Special Web Lecture Session

Topic: Application of Crystallization in Dairy Processing

Speaker: Mr. K. Halder
Time: : May 18, 2020 11:00 AM

https://us04web.zoom.us/j/78518185850?
pwd=YXJObEIzeWJNak1Udm91a3ZTTFJTUT
09 Organized by
Faculty of Dairy Technology, West Bengal University of Animal and Fishery Sciences
Mohanpur Campus, Nadia, West Bengal-741252
Under the aegis of
National Agricultural Higher Education Project
(Innovation Grant)
 Applications of
Crystallisation in Dairy
Processing
 Contents
 What is a crystal?
 What is crystallization process?
 Methods of achieving supersaturation
/crystallisation
 Nucleation
 Crystal growth
 Yield, heat and material balance
 Crystallization Equipments
Cont….

What is a crystal?
 Highly organized type of non-living matter

 A crystal is a solid form of substance (ice)

composed of atoms, ions or molecules arranged
in an orderly and repetitive manner (three
dimensional arrays or space lattice)

 Some crystals are very regularly shaped and can

be classified into one of several shape categories
such hexagonal, orthorhombic, triclinic etc.

 Crystals are grown to a particular size that is of

optimum use to the manufacturer.
Cont….
 What is crystallization process?
 Crystallization refers to the formation of solid
crystals from a homogeneous phase.

 Mass transfer process

 Can occur in the freezing of water to form ice

 Formation of solid particles from liquid melt

 Formation of solid crystals from liquid solution

 What is crystallization process?

Freezing of pure water and water Freezing of water containing

containing single solute multiple solute
 Application in dairy processing
 Ice-cream production

 Granulation in ghee manufacturing

 Lactose production from whey

 Butter manufacturing

 Application in food and chemical processing

(salt, sucrose, metallurgy etc.)
 Basics of Crystallization process
 Basics of crystallization process are common for
all the applications.
 Supersaturation condition
 Nucleation
 Crystal growth
 Supersaturation
 Supersaturation is the driving force for
 Nucleation
 Crystal Growth

 Soluble components are removed from solution by adjusting

the conditions so that the solution becomes supersaturated and
excess solute crystallizes out in a pure form

 This is generally done by lowering the temperature or by

concentrating the solution

 Two forms of supersaturation

 Metastable – just beyond saturation
 Labile – very supersaturated

 Crystallisation is normally operated in the metastable region

 Cont..
 Creation and control of supersaturation is the key to
successful crystallisation

 High supersaturation  High Crystal Growth + High

Nucleation

 High nucleation means a lot of fines (filtration problems)

 High crystal growth means inclusion of impurities

 Supersaturation is usually maintained at a low level in the

pharmaceutical industry so the right CSD is achieved
Achieving Supersaturation
Cont..
Labile
E
Concentration

D
C
A
B
Metastable
Stable
Temperature
ABC - If A is cooled, spontaneous nucleation not
possible until C is reached. No loss of solvent
ADE – If solvent is removed, nucleation occurs at E
 Nucleation
 Crystallisation starts with Nucleation
 There are two types of nucleation – Primary and
Secondary
 Primary relates to the birth of the crystal, where a
few molecules come together to start some form of
ordered structure
 Secondary nucleation can only happen if there are
some crystals present already. It can occur at a
lower level of supersaturation than primary
nucleation.
 Often, industrial crystallisers jump straight to
secondary nucleation by ‘seeding’ the crystalliser
with crystals prepared earlier
Primary Nucleation
 The birth of a new crystal is complex and involves
the clustering of few molecules which are held
together by intermolecular forces

 Homogeneous – small amounts of the new phase

are formed without any help from outside

 Heterogeneous – nucleation is assisted by

suspended particles of a foreign substance or by
solid objects such as the wall of the container or a
rod immersed in the solution – these objects
catalyse the process of nucleation so it occurs at
lower levels of supersaturation

 Homogenous conditions are difficult to create so

heterogeneous nucleation is more normal in
industrial crystallisation (if it is not seeded)
Primary Nucleation

Heterogeneous
Nucleation rate

Homogeneous

Supersaturation
 Secondary Nucleation
 Secondary nucleation is an alternative path to primary
nucleation and occurs when seed crystals are added

 Nucleation occurs at a lower supersaturation than primary

when crystals are already present

 Secondary nucleation is due to:

 Contact nucleation
 Shear nucleation

 Very important in industrial crystallisers as this is the main

type of crystal growth used

 Difficult to predict or model nucleation rates

 Crystallization equilibrium
 Once crystallization is concluded, equilibrium is
set up between the crystals of pure solute and the
residual mother liquor

 The balance being determined by the

solubility(concentration) and the temperature

 Driving force for making ice crystals grow is the

concentration excess(supersaturation) of the
solution above the equilibrium level
Crystal Growth
 Once nucleation has occurred crystal growth can
happen
 The objective of crystallisation is to produce the
required crystal size distribution (CSD)
 The actual CSD required depends on the process
 Crystal growth rate has proved difficult to model and
empirical relationships developed from laboratory
tests are generally used
 Two steps to crystal growth
 Diffusion of solute from bulk solution to the crystal surface
 Deposition of solute and integration into crystal lattice
 Supersaturation and Crystal Growth
 For low supersaturation primary nucleation is not
widespread. Secondary nucleation on existing crystals
is more likely. Result is small numbers of large crystals

 For high supersaturation primary nucleation is

widespread. This results in many crystals of small size.

 Slow cooling with low supersaturation creates large

crystals

 Fast cooling from high supersaturation creates small

crystals

 Agitation reduces crystal size by creating more

dispersed nucleation
 Yield, Heat and Material balance
 Yield
Yield of crystals from a crystallization process can be
calculated knowing the initial solute concentration, the final
temperature and solubility at this temperature.

 Heat Balance
Heat lost in the solution=Heat removed from the solution
Heat lost in the solution=Sensible heat + heat of
crystallization
Heat removed from the solution= Heat loss through walls +
latent heat of evaporation(In case of evaporation) + heat
removed by cooling

 Material Balance
Calculation for material balance are straightforward when
solute crystal are anhydrous. When the crystals are
hydrated, some of the water in the solution is removed with
the crystal as hydrate.
Heat removal in crystallization cooling of lactose
Cont..
 Equipment for Crystallization
 Can be classified according to the methods used for
supersaturation-

 Supersaturation by cooling the solution with negligible

evaporation-tank and batch type crystallizers

 Supersaturation produced by evaporation of the solvent

with little or no cooling – evaporator-crystallizers and
crystallizing evaporators by cooling the solution with
negligible evaporation-tank and batch type crystallizers

 Supersaturation by combined cooling and evaporation in

an adiabatic – Vacuum crystallizers