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Chapter 4 Crystallization

This document provides information on the process of crystallization including: 1) Crystallization is an important industrial process to obtain pure substances from impure solutions. Crystals form that are themselves pure. 2) Key factors in crystallization include yield, purity, size, and shape of crystals produced. 3) Solubility curves show the relationship between solute concentration and temperature. Solubility generally increases with temperature. 4) Material and heat balance calculations are used to determine yield of crystals from a solution by accounting for changes in concentration and temperature along with heat effects.

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472 views13 pages

Chapter 4 Crystallization

This document provides information on the process of crystallization including: 1) Crystallization is an important industrial process to obtain pure substances from impure solutions. Crystals form that are themselves pure. 2) Key factors in crystallization include yield, purity, size, and shape of crystals produced. 3) Solubility curves show the relationship between solute concentration and temperature. Solubility generally increases with temperature. 4) Material and heat balance calculations are used to determine yield of crystals from a solution by accounting for changes in concentration and temperature along with heat effects.

Uploaded by

prosedur
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© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
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CRYSTALLIZATION

• important industrially because:


i) a crystal formed from an impure solution and itself pure
ii) Practical method of obtaining pure chemical substances in a
satisfactory condition for packaging and storing

• solid-liquid separation process

• yield , purity, sizes & shapes of crystals important

• crystals - uniform in size

• formation of 1,4-naphthoquinone crystals from a liquid solution


SOLUBILITY CURVE

• equilibrium is attained when the solution or mother liquor is saturated


(represented by solubility curve)
• solubility dependent mainly on temperature
• solubilities of most salts increase slightly or markedly with temperature

Solubility curve for some typical salts in water Solubility curve for sodium thiosulfate
SOLID-LIQUID PHASE DIAGRAM
Saturation curve/line

Figure 27.3-Solubility curve for the MgSO4-nH2O system at 1 atm


YIELD & MATERIAL & HEAT BALANCES
• yield of crystals can be calculated by knowing:
initial concentration of solute
final temperature
solubility at this temperature
• material balances Mass balance :

kg H2O evaporate Water balance : Input = Output


Solute balance : Input = Output

F kg Hot solution S kg solution


X1 kg X2 kg solute/
solute/ 100 kg H2O
100 kg H2O

C kg Crystal

solute crystals are anhydrous - simple water & solute material balances
crystals are hydrated - some water in the solution is removed with crystals
EXAMPLE 2

A salt solution weighing 10000 kg with 30 wt. % Na2CO3 is cooled from 333K
to 293K. The salt crystallizes as the decahydrate. What will be the yield of
Na2CO3.10H2O crystals if the solubility is 21.5 kg anhydrous Na2CO3/100kg
water?
a) Assume that no water is evaporated.
b) Assume that 3% of the total weight of the solution is lost by evaporation of
water in cooling.
EXAMPLE 3

A solution consisting of 30 wt% MgSO4 and 70% water is


cooled to 60oF. During cooling 5% of the total water in the
system evaporates. How many kilograms of crystals are
obtained per 1000 kg of the original mixture?
SOLID-LIQUID PHASE DIAGRAM
Saturation curve/line

Solubility curve for the MgSO4-nH2O system at 1 atm


EXAMPLE 4

A feed of solution of 2268 kg at 327.6 K (54.4oC)


containing 48.2 kg MgSO4/100 kg total water is
cooled to 293.2 K (20oC), where MgSO4.7H2O
crystals are removed. The solubility of the salt is
35.5 kg MgSO4/100 kg total water. The average heat
capacity of the feed solution can be assumed as 2.93
kJ/kg.K. The heat of solution at 291.2 K (18oC) is
13.31 x 103 kJ/kg mol MgSO4.7H2O.

Calculate the yield of crystals.


HEAT BALANCES IN CRYSTALLIZATION

normally, crystallization is exothermic


W kg H2O
HV kJ/kg

F kg Hot solution S kg solution

hF kJ/kg hS kJ/kg

Total heat absorbed, q (kJ): C kg Crystal


hC kJ/kg

When Tdatum = 32oF = 0oC,


FhF + q = (S + C)hM + WHV
or
FhF + q = ShS + ChC + WHV
HEAT BALANCES IN CRYSTALLIZATION

normally, crystallization is exothermic


W kg H2O
HV kJ/kg

F kg Hot solution S kg solution

hF kJ/kg hS kJ/kg

Total heat absorbed, q (kJ):


C kg Crystal
hC kJ/kg

When Tdatum = Tequil./sat. , FhF + q = W + ChC = W + CH∞crys



heat of crystallization, Hcrys = - heat of solution at infinite dilution, H
soln

Heat absorbed, q = +’ve ,Heat given off , q = -’ve



EXAMPLE 4

A feed of solution of 2268 kg at 327.6 K (54.4oC)


containing 48.2 kg MgSO4/100 kg total water is
cooled to 293.2 K (20oC), where MgSO4.7H2O
crystals are removed. The solubility of the salt is
35.5 kg MgSO4/100 kg total water. The average heat
capacity of the feed solution can be assumed as 2.93
kJ/kg.K. The heat of solution at 291.2 K (18oC) is
13.31 x 103 kJ/kg mol MgSO4.7H2O.

Calculate the yield of crystals and make a heat


balance to determine the total heat
absorbed/released, q, assuming that no water is
vaporized.
ENTHALPY-CONCENTRATION DIAGRAM

a, b, c, d – saturation line, use to


find enthalphy of solution

i, h – complete crystallization,
use to find enthalphy of
crystallization
Fig 27.4-Enthalpy-concentration diagram
for the MgSO4-nH2O system at 1 atm
EXAMPLE 5

A 32.5% solution of MgSO4 at 120oF (48.9oC) is cooled, without appreciable


evaporation to 70oF (21.1oC) in a batch-cooled crystallizer. How much heat
must be removed from the solution per 100 Ib of the feed solution?
The average heat capacity of the feed solution is 0.72 Btu/Ib oF and the heat of
solution at 18oC is 23.2 Btu/Ib of MgSO4.7H20.

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