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EVAPORATION AND CRYSTALLIZATION Forced circulation evaporator

EVAPORATION  In these evaporator, the evaporating liquid is pumped


through a heat exchanger where the heating medium
Evaporation is the operation of concentrating a solution of boiling surrounds the tubes carrying the solution.
away the solvent. It consist of a heat exchanger capable of boiling  Pressure drop and hydrostatic head in combination are
the solution and a device to separate the vapour phase from the frequently great enough to prevent the solution from
boiling liquid. boiling the exchanger so that the vapour generated is
flashed off as the liquid enters the disengaging space.
Usually the desired product is the concentrated solution, but Since the flashing velocity is too high, impingement baffles
occasionally the evaporated solvent is the primary product – for are important to minimize entrainment.
example in the evaporation of seawater to make fresh water or  Heat transfer coefficient will depend upon circulation rate
evaporation of mineral bearing water to produce boiler feed water as well as over-all ∆T, boiling temperature, and system
(often called water distillation) properties.
 Advantage : Suitable for scaling solutions because of
It differs with other unit operations in such a way that:
turbulence, high velocity rate and high recirculation rate
 Distillation: in evaporation vapor is usually a single  Disadvantage : high pumping cost. Thus the decision to use
component this type of evaporator depends upon a favourable
economic balance that includes evaporator first cost, the
 Drying: in evaporation, residue is liquid, sometimes a
power cost and maintenance cost of the pump and
highly viscous one rather than a solid
cleaning cost of the tubes
 Crystallization: focus is on concentrating a solution rather
than forming crystals
Long tube vertical evaporator
Types of evaporator. See Perry Page 11-110 for more info:
 A natural circulation evaporator like horizontal and vertical
Horizontal-tube evaporator
type types
 The solution to be evaporated boils outside of horizontal  Essential parts are (1) a tubular exchanger with steam in a
tubes within which steam condenses. shell and liquid to be concentrated in the tubes (2) a
 The horizontal tubes interfere with the natural circulation separator or vapour space for removing the entrained
of the boiling liquid and thus minimize liquid agitation. As liquid from vapour (3) when operated as a circulation unit
a result, the over-all heat transfer coefficient (OHTC) is a return leg for the liquid from the separator to the
lower than in any form of evaporator, especially if the bottom of the exchanger
solution is viscous. Thus, it is not recommended to use this  Competes most favourably against forced circulation
type of evaporator for viscous fluids evaporator
 Disadvantage : Fouling from the evaporating solution  Although the OHTC is lower than the forced type, it
builds up on the outside of the tube. however requires no pump. Moreover, the fraction
 Application : For small installations, for dilute solutions evaporated per pass is usually larger than the forced type.
that do not foam nor deposit solids on the evaporator  It cannot handle viscous fluids, but it can handle foaming
tubes. materials and some heat sensitive solutions

Vertical tube evaporator Once through falling film evaporator:

 The solution boils inside the vertical tube with the heating  Once-through evaporators like this one is Ideal for most
medium, usually condensing steam, held in chest through heat sensitive solutions.
which the tube pass.  In this unit, the fluid is fed at the top of a long vertical
 Natural circulation is promoted having been measured rather than large diameter tubes (2-4’’) so that the fluid
between 1 to 3 ft/s. As a result, coefficients are somewhat flows down the tube walls in parallel with the flow of the
higher than horizontal tube evaporators. evaporated gas. The result is short contact time with the
 Any deposit that will build up inside the tube will be possibility of large fraction evaporation.
readily removed by mechanical cleaning:  The greatest challenge in this type is how to maintain the
 Completely satisfactory for most evaporation demands even distribution of fluids in the tubes. This can be
and are impractical to liquids that are viscous and foams overcome by using (1) levelled weirs , (2) perforated metal
markedly plates above the levelled tube sheet ,or (3) by spider
distributors with radial arms from which the feed is
sprayed at a steady rate inside the tube. Another way is to
spraying the fluid directly on the tube walls via spray
nozzle.

Agitated film evaporator

 A modified falling film evaporator with a single jacketed


tube containing an internal agitator
 Advantage : Suitable for giving high rates of heat transfer
with viscous fluids. Suitable also for heat sensitive
products such as gelatin, rubber latex, antibiotics and fruit
juices.
 Disadvantage : Maintenance of internal moving parts;
Mass Balance
Small capacity
OMB : F = V + P
Turbulent film evaporator
CB : Fxf = Pxp
Capacity = No of water evaporated per hour
 Applicable for handling both viscous and corrosive Steam economy = V/S
solutions. Can be used also for evaporating slurry to
dryness. Energy Balance :
 The unit is consist of a vertical tube heated over the
bottom two thirds with the steam jacket and containing First case:
S (hs – hc) = Php + VHv – Fhf
central rotor. Mounted on the rotor are blades extending
(applicable if the enthalpy-conc. diagram is available)
almost to the heated walls, The top third of the cylinder is
hs = enthalpy of steam
of larger diameter and is unheated hc = enthalpy of condensate
 Advantage : low residence time and low hold-up Reminder: If the steam and condensate are at the same temperature
hc – hs = λs (heat of condensation)
Submerged combustion burner
Second case:
 Applicable for handling both viscous and corrosive S (hs – hc) = Pcp (TP – T0) + VHv – FcpF (TF - T0)
solutions. applicable if the specific heat capacites of feed,cpf and concentrated
 With this burner, no metal heat transfer surface is liquor, cpL are given
required since the product of combustion bubbled up Reminder: If the problem only provides cp for feed and does not
indicate heat capacity of the concentrated product , we have no
through the process fluid.
choice but to assume that the given heat capacity of the feed will not
 Advantage : simple design reduce replacement cost to be affected by the changes in concentration, thus cpF = cpL. (This
minimum assumption is rough approximation because in reality, cp is directly
affected by the amount of solute present)
Evaporators according to number of effects
Heat Transfer Equation
A. Single Effect Evaporators – used when the required capacity of
operation is relatively small and/or cost of steam is relatively Q = UA(Ts-T1)
cheap compared to the evaporator cost. Vapor from single U = Over-all heat transfer coefficient based on area A
effect is usually condensed and discarded. Ts = steam inlet tem
T1 = operating temp inside the vessel
Ts-T1 = ∆T temperature drop
Heat and Material balance
In most cases, the controlling resistance comes from the boiling
liquid inside, thus OHTC will depend largely on the heat transfer
coefficient of the condensing steam outside thus, U will be
evaluated based on outside area (i.e Uo). This over-all heat transfer
coefficient depends upon: properties of solution, the heating
medium , surface geometry and the method of operation

The heat transfer coefficient of the boiling liquid depends primarily


on the velocity of the liquid over the heated surface.

The temperature drop, ∆T depends on the ff


 Solution being evaporated,
 difference in pressure between the steam chest and the
vapour space above the boiling liquid,
 depth of the liquid inside the evaporator
 and the velocity of liquid inside the tube (i.e frictional loss 5. **A single effect evaporator is being used to concentrate a feed
increases the effective pressure in the liquid of 10000lb/h of a cane sugar solution at 800F and containing a
 For multiple effect evaporator, the liquid head (pressure) sugar content of 150Brix to 300Brix for use in a food process.
and the boiling point elevation reduces the pressure drop Saturated steam at 2400F is available for heating. The vapour
space in the evaporator will be at at 1 atm abs pressure. The
Boiling point Elevation (BPE) –
Increased in boiling point of a solution above the boiling point of overall U = 350 BTU/h/ft2/F0 and the heat capacity of the feed
water at the prevailing temperature. BPE can be estimated using is 0.91 BTU/lb/F. The BPR can be estimated from BPR, 0F = 3.2x
Figure 11-124 (CHE HB 8th edition) + 11.2x2 where x is wt fraction of sugar sol’n. The heat of sol’n
can be considered negligible and neglected. Calculate the
BPE is insensitive to pressure. This generalization was first described required area. (Ans 676 ft2)
by by Duhring in 1878
Trivia: degree Brix is the percent by mass of soluble matter in
Duhring rule : The Boiling point of a solution is a linear function of sugar sol’n
the boiling point of pure water at the same pressure
6. **A forced-circulation evaporator is to concentrate 60,000 kg/h
of 44 percent NaOH to 65 percent using steam at 3 atm
PROBLEMS
pressure. The feed temperature and the condensing
1. A single effect evaporator concentrates 1 MT of 10% wt sucrose temperature are both 40°C. The density of the feed solution is
solution to 50%. The feed enters the evaporator at 20°C and 1,450 kg/m3. If the over-all heat transfer coefficient is 2,000
has a specific heat of 1.0. The evaporator is maintained at a W/m2·°C, calculate (a) the steam requirement, in kg/h (30,525
vacuum of 600 mm Hg against a barometric reading of 760 mm kg/h); (b) the heat transfer area required (283.64m2).
Hg. The heat is provided by saturated steam at 8.8 kg/cm2
gage. Assuming that no sensible heat is recovered in the
7. **A 10% wt NaOH at 80 °F is to be concentrated in a single
evaporator, calculate the weight of heating steam, in kg, effect evaporator to 40% wt. Steam is supplied at 20 psig and
needed for concentrating the sucrose solution. the vacuum pressure of the barometric condenser is 26 in Hg.
100 gpm of water is fed to the condenser and the water leaving
the condenser (including the condensate) is at 100 °F. OHTC of
2. ** A solution of organic colloids is to be concentrated from 20 evaporator is 200 BTU/h·ft2·°F. Calculate the heating surface
to 65% wt solids in an evaporator. Saturated steam is available required for the evaporator. (Ans 88.83 ft2)
at 172 kPa absolute and the pressure in the condenser is 30cm Hint: The vapour condenser operates at isobaric condition.
Hg vacuum. The feed enters at 25°C and its specific heat is 4.0
J/g·°C. The solution has a negligible elevation in boiling point.
B. Multiple Effect Evaporator
OHTC is 1,000 W/m2·°C and the evaporator must evaporate
9,000 kg/h. a) Determine the steam consumption, kg/h
In any evaporation operation, the steam consumed is the
(10759.3 kg/h) b) How many square meters of heating surface
major process cost. Thus methods of increasing steam economy
are required? (126.08 m2) c) What is the steam economy? (Ans
is very attractive. The most common technique is to feed the
0.84)
vapour generated from the first evaporator into a second unit,
then feeding the vapour coming out from the second unit to
3. ** A feed of 4,535 kg/h of a 2.0 % wt salt solution at 311 K
the third and so on; thus increasing the “effects” of steam fed
enters continuously a single effect evaporator and is being
to the first unit.
concentrated to 3%. The evaporation is at atmospheric
pressure and the area of the evaporator is 69.7 m2. Saturated
The major objective of increasing the number of units in series
steam at 383.2 K is supplied for heating. Since the solution is
is to obtain a number of pounds of vapour for each pound of
dilute, it can be assumed to have the same boiling point as
steam consumed equal to the number of evaporating bodies.
water. The heat capacity of the feed can be taken as Cp = 4.10
kJ/kg·K. Calculate the amounts of vapor and liquid product and
Thus, multiple effects evaporator (with no BPE) using n effects
the over-all heat transfer coefficient.. Ans (P = 3023.33kg/h; V
increases the steam economy but decreases the heat flux by
=1511.67kg/h, U = 1785.53 W/m2-K
about 1/n relative to the single effect under the same terminal
conditions. (e,g the capacity of a double effect evaporator
4. Determine the heating area required for the production of
concentrating a solution w/o BPE is equal to ½ capacity of two
10,000lb/h of 50% NaOH solution from a 10% feed entering at
single effects)
1000F. Evaporation is to be carried out in a single-body standard
evaporator for which an over-all coefficient of 500 is expected.
If the solution being evaporated has a significant BPE, the BPE
Steam is available at 50psig and the evaporator can be
reduces ∆T in each effect resulting to a very much reduced
operated at 50psig, and the evaporator can be operated at
capacity . (e,g the capacity of a double effect evaporator
10psi vacuum relative to a barometric pressure of 14.7 psia
concentrating a solution w/ BPE is less than ½ the capacity of
two single effects).
B.3. Parallel Feed Multiple Effect Evaporators – involves the
No matter how many effects are used, provided that OHTC’s in adding of fresh feed and the withdrawal of concentrated
each effect are the same, the capacity will be no greater that product from each effect. The vapor from each effect is still
that of a single effect having an area equal that of each effect in used to heat the next effect. This method is used mainly when
the multiple unit. the feed is almost saturated and solid crystals are the product,
as in the evaporation of brine to make salt.
Economics:
The cost of each effect of an evaporator per square meter or
square foot is a function of its total area and decreases with B.4. Mixed Feed Multiple Effect Evaporators – fresh feed enters
area approaching an asymptote for very large installation. any of the available effects and continues not necessarily to the
Investment required for an N effect is about N times that for a effect next to it.
single effect of the same capacity
Problems
B.1. Forward Feed Multiple Effect Evaporators – fresh feed is
1. A triple effect evaporator is supplied with saturated steam at
added to the first effect and flows to the next in the same
2500F. The temperature in the last effect is 1500F. The OHTC’s
direction as the vapor flow. This is used when the feed is hot or
are 150, 200, and 250 in the 1st, 2nd and 3rd effects
when the final concentrated product might be damaged at high
respectively. If the total BPR in the 3 effects is 550F, the area of
temperatures
the first effect in sq feet is ____ if the steam used is 10000lb/h.

Advantage : No pump is required to transfer liquids between


2. **A liquid with no appreciable elevation of boiling-point is
each effects since the pressure in each effect is lower than that
concentrated in a triple-effect evaporator. If the temperature of
in the previous effect.
the steam to the first effect is 395 K and vacuum is applied to
Disadvantage : If the feed is cold, much of the heating capacity
the third effect so that the boiling-point is 325 K, what are the
of the medium will be spent resulting in lower economy
approximate boiling-points in the three effects? The overall
transfer coefficients may be taken as 3.1, 2.3, and 1.1 kW/m2 K
in the three effects respectively. Ans. 381.5K, 363.2K, 325K

C. Vapor Recompression

In multiple effect evaporator, temperature drop is generated by


lowering the BP of the solution in a series of evaporators through
the use of lower absolute pressure. In vapour recompression, ∆T can
be enhanced by increasing the pressure (and therefore increasing
the condensing temperature)of the evolved vapour. The compressed
vapour is then fed back into steam chest of an appropriate
evaporator effect.
B.2. Backward Feed Multiple Effect Evaporators – fresh feed
enters the last and coldest effect and continues until the Vapor recompression can be done through the use of centrifugal or
concentrated product leaves the first effect. This is used when positive displacement compressor (called mechanical
the fresh feed is cold. This type of evaporation would requires recompression) or through steam jet injection(also called thermal
liquid pump for between each effect since flow is from low to compression).
high pressure
Application of mechanical recompression:

Advantage: Higher capacity than forward feed when thick liquor


 Water distillation
is viscous
 Evaporation of black liquor in the paper industry
 Evaporation of heat sensitive materials
Disadvantage; Lower economy than the forward feed when the
 Crystallisation of salts having inverted solubility curves
feed liquor is cold
Disadvantages of vapor recompression:

 The compressor is expensive and subject to higher


maintenance cost .
 In reasonable operating ranges, ∆T obtained is small about -
100F. As a result the evaporating equipment must be large
for a reasonable high production rate.
 Recompression evaporator requires auxiliary equipment
(steam traps, entrainment separators, etc.)
 If the solution has a large BPR, the cost of recompression B. Equilibrium
increases rapidly because the vapour must be compressed
Equilibrium in crystallization is reached when the solution is
to such pressure that is saturation tempeature is above the
saturated and the equilibrium relationship for bulk crystals is the
the temperature at which the solution boils.
solubility curve. In many industrial crystallization processes, the
In US , vapour recompression is unattractive because fuel cost is low crystal and the mother liquor contact long enough to reach
but electrical power is expensive. Vapor recompression on the other equilibrium, and the mother liquor is saturated at the final
hand is more feasible in Europe where fuel supply is scarce and yet temperature of the process.
the presence of several hydroelectric stations makes the power cost
When the rate of crystal growth is slow, considerable time is
relatively cheap
required to reach equilibrium. This is especially true when the sol’n
is viscous or when the little crystal surface is exposed to the super-
CRYSTALLIZATION
saturation solution. In such situation, the final mother liquor may
Refers to a solid-liquid separation process in which solid particles are retain appreciable supersaturation and the actual yield will be less
formed within a homogenous phase. ] than that calculated from the solubility curve

In crystallisation, the two phase mixture of mother liquor and Types of Solubility Curves
crystals of all sizes which occupies the crystallizer and is withdrawn
(1) Type 1 – Solubility increases with temperature, and there
as product is called magma.
are no hydrates or water of crystallisation
Crystallisation habit is strongly affected by the degree of (2) TYPE II: Solubility increases with temperature but curve is
supersaturation, the agitation intensity, size of crystals in the marked with extreme flatness.e.g NaCl
environment and purity of the solution (3) TYPE III: Solubility increasing fairly rapid with temperature
but is characterized by “breaks” and indicates different
Crystal Size Distribution (CSD) – it is the prime and major objective in “hydrates” or water of crystallization e.g NaHPO4
the design and operation of crystallizers. Other factors that influence (4) TYPE IV: Unusual Curve; Solubility increases at a certain
the design of crystallizer are crystal habit (mentioned before) and transition point while the solubility of the hydrate
the produce salability. decreases as temperature increases e.g Na2CO3

A. Crystal Geometry Some have inverted curve which means that their solubility
decreases with increasing temperature. Such crystals are called
A crystal is highly organized type of matter, the constituent particles invariant . Examples include MnSO4.7H2O, and CaSO4
of which are arranged in an orderly and repetitive manner; they are
arranged in orderly three dimensional arrays called SPACE LATTICES C. Heat and Mass Balance

Under ideal conditions, a growing crystal maintains a fixed


polyhedron face during growth. Such crystal is called invariant

Types of Crystal Geometry

(1) CUBIC SYSTEM – 3 equal axes at right angles to each other


(2) TETRAGONAL – 3 axes at right angles to each other, one axis
longer than the other 2
(3) ORTHOROMBIC – 3 axes at right angles to each other, all of
different lengths
(4) HEXAGONAL – 3 equal axes in one plane at 60° to each other, and
a fourth axis at a right angle to this plane and not necessarily at the
same length
(5) MONOCLINIC – 3 unequal axes, two at a right angles in a plane,
and a third at some angle to this plane
(6) TRICLINIC – 3 unequal axes at unequal angles to each other and
not 30°, 60°, or 90°
(7) TRIGONAL – 3 unequal and equally inclined axes

A given material may crystallize in two or more different classes


depending on the conditions of the crystallization. Calcium
carbonate occurs naturally in hexagonal form (calcite) but also
occurs in orthorhombic (aragonite)
crystallization by simultaneous cooling and evaporation of
the solvent
(4) REACTION / PRECIPITATION – by chemical reaction with
a third substance that will form an insoluble precipitate.
(5) SALTING – by the addition of a third component. The
third component may act physically by forming with the
original solvent, a mixed solvent in which the solubility of
OMB : F = L + C the solvent is sharply reduced.
CB: FXF = LXL + CXC (6) Combination of evaporation and cooling – Applicable for
sodium nitrate soln.
Heat Balance:
Fhf + q = LhL + Chc
For rough approximation, if the data for feed and liquor enthalpies
D.1 Primary Nucleation
are not available and assuming that specific heat capacity will not
vary with temperature (cpf = cpL) then the equation above can be  The rate of nucleation is the number of new particles
written as: formed per unit time per unit volume of magma or solids
free mother liquor. This quantity is the first kinetic
-q = Fcpf (tF – tL) + Chc
parameter controlling the CSD. Two types of nucleation
are possible : homogenous and heterogenous
 Homogenous nucleation is defined as the consequence of
rapid local fluctuations on a molecular scale in a
homogenous phase that is in the state of metastable
equilibrium, It is the formation of phase uninfluenced by
any foreign substance.
 Steps in homogenous nucleation:
Heat Balance for Crystallizers with Evaporated Water
Fhf + q = Lhl + Chc +Vhv o Particles associate randomly to form cluster ( a
For adiabatic crystlaiizer (Vacuum crystallizer), q = 0 loose aggregation which usually disappears quickly)
For rough approximation o Association of cluster form embryo, in which there
-q = Fcpf (tF – tL) + Chc – VλV are a beginning of the lattice arrangement and
Where λV is the heat of vaporization evaluated at product temp formation of new crystal face. Embryos are short
λV = saturated Hvap – saturated Hliq
lived and can revert back to clusters because the
concentration gradient favors transfer from
D. Crystal Formation embryo.
 Crystal formation requires two steps. The first step is o If supersaturation is large, embryo can grow to a
nucleation and the second one is crystal growth. The driving size that is in thermodynamic equilibrium with the
potential for both stages is supersaturation solution known as nucleus
 Supersaturation is a measure of the quantity of solids o Nucleus are smallest assemblage of particles that
actually present in solution as compared to the quantity will not redissolve and therefore grow to form
that is in equilibrium with the solution. Mathematically, S = crystal
(part of solute/100 parts solvent) / (part of solute at  Heterogenous nucleation occurs when solid particles of
equilibrium/100 parts solvent) foreign origin influence the nucleation process by
 Extent of supersaturation depends upon the number and catalysing an increase of nucleation rate at a given
shape of crystals upon which precipitation occurs, supersaturation or giving a finite rate at a supersaturation
temperature level, sol’n concentration and the violence of where homogenous nucleation would occur only after a
agitation vast time
 Crystallization cannot occur without supersaturation. There
D.2 Secondary Nucleation
are 5 basic methods of generating supersaturation
 Defined as the formation of nuclei attributable to the
(1) EVAPORATION – by evaporating a portion of the solvent; influence of the existing macroscopic crystals in the
applicable for solutions whose solubility is independent of magma. Two kinds are known : Fluid shear and Contact
temperature like NaCl. nucleation
(2) COOLING – by cooling a solution through indirect heat  When supersaturated solution moves past the surface of
exchange, applicable for solutions whose solubility the growing crystal at a substantial velocity, the shear
increases with temperature like potassium nitrate, sodium stress in the boundary layer may sweep embryos or nuclei
sulphite and majority of all known salts. that would otherwise be incorporated into the growing
(3) VACUUM COOLING – by flashing of feed solution crystal and so appear as new crystal
adiabatically to a lower temperature and inducing
 Contact nucleation is the most common type in industrial 𝑊𝑝
∫0
𝑊𝑠
𝑑𝑊𝑝 = ∫0 (1 +
∆𝐷
)^3 𝑑𝑊𝑠
𝐷𝑠
setup and is influenced by the intensity of agitation caused
by impeller or internal moving devices. It occurs at low C = Wp – Ws
supersaturation and proportional to the first power of
supersaturation instead of the 20th or greater power for
primary nucleation.
 Relationship of Nuclei, N to supersaturation, S and Energy G. Crytallization Equipment
of impact, E
o For inorganic crystal, the number of nuclei per
G.1 Supersaturation By Cooling
contact N is proportional to S
o For most organic and hydrated inorganic crystals, N Applicable for substance that have solubility curve that increases
is propostional to E with temperature (i.e steep solubility-temperature curve);
o For some organic crystals, lnN is proportional to E
o For anhydrous inorganic crystals, the energy Pan Crystallizers - Batch operation; seldom used in modern
required is larger than for other crystals and practice, except in small scale operations, because they are wasteful
threshold energy is required for nucleation. N is of floor space and of labor; usually give a low quality product
proportional to exp (E )
Agitated batch Crystallizers - Consist of an agitated tank; usually
E. Crystal growth Theories cone-bottomed, containing cooling coils. It is convenient in small
 Surface growth is based on the concept that growth occurs scale or batch operations because of their low capital costs,
layer by layer as a two dimensional nucleus attached to simplicity of operation and flexibility
the face. This theory predicts that growth does not start
Swenson Walker Crystallizer - A continuous crystallizer consist of an
until appreciable threshold supersaturation is reached and
open round bottomed-trough, 24-in wide by 10 ft long, and
the that the rate growth then increases rapidly until at
containing a long ribbon mixer that turns at about 7 rpm. As many of
some fairly high value of supersaturation , it becomes
these four these units maybe connected together with the agitators
linear with superstauration.
driven from a single shaft.
 Moreover, according to surface growth theory, crystals
have imperfections called dislocations, the most common G.2 Supersaturation By Evaporation Of Solvent
one is screw dislocation. The dislocation is in a shear plane
perpendicular to the crystal’s surface and the slipping of Applicable for the substance whose solubility is independent of
the crystal creates ramp temperature (i.e flat solubility-temp curve) and that yield of solids
 ∆L law – If all crystals in magma grow in a uniform by cooling is negligible
supersaturation field and at the same temperature and if
all crystals grow from birth at a rate governed by the Salting Evaporator
supersaturation, then all crystals are not only invariant
but also have the same growth rate that is independent of The most common of the evaporating crystallizers; in older form, the
size crystallizer consisted of an evaporator below which were settling
chambers into which the salt settled. The chambers were connected
F. Crystal Seeding in tandem so that the salt could be removed by one of them while
the other was connected to the system
The relation between seed and product particle sizes may be written
as Oslo Crystallizer

Lp = Ls + ∆L Modern form of evaporating crystallizer; this unit is particularly well


Lp = Ls + ∆L adopted to the production of large-sized uniform crystals that are
usually rounded; it consists essentially of a forced circulation
evaporator with an external heater containing a combination of salt
Where: Lp or Dp = characteristic particle dimension of the filter and particle size classifier on the bottom of the evaporator
product; Ls or Ds = characteristic particle dimension of the seed body
∆L or ∆D = change in size of crystals and is constant throughout the
range of size present Draft Tube Crystallizer

Since the rate of linear crystal growth is independent of crystal size, It consist of crystallizer body equipped with draft tube, which also
the seed and product masses may be related for acts as a baffle to control circulation of the magma, and an upward-
directed propeller agitator to provide a controllable circulation
Wp = Ws (Dp3/Ds3) within the crystallizer. Draft tube crystallizers are also equipped with
elutriation leg below the body to classify the crystal by size and may
also be equipped with baffled settling zones for fines removal.
G.3 Vacuum crystallizers 4 x 104 kJ. Calculate the heat to be removed in the cooling process.
(Ans 455 kJ)
 Evaporation is obtained by flashing a hot solution into a
low pressure space. 5. One ton of Na2S2O3·5H2O is to be crystallized per hour by cooling
 Supersaturation is obtained thru adiabatic evaporative a solution containing 56.5% Na2S2O3 to 30°C in a Swenson-Walker
cooling. crystallizer. Evaporation is negligible. The product is to be sized
 In its original and simplest form, it consist of closed vessel closely to approximately 14 mesh. Seed crystals closely sized to 20
in which vacuum is maintained by a condenser, usually mesh are introduced with the solution as it enters the crystallizer.
with the help of a steam-jet vacuum pump located How many tons of seed crystals and how many tons of solutions are
between the crystaliizer and the condenser. required per hour? At 30°C, solubility of Na2S2O3 is 83 parts per 100
 Energy of vaporization is obtained at the expense of parts water
sensible heat in the feed. As a result, the temperature of
the vapour – liquor mixture after flashing is much lower 6. ** A Swenson-Walker crystallizer is fed with a saturated solution
of magnesium sulfate at 110°F. The solution and its crystalline crop
than that of the liquor before flashing
are cooled to 40°F. The inlet solution contains 1 g of seed crystals
Problems per 100 g of solution. The seeds are 80 mesh. Assuming ideal
growth, what is the mesh size of the crystals leaving with the cooled
1. A Swenson-Walker crystallizer is to be used to produce 1 ton/h product? Evaporation may be neglected.
of copperas (FeSO4·7H2O) crystals. The saturated solution
enters the crystallizer at 120°F. The slurry leaving the Hint: Refer to 7th edition of Perry for Mesh Size
crystallizer will be at 80°F. Cooling water enters the crystallizer
(Ans 24 Mesh)
jacket at 60°F and leaves at 70°F. It may be assumed that the U
for the crystallizer is 35 BTU/h·°F·ft2. There are 3.5 ft2 of
cooling surface per ft of crystallizer length. a) Estimate the
cooling water required b) Determine the number of 10ft- Concept Sources : “Principles of Unit Operations”, 2ed by Foust et.al
crystallizer section to be used. “Unit Operations of Chemical Engineering”, 6ed by
McCabe Smith et.a
2. ** A hot solution of Ba(NO3)2 from an evaporator contains
30.6 kg Ba(NO3)2/100 kg H2O and goes to a crystallizer where
“In most time of our life, it is always the wrong people who teaches
the solution is cooled and Ba(NO3)2 crystallizes. On cooling,
us the right lessons” - Anon
10% of the original water present evaporates. For a feed
solution of 100 kg total, calculate the following: a) The yield of
crystals if the solution is cooled to 290K, where the solubility is
8.6 kg Ba(NO3)2/100 kg total water (17.5026 kg)
b) The yield if cooled instead to 283K, where the solubility is 7
kg Ba(NO3)2/100 kg total water (18. 6077kg)

3. ** The solubility of sodium sulfate is 40 parts Na2SO4 per 100


parts of water at 30°C, and 13.5 parts at 15°C. The latent heat of
crystallization (liberated when crystals form) is 18,000 g-cal per gmol
Na2SO4. Glauber’s salt (Na2SO4·10H2O) is to be made in a
SwensonWalker crystallizer by cooling a solution, saturated at 30°C,
to 15°C. Cooling water enters at 10°C and leaves at 20°C. The
overall heat transfer coefficient in the crystallizer is 25 BTU/h·ft2·°F
and each foot of crystallizer has 3 sq ft of cooling surface. How
many 10-ft units of crystallizer will be required to produce 1 ton/h of
Glauber’s Salt (30 Units)

4. **Lactose syrup is concentrated to 8 g lactose per 10 g of water


and then run into a crystallizing vat which contains 2,500 kg of the
syrup. In this vat, containing 2,500 kg of syrup, it is cooled from 57°C
to 10°C. Lactose crystallizes with one molecule of water of
crystallization. The specific heat of the lactose solution is 3470
J/kg·°C. The heat of solution for lactose monohydrate is -15,500
kJ/kmol. The molecular weight of lactose monohydrate is 360 and
the solubility of lactose at 10°C is 1.5 g/10 g water. Assume that 1%
of the water evaporates and that the heat loss trough the vat walls is

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