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1081ch8 18 PDF
1081ch8 18 PDF
B. G. LAKATOS (2005)
Product
Feed
Flow sheet symbol
1811
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
(differential pressure or any other type), which gives an indi- occur, producing a large amount of fines and causing build-
cation of the amount of crystals in the crystal slurry, appears up of solids on the walls of the crystallizer.
to be an important instrument. This measurement is based on In general, recirculation rates aim at restricting the flash-
the fact that the density of the clear liquor is constant. Hence, ing at the crystallizer walls or at other boiling surfaces to
the measurement of the differential pressure between two approximately 1.7–4.5°C (3–8°F) whereas a magma-density
points in the vessel is a measure of the amount of crystals in range of 15–25% is typical, even though the exact optimum
the suspension, because any change in density is caused by depends on the particular crystal system.
a change in the amount of crystals in the crystal slurry. 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-
EVAPORATIVE CRYSTALLIZERS 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.
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 FCV-2 valve in a selective manner, they are both provided
it varies the heat input in order to keep the crystal concen- with external feedback (FB) to make sure that their integrals
tration constant. will not wind up when the other controller is manipulating
the valve.
Advanced Controls
Draft-Tube Baffle Crystallizer
Figure 8.18e illustrates how a number of additional features
and flexibilities can be incorporated into the controls of a The draft-tube baffle produces larger crystals than the FC
circulating-magma crystallizer. In this configuration the steam crystallizers under equivalent conditions. It consists of a
flow is measured and controlled on a mass basis (FIC-1) so closed vessel with an inner baffle forming a partitioned set-
that it might be directly related to the feed flow (FIC-2). The tling area, inside which a tapered vertical-draft tube sur-
density of the feed stream is used to estimate the concentra- rounds the agitator, which enters from the top or the bottom.
tion of the solute. It can also be used to signal the need to The agitator is of the axial-flow type and operates at low
increase the steam-to-feed ratio in a feedforward whenever speeds. If additional classification of the crystals is desired,
the solvent content of the feed stream rises, i.e., when it an elutriating leg can be fitted to the bottom cone. The draft
becomes more dilute. The steam-to-feed ratio is trimmed by tube is centered by support vanes to prevent body swirl and
the feedback controller DIC-3 so as to guarantee consistent to minimize turbulence in the circulating magma. Supersat-
product concentration in the crystallizer. uration may be generated by either evaporation, cooling, or
In Figure 8.18e, in order to take full advantage of the vacuum cooling.
surge capacity of the feed tank, its level is not held constant The baffle controls the crystal size by permitting the
but is allowed to float up and down. This level variation separation of unwanted fine crystals. Figure 8.18f shows the
slowly adjusts the steam flow rate (FIC-1), which in turn control of the crystal size distribution in a draft-tube baffle-
changes the feed flow set point, and thereby keeps the feed type crystallizer using fines removal and their dissolution.
tank level within limits.
The lead-lag relay (L/L) provides dynamic compensation Multiple-Effect Operation
for the time constants of the process. The valve position con-
troller (VPC-4) serves to guarantee that the crystallizer will Evaporative crystallizers are often used as multiple-effect
not be starved for steam. Therefore, whenever the steam valve systems, because such configurations improve the product
opening approaches 100%, the low-signal selector on the feed size distribution because of the narrow residence time distri-
valve (FCV-2) blocks the control signal from FIC-2 and allows butions. Different strategies can be employed to improve the
VPC-4 to reduce the feed flow as required to match the avail- product CSD. A successful strategy is, for instance, to permit
ability of the steam. Because VPC-4 and FIC-2 control the nucleation in the first stage and only growth in the subsequent
PRC
PT
M
Vacuum system
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).
FT
Submerged-Combustion Crystallizers Steam Centrifuge
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.
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.
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
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 because of the phase changes and because of the dispersed
the temperature can be controlled by bleeding in air to adjust nature of the crystalline product, strong interactions exist
the pressure. 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-
AUXILIARY EQUIPMENT
step analysis.
Pilot plant studies are often recommended, because
The control requirements of crystallizers are also a function
small variations in the feed liquor compositions can have
of the equipment associated with them. There are four sub-
tremendous influence upon nucleation and crystal growth.
systems whose control should be considered in particular:
Also, minor differences in operating conditions can produce
1. The feed system, including the feed liquor, recycle, and crystals showing significantly different properties. The de-
wash streams. veloper of a control system should take these factors into
2. Vacuum control to maintain predetermined pressure in consideration.
the system as a common means of crystallizer temper-
ature control.
3. Dewatering system control. This includes filters or
centrifuges. Bibliography
4. In the case of external classification equipment, in
Bamford, A. W., Industrial Crystallization, New York: Macmillan, 1966.
order to improve the crystal size distribution of the Mullin, J. W., Crystallization, London: Butterworth & Co., 1972.
product, hydrocyclones, vibrating screens, and other Nyvlt, J., Industrial Crystallization: The Present State of the Art, Wienheim:
external classification devices can be used. Verlag Chemie, 1978.
Perry, R. H., and Chilton, C. H., Chemical Engineering Handbook, New
York: McGraw-Hill.
CONCLUSIONS Randolph, A. D., and Larson, M. A., The Theory of Particulate Processes,
New York: Academic Press, 1988.
In this section some of the common methods of crystallizer Tavare, N. S., Industrial Crystallization. Process Simulation, Analysis, and
Design. New York: Plenum Press, 1995.
control have been outlined. In the crystallization process,