Crystallization

The process of forming crystals from solution

The liquid phase remaining after the formation of the crystals is called
‘mother liquor ’ .
• Typical examples are the crystallization of sugar in jams and preserves,
• Crystallization of lactose in ice cream, which
• is the cause of a defect known as ‘ sandiness ’ and
• Recrystallization of cocoa butter in chocolate in the form of white crystals
(bloom) on the surface of the product.
• Crystallization can occur only in supersaturated solutions. A solution can be
brought to supersaturation by a number of methods:

• ● Removal of the solvent by evaporation, membrane separation or freeze

concentration
• ● Cooling the solution (assuming that the solubility increases with the
temperature, which is the case with most but not all solutes)
• ● Changing the pH or the ionic strength
• ● Addition of a second solvent, miscible with the solution, so as to reduce the
solubility of the solute
• ● Chemical complexation, chemical precipitation.
 Principal of Crystallization

• Crystallization The process of crystallization comprises two

mechanisms, namely,
• nucleation as a seed crystal and
• crystal growth of seed crystal to a microscopic size.
• Both occur only in supersaturated solutions.
• Thus, the sequence of crystallization process may be
summarized as
• Cluster--- Embryo----- Nucleus-----Crystal
Rate of Nucleation
Crystal growth
 Equipment

• In industry, crystallization is carried out in crystallizers ,

commonly called pans .
• Pans can be batch or continuous, vacuum or atmospheric
• In pan supersaturation is maintained by evaporation
(evaporative crystallizers), by cooling (cooling crystallizers)
or both.
• Continuous pans are extensively used in modern, large-scale
plants.
• Batch pans are used for the production of ‘ seeds ’ (primary
homogeneous
• nucleation) or for small-scale crystallization processes.
 Recycling crystallization pan
• Typically, a crystallization pan is a vessel
equipped with heat exchange areas (for
• heating or cooling) and agitation
• The heat exchange areas may be provided by a
jacket or by a tubular heat exchange element.
• Agitation may be provided either by a mechanical
stirrer or by recycling.
• Recycling pans with external heat exchangers are
frequently used in the production of salt, citric
acid etc., but not in the sugar industry, because of
the high viscosity of the material.
• Agitation must be sufficiently vigorous to
facilitate mass transfer and good mixing but gentle
enough to prevent crystal fracture, abrasion and
secondary nucleation.
• Vacuum is applied to lower the boiling
temperature and prevent thermal damage when
necessary (e.g. inversion and
caramelization/browning in sugar syrups).
 Distillation

• Distillation is a separation operation based on differences in

volatility.
• If a mixture containing substances that differ in their volatility
is brought to ebullition, the composition of the vapors released
will be different from that of the boiling liquid.
• After condensation, the vapors constitute the ‘ distillate ’ .
• The remaining liquid is called‘ residue ’ or ‘ bottoms ’ .
• In the food sector, its main application is in the production of ethanol and
alcoholic beverages from fermented liquids.
• Other food-related applications include the recovery, fractionation and
concentration of volatile aromas as well as recovery of organic solvents
(desolventation) in the production of edible oils by solvent extraction and
removal of undesirable odorous substances (e.g. Deodorization of cream).
• Distillation may be carried out as a
– Batch or as a continuous process.
Vapor–Liquid Equilibrium (VLE)
 Continuous Flash Distillation

Continuous fl ash distillation is one of the simplest methods of

distillation.
In the food industry, it is mainly used in the primary recovery of
aroma from fruit juices or for deodorization.
Batch (Differential) Distillation
Batch distillation is, in essence, the simplest type of distillation, familiar to all from
laboratory exercises ( Figure 13.4 ).
A batch of the mixture to be distilled is boiled in a closed vessel.
The vapors are condensed by cooling and the distillate is collected.
In contrast to continuous distillation, batch distillation does not take place at steady state.
The composition of the boiling liquid, that of the vapors and that of the collected distillate
change continuously during the process
Fractional Distillation
Basic concepts
The distillation column contains the multiple contact stages, known as plates or trays ,
through which liquid and vapor move in opposite directions
The vapor moves up and the liquid moves down.
The mixture to be distilled is introduced at a certain location.
The portion of the column above that location is
called the rectifi cation zone , while the portion below the feed entrance is the stripping zone .
The column is connected to a reboiler where heat is supplied for vaporization (boiling) and a
condenser where the vapor is condensed by cooling.
In its travel up the column, the vapor is cooled by the descending liquid and the liquid is
heated by the vapor.
This exchange of heat results in the condensation of the less volatile
component from the gas and the evaporation of the more volatile component
from the liquid.
The gas is thus enriched in volatile component as it moves up and the liquid is stripped of its
more volatile component as it flows down the column.
The liquid obtained by condensation in the condenser is divided into two parts: one part is
fed back into the column in order to provide sufficient liquid for contact with the gas.
This part is called the reflux .
The other part is the distillate .
Vapor can be taken out and condensed at any position on the column, producing distillates of
fractions of different compositions, hence the name of ‘ fractional distillation ’ given to the
process.