usually on flow control.
3. Feed enters the feed tank on level control, where it is I LT II LT III LT
mixed with the mother liquor from the centrifuge of
the crystalline product. Temperature control in the last LIC LIC LIC
unit is obtained by pressure control of the air bleed. Cond Cond Cond

In these control systems, density recorders can also be used.

If boiling point elevation is sufficiently large, the detected
density can also be used to directly control the effluent liquor
concentration, as was the case in Figure 8.18e.
FRC

FT
Submerged-Combustion Crystallizers Steam Centrifuge

Submerged-combustion crystallizers are used on corrosive Product

Feed
applications or in cases where the salts have inverted solubility.
Feed
One possible control configuration is shown in Figure 8.18h. tank
LT LIC
Here, the clear liquor is fed under flow control, while the
burner fuel gas can be under either flow or pressure control,
in which case a bypass controls the flow of combustion air FIG. 8.18g
to the burner. The basic controls of a three-effect crystallizer.

© 2006 by Béla Lipták

1816 Control and Optimization of Unit Operations

Burner FRC
combustion
Air products FT Coolant
Burner Feed inlet
Fuel Stack

FRC Product M
FT slurry Coolant Product
Feed outlet outlet slurry

FT TIT
FIG. 8.18h
FRC Set point TRC
Submerged combustion-type evaporator crystallizer.

FIG. 8.18j
The controls of a cooling crystallizer that is cooled by a liquid
COOLING CRYSTALLIZERS coolant.

In principle, cooling crystallizers operate at atmospheric

pressure, and their heat is transferred to a cooling medium
or to air by either indirect or direct contact.
There are many types of cooling crystallizers, but the
majority falls into three categories: (1) controlled-growth
magma crystallizers, (2) classifying crystallizers, and (3) direct-
contact crystallizers.
Controlled-Growth Magma Crystallizers
A variety of cradle crystallizers and scraped-surface units
belong to this category. The cradle types are used in small
applications and involve little instrumental control. The var-
ious scraped-surface crystallizers are used in crystallization
from high-viscosity liquors or in open-tank crystallizers, as
coolers to induce nucleation. Two designs of controlled-
growth magma crystallizers and their controls are shown in
Figures 8.18i and 8.18j. In Figure 8.18i an evaporating refrig-
erant cools the shell of the unit, while the crystallization
Vapor
refrigerant
outlet
PIC
Liquid
PT refrigerant
inlet
M LIC
FRC LT
FT Product
Feed
FIG. 8.18i
The basic controls of a refrigerant-cooled crystallizer.
process takes place in the tubes. Usually several scraped-
surface tubes are used in series.
The control system operation is as follows:
1. Clear liquor is fed under flow control. Because the
residence time in the tubes is large and because it is
required in order to obtain the required crystal size, prod-
uct quality-based feedback control from the product out-
let is not practical. Yet, in some applications, feedback
control with dead-time compensation has been applied.
2. In Figure 8.18i, liquid refrigerant enters under level
control and leaves the system as a vapor under pressure
control. In other applications, the refrigerant liquid is
introduced under flow control provided by a metering
pump. Both two- and three-mode controllers have
been used to provide pressure control.
In other cooling crystallizer applications, liquid coolant
is used as the heat transfer fluid. Figure 8.18j illustrates the
control system of such a unit, where the cooling fluid flow
is controlled in cascade by the outlet temperature of the
product slurry.
Classifying Crystallizers
In the Oslo “Krystal” cooling crystallizer the supersaturation
is generated entirely by cooling. In this design the feed is
introduced into a circulating loop, which is also being cooled.
The control configuration for a cooling-type classifying crys-
tallizer is shown in Figure 8.18k.
The functions of the control loops are as follows:
1. Flow control of feed liquor is provided to maintain con-
stant throughput.
2. Flow of coolant is controlled in cascade to maintain
the outlet temperature of the process fluid at the outlet
of the heat exchanger. One refinement is to interlock
the coolant flow with the circulation pump motor.

© 2006 by Béla Lipták

 8.18 Crystallizer Controls 1817

Set fication in a cooling crystallizer. Here, the cooling occurs

FSL point through a jacket under cascade control. The undersize frac-
FRC TRC
tion of crystals leaving the hydrocyclone with the mother
FT
Coolant liquor is returned to the crystallizer. Such operational con-
outlet figuration is very effective to control the size of the crystals,
Overflow but it also has a tendency to cause steady-state oscillation.
TIT
To minimize such oscillations requires more sophisticated
Coolant DR control systems.
inlet LIC Recycle
PDT tank
LT Direct-Contact Crystallizers
M LT
FRC Product to LIC In such units, the coolant is an evaporating refrigerant or
centrifuge brine, and it is in direct contact with the process slurry. Basic
FT control methods are similar to those in controlled-growth
Mother
Feed liquor Mother crystallizers (Figure 8.18i). These involve constant feed rate
liquor and flow controls of the evaporating refrigerant, based on
process fluid outlet temperature or on tank level.
FIG. 8.18k
The controls of a classifying crystallizer with external circulation
for cooling.
VACUUM CRYSTALLIZERS
3. Overflow from the crystallizer is on level control. Dif-
ferential pressure-type level measurement is accept- In vacuum crystallizers, heat input to produce adiabatic evap-
able for this application. oration comes entirely from the sensible heat of the feed liquor
4. Mother liquor outflow from the recycle vessel is on and from the heat of crystallization of the crystalline product.
level control. Thus, supersaturation is generated by a combination of cool-
ing and concentrating the liquor. The forced-circulation and
Figure 8.18l illustrates a design that improves the crystal draft-tube baffle crystallizer designs are both used in this
size distribution of the product by providing external classi- operation mode.

PRC
PT

M
Vacuum
Air system
TT
LT
Set point
TIC
Coolant
outlet

TIC TT
LIC

Coolant
inlet
Hydrocyclon

Product
slurry

Feed Feed
tank
LT LIC

FIG. 8.18l
The controls of a jacketed cooling crystallizer with classified product removal.

© 2006 by Béla Lipták

1818 Control and Optimization of Unit Operations

PIC the coolant outlet. This vacuum indirectly controls the process
PT temperature.
The control system consists of (1) feed flow control, (2)
Steam product removal control based on level measurement, and (3)
M
temperature control accomplished indirectly by manipulation
Water of jacket coolant. Use of suspension density recorder and
other refinements can also be used.
LT
TIC REACTION CRYSTALLIZERS

TT
In reaction crystallizers, crystallization is associated with a
chemical reaction that usually produces the solute directly.
LIC Sump
Chemical reactions between two components, however, may
also produce some diluents, in turn causing “salting-out.” In
a reaction crystallizer, once the reaction mixture is saturated
with respect to the crystallizing substance, the reaction rate
would determine the rate of supersaturation. In some cases,
Centrifuge
the heat of exothermic reaction may be used in evaporating
the solvent, thereby producing additional supersaturation dur-
Product
ing the course crystallization.
A control configuration for a reaction crystallizer is shown
Feed Feed
tank
in Figure 8.18o, where one of the reactants is fed into the
LT FT crystallizer in the gaseous phase while the second reactant is
fed in the form of aqueous solution. Here, the aqueous solu-
FIG. 8.18m tion feed is on flow control, the total liquid feed is on level
Draft-tube-type baffle crystallizer, provided with vacuum control control, while the gaseous reactant is added on pH-cascaded
and mother liquor recirculation. control. The pH metering lines should be continuously
flushed when this system is used.
In the case when both reactants A and B are liquids, they
The control strategy for a draft-tube baffle crystallizer can be charged into the crystallizer under ratio control to
with vacuum cooling is shown in Figure 8.18m. Here, the maintain either the stoichiometric or any other predetermined
vacuum is on control with steam jet ejector. Air bleed is on ratio of these reactants. As shown in Figure 8.18p, the total
pressure control, and both the steam and water supplies are
on automatic control, which allows achieving the minimum
Vacuum
cost of utilities. system
Another control configuration is shown in Figure 8.18n. PRC
pHRC
Here, the vacuum in the crystallizer is maintained by throttling PT
pHIT Air
Set
point
Vacuum
FRC pHE
system
FRC
PT FRC Sparger LT
FT
PRC M FT
FT Water
Coolant Feed Gaseous
outlet ammonia
FRC
LIC
Coolant FT Aqueous
inlet LIC Crystal acid
Product magma to
LT slurry dewatering
Feed
outlet
tank

FIG. 8.18n FIG. 8.18o

Draft-tube baffle crystallizer with combination of cooling and vac- The controls of a reaction crystallizer that is utilizing both gaseous
uum control. and liquid reactants.

© 2006 by Béla Lipták

 8.18 Crystallizer Controls 1819

PRC PT
Vacuum system

Air

LT

FFIC
PDT
SP

FT

Product
% FT
slurry to
filtration
B species Ratio SP
LIC
Feed
tank
LIC LT
Feed A Species
tank LIC
LT

FIG. 8.18p
Reaction crystallizer controls provide ratio control of the reactants A and B.

flow into the reactor crystallizer can be on level control and
the temperature can be controlled by bleeding in air to adjust
the pressure.
AUXILIARY EQUIPMENT
The control requirements of crystallizers are also a function
of the equipment associated with them. There are four sub-
systems whose control should be considered in particular:
1. The feed system, including the feed liquor, recycle, and
wash streams.
2. Vacuum control to maintain predetermined pressure in
the system as a common means of crystallizer temper-
ature control.
3. Dewatering system control. This includes filters or
centrifuges.
4. In the case of external classification equipment, in
order to improve the crystal size distribution of the
product, hydrocyclones, vibrating screens, and other
external classification devices can be used.
CONCLUSIONS
In this section some of the common methods of crystallizer
control have been outlined. In the crystallization process,
because of the phase changes and because of the dispersed
nature of the crystalline product, strong interactions exist
between the process variables. Because of the complex,
multiple-input/multiple-output nature of this process, the
control system development should be based on a step-by-
step analysis.
Pilot plant studies are often recommended, because
small variations in the feed liquor compositions can have
tremendous influence upon nucleation and crystal growth.
Also, minor differences in operating conditions can produce
crystals showing significantly different properties. The de-
veloper of a control system should take these factors into
consideration.
Bibliography
Bamford, A. W., Industrial Crystallization, New York: Macmillan, 1966.
Mullin, J. W., Crystallization, London: Butterworth & Co., 1972.
Nyvlt, J., Industrial Crystallization: The Present State of the Art, Wienheim:
Verlag Chemie, 1978.
Perry, R. H., and Chilton, C. H., Chemical Engineering Handbook, New
York: McGraw-Hill.
Randolph, A. D., and Larson, M. A., The Theory of Particulate Processes,
New York: Academic Press, 1988.
Tavare, N. S., Industrial Crystallization. Process Simulation, Analysis, and
Design. New York: Plenum Press, 1995.

© 2006 by Béla Lipták