notes in crystallization

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notes in crystallization

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CRYSTALLIZATION

Compilation of Lectures and Solved Problems

CRYSTALLIZATION

CRYSTALLIZATION

Refers to a solid-liquid separation process in which solid particles are formed within a homogenous phase.

It can occur as:

(1) formation of solid particles in a vapor

(2) formation of solid particles from a liquid melt

(3) formation of solid crystals from a solution

The process usually involves two steps:

(1) concentration of solution and cooling of solution until the solute concentration becomes greater than its

solubility at that temperature

(2) solute comes out of the solution in the form of pure crystals

Crystal Geometry

A crystal is highly organized type of matter, the constituent particles of which are arranged in an orderly and

repetitive manner; they are arranged in orderly three dimensional arrays called SPACE LATTICES

Supersaturation

Supersaturation is a measure of the quantity of solids actually present in solution as compared to the

quantity that is in equilibrium with the solution

supersaturation

(2) COOLING by cooling a solution through indirect heat exchange

(3) VACUUM COOLING by flashing of feed solution adiabatically to a lower temperature and inducing

crystallization by simultaneous cooling and evaporation of the solvent

(4) REACTION by chemical reaction with a third substance

(5) SALTING by the addition of a third component to change the solubility relationship

CRYSTALLIZATION

Mechanism of Crystallization Process

There are two basic steps in the over-all process of crystallization from supersaturated solution:

(1) NUCLEATION

a. Homogenous or Primary Nucleation occurs due to rapid local fluctuations on a molecular scale in

a homogenous phase; it occurs in the bulk of a fluid phase without the involvement of a solid-fluid

interface

b. Heterogeneous Nucleation occurs in the presence of surfaces other than those of the crystals

such as the surfaces of walls of the pipe or container, impellers in mixing or foreign particles; this is

dependent on the intensity of agitation

c. Secondary Nucleation occurs due to the presence of crystals of the crystallizing species

(2) CRYSTAL GROWTH a layer-by-layer process

a. Solute diffusion to the suspension-crystal interface

b. Surface reaction for absorbing solute into the crystal lattice

Crystallization Process

SOLUTION

WATER

CRYSTALS

Solution is concentrated

by evaporating water

The concentrated

solution is cooled until

the concentration

becomes greater than

its solubility at that

temperature

(1) Yield

(2) Purity of the Crystals

(3) Size of the Crystals should be uniform to minimize caking in the package, for ease in pouring, ease

in washing and filtering and for uniform behaviour when used

(4) Shape of the Crystals

Magma

It is the two-phase mixture of mother liquor and crystals of all sizes, which occupies the crystallizer and is

withdrawn as product

CRYSTALLIZATION

(1)

(2)

(3)

(4)

TETRAGONAL 3 axes at right angles to each other, one axis longer than the other 2

ORTHOROMBIC 3 axes at right angles to each other, all of different lengths

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

Classification of Crystallizer

(1) May be classified according to whether they are batch or continuous in operation

(2) May be classified according on the methods used to bring about supersaturation

(3) Can also be classified according on the method of suspending the growing product crystals

Equilibrium Data (Solubilities)

Represent equilibrium conditions

Plotted data of solubilities versus temperatures

In general, solubility is dependent mainly on temperature although sometimes on size of materials and

pressure

Expressions of Solubilities

Parts by mass of anhydrous materials per 100 parts by mass of total solvent

Mass percent of anhydrous materials or solute which ignores water of crystallization

CRYSTALLIZATION

and there are no hydrates or water of

crystallization

300

250

200

150

100

50

0

0

20

40

60

80

100

80

100

but curve is marked with extreme flatness

Temperature, C

250

200

150

100

50

0

0

20

40

60

Temperature, C

temperature but is characterized by breaks

and indicates different hydrates or water of

crystallization

250

200

150

Na2HPO42H2O

Na2HPO47H2O

100

Na2HPO4

Na2HPO412H2O

50

0

0

20

40

60

80

100

at a certain transition point while the solubility of

the hydrate decreases as temperature

increases

Temperature, C

Solubility of Na2HPO4 (CHE HB 8th edition)

60

50

40

Na2CO3H2O

30

20

Na2CO310H2O

10

0

0

20

40

60

80

100

Temperature, C

Solubility of Na2CO3 (CHE HB 8th edition)

SUPERSATURATION BY COOLING

Crystallizers that obtain precipitation by cooling a concentrated hot solution; applicable for substance that

have solubility curve that decreases with temperature; for normal solubility curve which are common for

most substances

CRYSTALLIZATION

Pan Crystallizers

Batch operation; seldom used in modern practice, except in small scale operations, because they are

wasteful of floor space and of labor; usually give a low quality product

Agitated batch Crystallizers

Consist of an agitated tank; usually cone-bottomed, containing cooling coils. It is convenient in small scale

or batch operations because of their low capital costs, simplicity of operation and flexibility

Swenson Walker Crystallizer

A continuous crystallizer consist of an open round bottomed-trough, 24-in wide by 10 ft long, and containing

a long ribbon mixer that turns at about 7 rpm.

CALCULATIONS:

L

XL

hL

tL

F

XF

hf

tF

W

t1

W

t2

C

XC

hC

tC

Solute Balance:

Enthalpy Balance:

Heat Balance:

(

)

(

[

)

]

where:

= mass of the feed solution

= mass of the mother liquor, usually saturated solution

= mass of the crystals

= mass of the cooling water

= mass solute (salt) in the feed solution per mass of feed solution

= mass of solute (salt) in the mother liquor per mass of mother liquor

= mass of solute (salt) in the srystals per mass of crystals

= enthalpy of the feed solution

= enthalpy of the mother liquor

= enthalpy of the crystals

= heat absorbed by the cooling water

= heat loss by the crystals

= specific heat of the feed solution

= specific heat of cooling water

= heat of crystallization

= over-all heat transfer coefficient

= heat transfer area

= temperature of the feed solution

= temperature of the mother liquor

= inlet temperature of cooling water

= outlet temperature of cooling water

CRYSTALLIZATION

Crystallizers that obtain precipitation by evaporating a solution; applicable for the substance whose solubility

curve is flat that yield of solids by cooling is negligible; acceptable to any substance whose solubility curve is

not to steep

Salting Evaporator

The most common of the evaporating crystallizers; in older form, the crystallizer consisted of an evaporator

below which were settling chambers into which the salt settled

Oslo Crystallizer

Modern form of evaporating crystallizer; this unit is particularly well 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 filter and particle size classifier on the bottom of the

evaporator body

CALCULATIONS:

V

hV

F

XF

hf

tF

L

XL

hL

tL

W

t1

W

t2

C

XC

hC

tC

Solute Balance:

Solvent Balance:

(

)

Enthalpy Balance:

Heat Balance:

(

)

(

where:

= mass of the feed solution

= mass of the mother liquor, usually saturated solution

= mass of the crystals

= mass of the cooling water

= mass of the evaporated solvent

= mass solute (salt) in the feed solution per mass of feed

solution

= mass of solute (salt) in the mother liquor per mass of

mother liquor

= mass of solute (salt) in the srystals per mass of crystals

= enthalpy of the feed solution

= enthalpy of the mother liquor

= enthalpy of the crystals

= enthalpy of the vapor

= heat absorbed by the cooling water

= heat loss by the crystals

= specific heat of the feed solution

= specific heat of cooling water

= heat of crystallization

= latent heat of vaporization

= over-all heat transfer coefficient

= heat transfer area

= temperature of the feed solution

= temperature of the mother liquor

= inlet temperature of cooling water

= outlet temperature of cooling water

CRYSTALLIZATION

V

hV

F

XF

hf

L

XL

hL

C

XC

hC

Solute Balance:

Solvent Balance:

(

)

where:

= mass of the feed solution

= mass of the mother liquor, usually saturated solution

= mass of the crystals

= mass of the cooling water

= mass of the evaporated solvent

= mass solute (salt) in the feed solution per mass of feed

solution

= mass of solute (salt) in the mother liquor per mass of

mother liquor

= mass of solute (salt) in the srystals per mass of crystals

= enthalpy of the feed solution

= enthalpy of the mother liquor

= enthalpy of the crystals

= enthalpy of the vapor

= heat of crystallization

= temperature of the feed solution

= temperature of the mother liquor

= inlet temperature of cooling water

= outlet temperature of cooling water

Enthalpy Balance:

CRYSTALLIZATION BY SEEDING

L Law of Crystals

States that if all crystals in magma grow in a supersaturation field and at the same temperature and if

all crystal grow from birth at a rate governed by the supersaturation, then all crystals are not only

invariant but also have the same growth rate that is independent of size

The relation between seed and product particle sizes may be written as

Where:

= characteristic particle dimension of the product

= characteristic particle dimension of the seed

= change in size of crystals and is constant throughout the range of size present

CRYSTALLIZATION

Since the rate of linear crystal growth is independent of crystal size, the seed and product masses may

be related for

(

(

)

)

)

[

(

(

]

)

All the crystals in the seed have been assumed to be of the same shape, and the shape has been assumed

to be unchanged by the growth process. Through assumption is reasonably closed to the actual conditions

in most cases. For differential parts of the crystal masses, each consisting of crystals of identical

dimensions:

CRYSTALLIZATION

PROBLEM # 01:

A 20 weight % solution of Na2SO4 at

200F is pumped continuously to a

vacuum crystallizer from which the

magma is pumped at 60F. What is

the composition of this magma, and

what percentage of Na2SO4 in the

feed is recovered as Na2SO410H2O

crystals after this magma is

centrifuged?

Na2SO4 solution

xF = 0.20

tF = 200F

Na2SO4 10H2O

C

Magma, M

tM = 60F

SOLUTION:

Basis: 100 lb feed

From table 2-122 (CHE HB), solubility of Na2SO410H2O

T,C

10

15

20

g/100 g H2O

9.0

19.4

40.8

Consider over-all material balance:

)(

Substitute

)( )

)( )

in

(

Magma composition:

% Recovery:

)(

(

(

)(

)

)

CRYSTALLIZATION

PROBLEM # 02:

A solution of 32.5% MgSO4 originally

at 150F is to be crystallized in a

vacuum adiabatic crystallizer to give

a product containing 4,000 lb/h of

MgSO47H2O crystals from 10,000

lb/h of feed. The solution boiling

point rise is estimated at 10F.

Determine the product temperature,

pressure and weight ratio of mother

liquor to crystalline product.

MgSO4 solution

F = 10,000 lb/h

xF = 0.325

tF = 150F

MgSO4 7H2O

C = 4,000 lb/h

SOLUTION:

Consider over-all material balance:

)(

( )

)(

THE PROBLEM CAN BE SOLVED BY TRIAL AND ERROR SINCE TEMPERATURE OF THE

SOLUTION AFTER CRYSTALLIZATION IS UNKNOWN AND ENTHALPIES ARE DEPENDENT

ON TEMPERATURE

1. Assume temperature of the solution

th

2. From figure 27-3 (Unit Operations by McCabe and Smoth 7 edition), obtain mass fraction of

MgSO4 at the assumed temperature of the solution

3. Solve for L using equation

4. Solve for V using equation

5. Check if assumed temperature is correct by conducting enthalpy balance

a. Obtain values of hF, hC and hL from figure 27-4 (Unit Operations by McCabe and

th

Smith 7 edition) at the designated temperatures and concentrations

b. Compute for hV

c. Using the enthalpy balance equation, compute for V using the value of L from step

3

6. Compare values of V from step 4 with that from step 5-c

7. If not the same (or approximately the same), conduct another trial and error calculations

CRYSTALLIZATION

TRIAL 1: Assume temperature of the solution at 60F

th

From figure 27-3 (Unit Operations by McCabe and Smith 7 edition)

Substitute to equation

Substitute to equation

th

From steam table at 50F,

)(

[(

)(

)( )

)]

)(

)(

Since % error is less than 5%, assumed value can be considered correct.

Product temperature

Operating Pressure

From steam table for vapor temperature of 50F

CRYSTALLIZATION

PROBLEM # 03 :

A plant produces 30,000 MT of anhydrous

sulfate annually by crystallizing sulfate brine at

0C, yields of 95% and 90% in the

crystallization and calcinations operations are

obtained respectively. How many metric tons

of liquor are fed to the crystallizer daily? Note:

300 working days per year

CALCINATION

YIELD = 90%

SOLUTION:

Assume that the liquor entering the crystallizer is a saturated solution at 0C

From table 2-120 (CHE HB), solubility at 0C:

CRYSTALLIZATION

T=0C

YIELD = 95%

P

Na2SO4

30,000 MT/yr

CRYSTALLIZATION

PROBLEM # 04 :

1,200 lb of barium nitrate are dissolved in

sufficient water to form a saturated solution at

90C. Assuming that 5% of the weight of the

original solution is lost through evaporation,

calculate the crop of the crystals obtained

when cooled to 20C. solubility data of barium

nitrate at 90C = 30.6 lb/100 lb water; at 20C =

9.2 lb/100 lb water

C

T = 20 C

F

1,200 lb BaNO3

CRYSTALLIZER

T = 90 C

L

T = 20 C

SOLUTION:

(

)

(

(

Substitute

)( )

)( )

in

(

[(

)

)(

)]

CRYSTALLIZATION

PROBLEM # 05:

A Swenson-Walker crystallizer is to be used

to produce 1 ton/h of copperas (FeSO47H2O)

crystals. The saturated solution enters the

crystallizer at 120F. The slurry leaving the

crystallizer will be at 80F. Cooling water

enters the crystallizer jacket at 60F and

leaves at 70F. It may be assumed that the U

2

for the crystallizer is 35 BTU/hFft . There

2

are 3.5 ft of cooling surface per ft of

crystallizer length.

a) Estimate the cooling water required

b) Determine the number of crystallizer

section to be used.

Data:

specific heat of solution = 0.7

BTU/lbF; heat of solution= 4400 cal/gmol

copperas; solubility at 120F = 140 parts

copperas/100 parts excess water; solubility at

80F = 74 parts copperas/100 parts excess

water

SOLUTION:

Consider over-all material balance:

Equate

)( )

)(

and

(

)( )

F

tF = 120 F

L

tL = 80 F

SWENSON-WALKER

CRYSTALLIZER

W

t1 = 60 F

t2 = 70 F

C, 1 ton/h

Fe2SO47H2O

tC = 80 F

CRYSTALLIZATION

[(

)(

)(

[(

)(

(

)

)(

)

(

]

)]

)(

CRYSTALLIZATION

PROBLEM # 06:

Crystals of Na2CO310H2O are dropped into a saturated solution of Na2CO3 in water at 100C.

What percent of the Na2CO3 in the Na2CO3H2O is recovered in the precipitated solid? The

precipitated solid is Na2CO3H2O. Data at 100C: the saturated solution is 31.2% Na 2CO3;

molecular weight of Na2CO3 is 106

SOLUTION:

Assume 100 g of Na2CO310H2O added into the saturated solution

CRYSTALLIZATION

PROBLEM # 07:

A solution of MgSO4 at 220F containing 43 g

MgSO4 per 100 g H2O is fed into a cooling

crystallizer operating at 50F. If the solution

leaving the crystallizer is saturated, what is the

rate at which the solution must be fed to the

crystallizer to produce one ton of MgSO47H2O

per hour?

F

tF = 220 F

43 g MgSO4/100 g H2O

L

tL = 50 F

COOLING CRYSTALLIZER

C, 1 ton/h

MgSO47H2O

tC = 50 F

SOLUTION:

Consider over-all material balance:

th

From table 27-3 (Unit Operations by McCabe and Smith, 7 edition), at 50F

Equate

)( )

and

)( )

)( )

CRYSTALLIZATION

PROBLEM # 08:

The solubility of sodium bicarbonate in water

is 9.6 g per 100 g water at 20C and 16.4 g

per 100 g water at 60C. If a saturated

solution of NaHCO3 at 60C is cooled to 20C,

what is the percentage of the dissolved salt

that crystallizes out?

SOLUTION:

Basis: 100 kg feed

Consider over-all material balance:

(

(

)(

Equate

)( )

( )( )

)(

and

V

F

tF = 20 C

8.4% Na2SO4

L

tL = 20 C

CRYSTALLIZER

C,

tC = 20 C

F

tF = 60 F

16.4 g

NaHCO3 /100 g

H2O

L

tL = 20 F

COOLING CRYSTALLIZER

C,

9.6 g NaHCO3

per 100 g H2O

tC = 20 F

CRYSTALLIZATION

PROBLEM # 09:

Glaubers salt is made by crystallization from a water solution at 20C. The aqueous solution at

20C contains 8.4% sodium sulfate. How many grams of water must be evaporated from a liter of

such solution whose specific gravity is 1.077 so that when the residue solution after evaporation

is cooled to 20C, there will be crystallized out 80% of the original sodium sulfate as Glaubers

salt. The solubility of sodium sulfate in equilibrium with the decahydrate is 19.4 g Na2SO4 per 100

g H2O.

SOLUTION:

Basis: 1 L feed

(

(

)(

)(

Substitute to equation

(

(

)( )

Substitute to equation

CRYSTALLIZATION

PROBLEM # 10:

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 the solution is

cooled and Ba(NO3)2 crystallizes. On cooling,

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

b) The yield if cooled instead to 283K, where

the solubility is 7 kg Ba(NO 3)2/100 kg total

water

V

L

F

30.6 kg Ba(NO3)2/100 kg H2O

CRYSTALLIZER

Source:

Transport Processes and Unit

Operations (Geankoplis)

SOLUTION:

a) If solution is cooled to 290K

Consider over-all material balance:

(

)

(

)

(

)

(

)(

)

(

(

(

Equate

)(

and

)( )

)( )

CRYSTALLIZATION

Consider over-all material balance:

(

)

(

)

(

)

(

)(

)

(

(

(

Equate

)(

and

)( )

)( )

CRYSTALLIZATION

PROBLEM # 11:

A batch of 1,000 kg of KCl is dissolved in

sufficient water to make a saturated solution at

363 K, where the solubility is 35 wt % KCl in

water. The solution is cooled to 293 K, at

which temperature its solubility is 25.4 wt %.

a) What are the weight of water required for

the solution and the weight of KCl crystals

obtained?

b) What is the weight of crystals obtained if

5% of the original water evaporates on

cooling?

V

F

1,000 kg KCl

363K

Source:

Transport Processes and Unit

Operations (Geankoplis)

SOLUTION:

c) Assume crystallization by cooling (without evaporation)

Consider over-all material balance:

)( )

Equate

)( )

and

)(

L

293K

CRYSTALLIZER

C

293K

CRYSTALLIZATION

Consider over-all material balance:

(

Equate

)( )

and

)( )

CRYSTALLIZATION

PROBLEM # 12:

The solubility of sodium sulfate is 40 parts

Na2SO4 per 100 parts of water at 30C, and

13.5 parts at 15C.

The latent heat of

crystallization (liberated when crystals form) is

18,000 g-cal per gmol Na2SO4. Glaubers salt

(Na2SO410H2O) is to be made in a SwensonWalker crystallizer by cooling a solution,

saturated at 30C, to 15C. Cooling water

enters at 10C and leaves at 20C. The overall heat transfer coefficient in the crystallizer is

2

25 BTU/hft 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 Glaubers Salt

Source: Unit Operations (Brown)

SOLUTION:

Consider over-all material balance:

)

(

Equate

and

F

tF = 30 C

L

tL = 15 C

SWENSON-WALKER

CRYSTALLIZER

W

t1 = 10 C

t2 = 20 C

C, 1 ton/h

Na2SO410H2O

tC = 15 C

CRYSTALLIZATION

Consider heat balance:

(

)

(

)

)

th

[(

)(

[(

)(

)(

)(

[(

)(

)

)(

)]

]

)]

CRYSTALLIZATION

PROBLEM # 13:

A continuous adiabatic vacuum crystallizer is

to be used for the production of MgSO47H2O

crystals from 20,000 lb/h of solution containing

0.300 weight fraction MgSO4. The solution

enters the crystallizer at 160F.

The

crystallizer is to be operated so that the

mixture of mother liquor and crystals leaving

the crystallizer contains 6,000 lb/h of

MgSO47H2O crystals. The estimated boiling

point elevation of the solution in the

crystallizer is 10F. How many pounds of

water are vaporized per hour?

F, 20,000 lb/h

xF = 0.3000

tF = 160 F

ADIABATIC VACUUM

CRYSTALLIZER

C = 6,000 lb/h

MgSO47H2O

L

BPE = 10 F

SOLUTION:

Consider over-all material balance:

)(

( )( )

)(

THE PROBLEM CAN BE SOLVED BY TRIAL AND ERROR SINCE TEMPERATURE OF THE

SOLUTION AFTER CRYSTALLIZATION IS UNKNOWN AND ENTHALPIES ARE DEPENDENT

ON TEMPERATURE

1. Assume temperature of the solution

th

2. From figure 27-3 (Unit Operations by McCabe and Smoth 7 edition), obtain mass fraction of

MgSO4 at the assumed temperature of the solution

3. Solve for L using equation

4. Solve for V using equation

5. Check if assumed temperature is correct by conducting enthalpy balance

a. Obtain values of hF, hC and hL from figure 27-4 (Unit Operations by McCabe and

th

Smith 7 edition) at the designated temperatures and concentrations

CRYSTALLIZATION

b. Compute for hV

c. Using the enthalpy balance equation, compute for V using the value of L from step

3

6. Compare values of V from step 4 with that from step 5-c

7. If not the same (or approximately the same), conduct another trial and error calculations

th

From figure 27-3 (Unit Operations by McCabe and Smith 7 edition)

Substitute to equation

Substitute to equation

th

From steam table at 50F,

)(

[(

( )(

)( )

)(

)]

)(

CRYSTALLIZATION

PROBLEM # 14:

Crystals of CaCl26H2O are to be obtained

from a solution of 35 weight % CaCl2, 10

weight % inert soluble impurity, and 55

weight % water in an Oslo crystallizer. The

solution is fed to the crystallizer at 100F

and receives 250 BTU/lb of feed from the

external heater. Products are withdrawn

from the crystallizer at 40F.

a) What are the products from the

crystallizer?

b) The magma is centrifuged to a moisture

content of 0.1 lb of liquid per lb of

CaCl26H2O crystals and then dried in a

conveyor drier. What is the purity of the

final dried crystalline product?

Source: Principles of Unit Operations 2

edition (Foust, et al)

F

CaCl2 = 35%

Inert = 10%

H2O = 55%

tF = 100 F

OSLO CRYSTALLIZER

M (magma)

C

Inert

L

tF = 40 F

CENTRIFUGE

C

CaCl26H2O

DRYER

nd

SOLUTION:

Basis: 1 lb of inert soluble-free feed

th

from table 2-120 (CHE HB 8 edition), solubilities of CaCl26H2O

0C

59.5 lb/100 lb H2O

10C

65 lb/100 lb H2O

20C

74.5 lb/100 lb H2O

30C

102 lb/100 lb H2O

At 100F (37.8C), solubility is (by extrapolation), 123.45 lb/100 lb H 2O

At 40F (4.4C), solubility is 61.92 lb/100 lb H2O

Since the equipment is Oslo crystallizer, there the process is supersaturation by evaporation

By heat balance around the crystallizer

(

)

From table 2-194, specific heat of CaCl2, cal/Kmol

where T is in K

At 100F (310.93 K)

At 40F (277.59 K)

CRYSTALLIZATION

(

)(

)

(

)(

th

From table 2-224 (CHE HB 8 edition), heat of solution of CaCl26H2O = -4,100 cal/mol;

in the absence of data on heat of crystallization, heat of solution can be used instead but

of opposite sign

)( )

( )(

)(

)( )

Substitute

(

in

)

(

(

Equate

)( )

)( )

( )( )

and

(

(

)

)

)( )

CRYSTALLIZATION

(

CaCl26H2O

H2O

inerts

lb

0.0056

0.0090

0.1000

0.1146

%

4.89

7.85

87.26

100.00

lb

CaCl26H2O

crystallized

from liquor

0.0762 x 0.0489

0.7620

0.0037

H2O

inerts

0.0762 x 0.0785

0.0762 x 0.8726

0.0060

0.0665

Composition of dried crystals

lb

CaCl26H2O

0.7657

inerts

0.0665

0.8322

%

92.01

7.99

100.00

0.7657

0.0060

0.0665

0.8382

CRYSTALLIZATION

PROBLEM # 15:

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 57C to 10C. Lactose

crystallizes with one molecule of water of

crystallization.

The specific heat of the

lactose solution is 3470 J/kgC. 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 10C is 1.5 g/10 g water. Assume

that 1% of the water evaporates and that the

4

heat loss trough the vat walls is 4 x 10 kJ.

Calculate the heat to be removed in the

cooling process.

F

2,500 kg

8 g lactose per 10 g

water

tF = 57 C

L

1.5 g lactose

per 10 g water

SOLUTION:

Consider over-all material balance

(

(

Equate

)(

and

)( )

)( )

OSLO CRYSTALLIZER

C

tC = 10 C

CRYSTALLIZATION

(

)

At 10C (50F),

)(

[(

[(

)(

)(

)

)]

[(

)(

)]

CRYSTALLIZATION

PROBLEM # 16:

Sal soda (Na2CO310H2O) is to be made by dissolving soda ash in a mixture of mother liquor and

water to form a 30% solution by weight at 45C and then cooling to 15C. The wet crystals

removed from the mother liquor consist of 90% sal soda and 10% mother liquor by weight. The

mother liquor is to be dried on the crystals as additional sal soda. The remainder of the mother

liquor is to be returned to the dissolving tanks. At 15C, the solubility of Na 2CO3 is 14.2 parts per

100 parts water.

Crystallization is to be done in a Swenson-Walker crystallizer. This is to be supplied with water at

10C, and sufficient cooling water is to be used to ensure that the exit water will not be over 20C.

2

The Swenson-walker crystallizer is built in units 10 ft long, containing 3 ft of heating surface per

2

foot of length. An over-all heat transfer coefficient of 35 BTU/ft hF is expected.

The latent heat of crystallization of sal soda at 15C is approximately 25,000 cal/mol. The

specific heat of the solution is 0.85 BTU/lbF. A production of 1 ton/h of dried crystals is desired.

Radiation losses and evaporation from the crystallizer are negligible.

a) What amounts of water and sal soda are to be added to the dissolver per hour?

b) How many units of crystallizer are needed?

c) What is to be the capacity of the refrigeration plant, in tons of refrigeration, if the cooling

water is to be cooled and recycled? One ton of refrigeration is equivalent to 12,000 BTU/h.

F (Soda Ash)

W (Water)

V

A

DISSOLVER

CRYSTALLIZER

45C

FILTER

DRYER

15C

R (remainder

mother liquor)

C (Sal Soda)

SOLUTION:

Basis: 2,000 lb/h (1 ton/h) of sal soda

Consider over-all material balance of the system

)(

CRYSTALLIZATION

Substitute to equation

(

)(

)(

Substitute to equation

(

(

)(

)

)( )

)( )

)(

CRYSTALLIZATION

Equate

and

(

)

(

[(

)(

)(

[(

)(

Refrigeration capacity:

)]

[(

)(

)]

CRYSTALLIZATION

PROBLEM # 17:

One ton of Na2S2O35H2O is to be crystallized per hour by cooling a solution containing 56.5%

Na2S2O3 to 30C in a Swenson-Walker crystallizer. Evaporation is negligible. The product is to

be sized closely to approximately 14 mesh. Seed crystals closely sized to 20 mesh are

introduced with the solution as it enters the crystallizer. How many tons of seed crystals and how

many tons of solutions are required per hour? At 30C, solubility of Na 2S2O3 is 83 parts per 100

parts water

Source: Unit Operations (Brown, et al)

SOLUTION:

)

th

(

(

Equate

and

)( )

)( )

Equate

and

)(

)

)

CRYSTALLIZATION

PROBLEM # 18:

A Swenson-Walker crystallizer is fed with a saturated solution of magnesium sulfate at 110F.

The solution and its crystalline crop are cooled to 40F. The inlet solution contains 1 g of seed

crystals 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 product? Evaporation may be neglected.

SOLUTION:

Basis: 100 lb feed

Consider over-all material balance

th

From figure 27-3 (Unit Operation 7 edition, McCabe and Smith) at 110F

th

From figure 27-3 (Unit Operations 7 edition, McCabe and Smith) at 40F

)(

Equate

)( )

and

)( )

]

th

(

(

th

CRYSTALLIZATION

PROBLEM # 19:

Trisodium phosphate is to be recovered as Na3PO412H2O from a 35 weight % solution originally

at 190F by cooling and seeding in a Swenson-Walker crystallizer. From 20,000 lb/h feed, 7,000

lb/h of product crystals in addition to the seed crystals are to be obtained. Seed crystals fed at a

rate of 500 lb/h have the following size range:

Weight Range

Size Range, in

10 %

- 0.0200 + 0.0100

20 %

- 0.0100 + 0.0050

40 %

- 0.0050 + 0.0025

30 %

- 0.0025 + 0.0010

Latent heat of crystallization of trisodium phosphate is 27,500 BTU/lbmol. Specific heat for the

trisodium phosphate solution may be taken as 0.8 BTU/lbF.

a) Estimate the product particle size distribution

b) To what temperature must the solution be cooled, and what will be the cooling duty in BTU/h

SOLUTION:

)

(

(

Where:

Solve for required

)

= fractional weight range

:

1. Assume value of

2. Solve for (

) for each size range, use the mean for each size range

3. Solve for

4. Get the total

5. If

, then assumed

CRYSTALLIZATION

TRIAL 1: Assume

For particle size distribution:

Size Range, in

Size Range, in

Wt %

)(

( )(

)(

Wt %

CRYSTALLIZATION

(

th

50C

60C

43 lb/100 lb H2O

55 lb/100 lb H2O

Cooling Duty:

Consider heat balance:

(

)

[(

)(

)(

[(

)(

)]

CRYSTALLIZATION

PROBLEM # 20:

How much CaCl26H2O must be dissolved in 100 kg of water at 20C to form a saturated

solution? The solubility of CaCl2 at 20C is 6.7 gmol anhydrous salt (CaCl2) per kg of water.

SOLUTION:

For a saturated solution utilizing 100 kg water as solvent:

1. Mole of CaCl2 required

Since there should only be total of 100 kg water in the solution, the amount of free water (net

of water of hydration)

(

6. Amount of CaCl26H2O required for every 100 kg free water (net of water of hydration)

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