CP 432 UNIT OPERATIONS II

TUTORIAL No. 4: CRYSTALLIZATION

Question 1:
A 20 weight % solution of Na2SO4 at 200°F is pumped continuously into a vacuum crystallizer
from which the magma is pumped at 60°F.What is the composition of this magma, and what
percentage of Na2SO4 in the feed is recovered as Na2SO4·10H2O crystals after this magma is
centrifuged?

Question 2
A solution of 32.5% MgSO4 originally at 150°F is to be crystallized in a vacuum adiabatic
crystallizer to give a product containing 4,000 lb/h ofMgSO4·7H2O crystals from
10,000lb/h of feed. The solution boiling point rise is estimated at 10°F. Determine the product
temperature, pressure and weight ratio of mother liquor to crystalline product.
Assume temperature of the solution at 60°F. Assume XL = 0.245 lb MgSO4/lb liquor.

Question 3
A plant produces 30,000 MT of anhydrous sulfate annually by crystallizing sulfate brineat 0°C,
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? Assume:
300 working days per year; the liquor entering the crystallizer is a saturated solution at 0°C;
solubility at 0°C = 5 g MgSO4.10H2O/100 g H2O.
Question 4
In a newly established process, about 1,200 lb of barium nitrate are dissolved insufficient water to form a
saturated solution at90°C. Assuming that 5% of the weight of the original solution is lost
through evaporation, calculate the crop of the crystals obtained
when cooled to 20°C. Solubility data of barium nitrate at 90°C = 30.6 lb/100 lb water; at 20°C
= 9.2 lb/100 lb water.
Question 5
A Swenson-Walker crystallizer is to be used to produce 1 ton/h of copperas
(FeSO4·7H2O) crystals. The saturated solution enters the crystallizer at 120°F. The slurry
leaving the crystallizer will be at 80°F.Cooling water enters the crystallizer jacket at60°F
and leaves at 70°F. It may be assumed that the U for the crystallizer is 35BTU/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 crystallizersection to be used.
Data: specific heat of solution = 0.7BTU/lb·°F; heat of solution= 4400 cal/gmol copperas;
solubility at 120°F = 140 parts copperas/100 parts excess water; solubility at 80°F = 74 parts
copperas/100 parts excess water.

Question 6
The solubility of sodium sulfate is 40 parts Na2SO4 per 100 parts of water at 30°C, and13.5
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 Swenson-Walker
crystallizer by cooling a solution, saturated at 30°C, to 15°C. Cooling water enters at 10°C
and leaves at 20°C. The over-all heat transfer coefficient in the crystallizer is 25
BTU/h·ft2·°F and each foot of crystallizer has 3 sq ft of cooling surface. The crystals contain
0.441 g Na2SO4 per g NaSO4.10H2O. If the Cp for Na2SO4 is 32.8 cal/mol.°C, how many 10-ft
units of crystallizer will be required to produce 1 ton/h of Glauber’s Salt.

Question 7
Crystals of CaCl2·6H2O are to be obtained from a solution of 35 weight % CaCl2, 1 0 weight % inert
soluble impurity, and 55weight % water in an Oslo crystallizer. The solution is fed to the
crystallizer at100°F and receives 250 BTU/lb of feed from the external heater. Products are
withdrawn from the crystallizer at 40°F.
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
CaCl2·6H2O crystals and then dried in a conveyor drier. What is the purity of the final dried
crystalline product?
Cp(CaCl2) = 16.9 + 0.00386 T (cal/mol.K, T in K)
Hsoln(CaCl2.6H20) = -4.1 kcal/mol = -Hcrystalzn
Hvap (40°F) = 1,071 Btu/lb

Fig. Qn. 7

Question 8
Sal soda (Na2CO3·10H2O) is to be made by dissolving soda ash in a mixture of mother liquor
and water to form a 30% solution by weight at 45°C and then cooling to 15°C. 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 15°C, the solubility of Na2CO3 is 14.2 parts
per 100 parts of water. Crystallization is to be done in a Swenson-Walker crystallizer. This is
to be supplied with water at10°C, and sufficient cooling water is to be used to ensure that the
exit water will not be over 20°C.The Swenson-walker crystallizer is built in units 10 ft
long, containing 3 ft2 of heating surface per foot of length. An over-all heat transfer
coefficient of 35 BTU/ft2·h·°F is expected. The latent heat of crystallization of sal soda at 15°C
is approximately 25,000 cal/mol. The specific heat of the solution is 0.85 BTU/lb·°F. 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.

Fig. Qn. 8

Question 9
One ton of Na2S2O3·5H2O is to be crystallized per hour by cooling a solution containing 56.5%
Na2S2O3 to 30°C 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 30°C, solubility of Na2S2O3 is 83 parts
per100 parts water.
DP = mesh 14 = 1.19 mm (sieve opening)
DS = mesh 20 = 0.841 mm (sieve opening)

Question 10

Trisodium phosphate is to be recovered as Na3PO4·12H2O from a 35 weight % solution originally

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

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/lb·°F.
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.

Prof. S.V. Manyele

P107