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Unit Operation Solved Problems From Exams

Crystalline materials frequently cake or cement together when stored due to moisture absorption. Caking can be minimized by efficient drying, airtight packaging, and avoiding compaction during storage. Small crystals are more prone to caking than large crystals due to having more contact points, though size distribution and shape are also important factors. Crystal shape and size distribution can be controlled during crystallization to reduce caking tendency.

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969 views2 pages

Unit Operation Solved Problems From Exams

Crystalline materials frequently cake or cement together when stored due to moisture absorption. Caking can be minimized by efficient drying, airtight packaging, and avoiding compaction during storage. Small crystals are more prone to caking than large crystals due to having more contact points, though size distribution and shape are also important factors. Crystal shape and size distribution can be controlled during crystallization to reduce caking tendency.

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yaseen ali
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852 CHEMICAL ENGINEERING

The yield is then given by equation 15.22 as:

y = (0.56(100 − 40)/100)1.66[0.667 − 0.539(1 − 0.153)]/[1 − 0.539(1.66 − 1)]


= 0.183 kg/s

15.2.6. Caking of crystals

Crystalline materials frequently cake or cement together on storage and crystal size, shape,
moisture content, and storage conditions can all contribute to the caking tendency. In
general, caking is caused by a dampening of the crystal surfaces in storage because of
inefficient drying or an increase in atmospheric humidity above some critical value that
depends on both substance and temperature. The presence of a hygroscopic trace impurity
in the crystals, can also greatly influence their tendency to absorb atmospheric moisture.
Moisture may also be released from inclusions if crystals fracture under storage conditions
and, if crystal surface moisture later evaporates, adjacent crystals become firmly joined
together with a cement of re-crystallised solute. Caking may be minimised by efficient
drying, packaging in airtight containers, and avoiding compaction on storage. In addition,
crystals may be coated with an inert dust that acts as a moisture barrier. Small crystals are
more prone to cake than large crystals because of the greater number of contact points per
unit mass, although actual size is less important than size distribution and shape and the
narrower the size distribution and the more granular the shape, the lower is the tendency
of crystals to cake. Crystal size distribution can be controlled by adjusting operating condi-
tions in a crystalliser and crystal shape may be influenced by the use of habit modifiers.
A comprehensive account of the inhibition of caking by trace additives has been given by
PHOENIX(61) .

15.2.7. Washing of crystals

The product from a crystalliser must be subjected to efficient solid–liquid separation in order
to remove mother liquor and, whilst centrifugal filtration can reduce the liquor content of
granular crystals to 5–10 per cent, small irregular crystals may retain more than 50 per cent.
After filtration, the product is usually washed to reduce the amount of liquor retained still
further and, where the crystals are very soluble in the liquor, another liquid in which the
substance is relatively insoluble is used for the washing, although this two-solvent method
means that a solvent recovery unit is required. When simple washing is inadequate, two
stages may be required for the removal of mother liquor with the crystals removed from the
filter, re-dispersed in wash liquor and filtered again. This may cause a loss of yield although
this is much less than the loss after a complete re-crystallisation.
If, for simplicity, it is assumed that the soluble impurity is in solution and that solution
concentrations are constant throughout the dispersion vessel, then wash liquor requirements
for decantation washing may be estimated as follows.
If, in batch operation, cio and cin denote the impurity concentrations in the crystalline
material (kg impurity/kg product) initially and after washing stage n respectively, and F
CRYSTALLISATION 853
is the fraction of liquid removed at each decantation, then a mass balance gives:
cin = cio (1 − F )n (15.24)
or: ln(cin /cio ) = n ln(1 − F ) (15.25)
For continuous operation, where fresh wash-liquid enters the vessel continuously and liquor
is withdrawn through a filter screen, then a mass balance gives:
VL dc = −ci dVW (15.26)
or: ln(cin /cio ) = −VW /VL (15.27)
where cio and cin are the initial and final concentrations and VL and VW are the volumes
of liquor in the vessel and of the wash-water respectively. Combining equations 15.25 and
15.27:
n ln(1 − F ) = −VW /VL (15.28)
1 Vw 1−F
or: = − ln (15.29)
nF VL F
As MULLIN(3) points out, this equation can be used for comparing batch and continuous
processing since VW and nF VL represent the wash liquor requirements for both cases.

15.3. CRYSTALLISATION FROM SOLUTIONS


Solution crystallisers are usually classified according to the method by which supersatu-
ration is achieved, that is by cooling, evaporation, vacuum, reaction and salting out. The
term controlled denotes supersaturation control whilst classifying refers to classification of
product size.

15.3.1. Cooling crystallisers


Non-agitated vessels
The simplest type of cooling crystalliser is an unstirred tank in which a hot feedstock
solution is charged to an open vessel and allowed to cool, often for several days, by natural
convection. Metallic rods may be suspended in the solution so that large crystals can grow
on them thereby reducing the amount of product that sinks to the bottom of the unit. The
product is usually removed manually. Because cooling is slow, large interlocked crystals
are usually produced. These retain mother liquor and thus the dried crystals are generally
impure. Because of the uncontrolled nature of the process, product crystals range from a
fine dust to large agglomerates. Labour costs are high, but the method is economical for
small batches since capital, operating, and maintenance costs are low, although productivity
is low and space requirements are high.

Agitated vessels
Installation of an agitator in an open-tank crystalliser gives smaller and more uniform
crystals and reduces batch times. Because less liquor is retained by the crystals after filtration

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