Sugar Processing Technology

Chapter 5

Crystallization and Cetrifugale

Separation

Food Process Engineering

DEPARTMENT
Chapter 5: Crystallization and Centrifugal Separation

5.1. Crystallization /Pan Boiling/

 Objective :-

 To separate sucrose from impurities and maximize sugar

recovery
 To grow sugar crystals to a desired size

 To Concentrate material

 Pan boiling is a unit operation performed in a sugar factory to take

out the sugar crystal from the mother liquor through crystallization.
 The work is accomplished by boiling the clarified syrup in specially

designed heat exchangers known as vacuum pans.

 Con’t
 Crystallization is the process of forming a crystalline material from
a liquid, gas or amorphous solid
 After the juice is concentrated to the optimum /desired brix (60-70)
in multiple effect evaporators which is called Syrup, then transferred
to single effect evaporator (pan boiling)
 In pan boiling the syrup is further concentrated to 78 – 80 degree
brix at which crystallization of sucrose begins.
 Crystallization of Sucrose

a) Crystallization by evaporation
 Is done in a single effect vacuum evaporator known as vacuum
pan
 A pan is an evaporator crystallizer, that is a unit where
crystallization is done by evaporating water contained in the syrup
b) Crystallization by cooling
 The name of equipment which crystallises sugar by cooling is
crystallizer
 Is employed to complete the job of crystallization which starts at
the pan station
 Vacuum Pan
 The basic goal of the vacuum pan operation is to produce sugar
crystals of a specified size from a solution containing sugar and non-
sugars.
 Crystallization of sucrose by evaporation is done by in a vacuum
evaporator designed for handling viscous materials & known as
vacuum pan
 pan boiling /crystallization in which syrup is further
concentrated from 60-70 (syrup) to 78 – 80 (massecuite) degree
brix at which crystallization of sucrose begins.
 Con’t

• Vacuum pan is entirely similar to that of evaporator body,

however different tube diameter,
• In this vessel syrup is boiled under vacuum to form a mixture of
crystals and mother liquor called Massecuite
 This Massecuite viscosity is high, handling it in narrow tubes of
evaporator is difficult, for this reason a change is made to the
pans in which tubes are wide in diameter and short in length for
effective circulation of Massecuite while boiling.
 NB: out of all the sugar losses ocuuring during processing, max.
Loss of sugar takes place in molasses, hence, the pan boiling
operation assumes greater significance.
 Con’t

 Crystallization is initiated by adding a slurry of sugar fines

and alcohol, which provides the nuclei to start crystallization
in vacuum pans
 In the pan boiling process, the syrup is evaporated until it
reaches the super saturation stage
 At this point the crystallization process is initiated by
“seeding” the solution
 The process is done under a vacuum such that the water boils
at about 65oc in order to minimize the thermal destruction of
sucrose
Vacuum Pan
 Points to be considered during the design of pan

a) Provide uniform distribution of steam/vapour

b) Uniform and quick distribution of feed
c) Efficient removal of condensate
d) Efficient removal of non–condensable gases
e) Efficient circulation
 Principles involved in pan boiling
1) Solubility :-
 Pure sucrose dissolves in water this dissolution is called solubility.

 Solubility increase with increase in temperature for examples 1 kg of

water dissolves 2.334 kg sugar at 400C but at 820C 1kg water dissolves
3.703kg of sugar.

2) Saturated solution :-
 When a solution contains the total maximum quantity of sugar/sucrose
which is in dissolved state. It is said to be saturated solution when this
state of the solution is reached it can not further accept a smallest
amount of sucrose in it.
 Saturation is a state of stable equilibrium
3) Solubility Coefficient :-
 The Solubility of sucrose varies with the impurities present in the solution in case of
beet juice impurrities increase the solubility.
 The opposite hold with the cane products in this case the solubility of sucrose
decreases with decreasing purities.
 The effect varies with the nature of impurites in each case with cane it is mainly
reducing sugar which cause the decrease in the solubility of sucrose.
 The solubility Coefficient (S) is the ratio of the Quantity of sucrose soluble in a given
weight of water in an impure solution at a certain temperature, to the quantity of
sucrose soluble in pure water at the same temperature.

(S)= Solubility of sucrose % water in impure solution

Solubility of sucrose % water in pure solution
4) Super Saturation :-
 Supersaturated solution: when a saturated solution is cooled or
when its water is evaporated in such a way that no sugar crystals
are formed, the solution is termed as supersaturated.
• When sucrose solution contains the total quantity of sucrose
which it can dissolve (maximum possible sucrose) at a given
temperature, it is said to be saturated solution
• If the solution contains more dissolved sucrose than the saturated
solution it is termed as super saturation
 Con,t
Super saturation coefficient :-
 Super saturation coeficient is the ratio of the weight of sucrose %
water contained in a super saturated solution to the weight of
sucrose % water which would be present in a saturated solution
having the same temperature and the same purity.
sucrose% water in super saturated solution
S = ------------------------------------------------------------
sucrose % water in saturated solution
 The value of this coefficient plays an important role in massecuite
boiling.
 As the crystallisation progresses the water content of the solution
decreases & brix % of the material increase finally the super
satuaration state is reached and the coefficient increased from 1.0 to
1.5.
 Con’t
• On the basis of super saturation coeffcient weber distingish
different zone in the sugar saturated phase they are as
follows.
1) Unsaturated Zone:- Coefficient below 1.0
2) Metastable Zone :- Coefficient between 1.0 to 1.2
3) Intermediate Zone :- Coefficient between 1.2 to 1.3
4) Labile Zone :- coefficient above 1.3
 Con’t
There are 3 zones of Super Saturation. These are :

a) Metastable Zone: solution is supersaturated and only existing

sugar crystals grow in size, but no new grain crystals are formed

b) Intermediate Zone: S.S. Is relatively higher, not only existing

crystal grow but there are chances of formation of new sugar
crystals.

c) Labile zone: supersaturation is very high and new crystals are

formed spontaneously

N.B This is the reason, pan boiling is carried out in metastable zone
only & higher zones of supersaturations are avoided.
 Solubility curve - Saturation diagram

Labil te
dia
e e
rm
nte
I

t able
e tas
M Stable

 Stable Zone – crystallisation not possible

 Metastable Zone – crystallisation possible but not spontaneous
 Intermediate Zone- crystallisation possible but on present crystals.
 Labile – crystallisation possible and spontaneous
N.B. We need a supersaturated solution for crystallisation
 Con’t

The over all process of crystallization may be considered to consist of

two steps
1) Nucleus Formation (Seed Addition)
2) Crystal Growth
 Which means that once the nucleus has formed by the aggregation
of solute and then it started to grow in size
 The dissolved sucrose from the mother liquor is deposited on the
crystals by Adsorption
 The speed of this sucrose adsorption by the given crystals is
proportional to its surface area
 The smaller crystals grow more quickly than larger one and hence
at given size crystal,
 the greater the number of grain (crystal), the greater the surface
area and the speed of adsorption of sucrose from the mother liquor
 The general procedure/phase employed during boiling
1) Concentration
 A certain quantity of syrup or a mixture of syrup & molasses of high purity
introduces in to a pan
 Then the syrup/molasses is boiled up to a predefined super saturation point.
2) Graining
 As the syrup concentrated, it becomes more viscous.
 When the super saturation has attained the required value, graining is carried
out.

The Method of Graining mostly employed is the Seed Slurry Method

 The prepared seed in the form of saturated is introduced in the pan at a super

saturation and then the sucrose molecules is forced to deposit on the seed

particles which act as nuclei

 The slurry is added while the material is in the meta stable zone and the charge is

held in that zone through out the boiling

 Con’t

3) Building (Developing) Up the Grain

 In pan boiling, the grain is further developed in to the desired
grain size by feeding of syrup/molasses/ melt or a
combination of them depending on the grade or purity of the
massecuite.
For Example:
 The grain is developed by A-molasses and C-wash for A
footing strike (A fine)
 The grain is developed by A- molasses only for B-footing
strike (B fine)
 The grain is developed by B-molasses only for C-footing
strike (C fine)
 Con’t
4) Tightening the Massecuite
Massecuite is considered tight when the crystals have grown to the point that they
almost fill the void spaces left by the molasses, causing it to lose fluidity.
In pan boiling operation the syrup/molasses is introduced in to pan at a rate of
sufficient :
 To compensate for the quantity of water
 To increase slowly and progressively the volume of the Massecuite in the pan,
in such away that concentration increases with the level of Massecuite and so
that the brix will approximate to the maximum value desired
 During the last phase of the strike, we have therefore in the pan a very tight and
a very viscous Massecuite
 When it is observed that the crystals occupy the maximum space and that of the
mother liquor occupies only the void volume remaining between the adjacent
crystals which are touching each other, the strike is dropped from the pan during
normal operation.
 Con’t
• The bulk of crystallization occurs in vacuum pans operated at 24
to 26 in. Hg vacuum so that boiling occurs at a reduced
temperature.
– Crystallization will be done under vacuum at a temperature of
65°C.
Higher temperatures cause sucrose degradation.(Caramelization)
• Crystallization, is usually carried out in the absence of nucleation
(the generation of further fine crystals) and, thus, seed crystals
must be fed to the pans. (A source of nuclei is necessary).
– If too many nuclei are provided, the crystals will be small;
– if too few, large.
 Factors Affecting the Rate Crystallization
• Factors Affecting the Rate Crystallization

1) Purity
• The rate of crystallisation falls very rapidly as the purity of the
mother liquor decreases.
• That is the rate of crystallisation is proportional to the material
purity.
• This is the reason why the low grade strike requires more time than
the high grade massecuite.
• As can see from the graph, as the purity of the mother-liquor
decreases, the rate crystallization gets decrease.
Rate of crystallization vs purity of
mother-liquor
 Con’t
2) Viscosity of the Massecuite
 The viscosity of the massecuit is inversely proportional to the
temperature and the purity of the material.
 The viscosity is higher for the lower grade massecuite (C-
Massecuite ) being of lower purity than B massecuite.
 The rate of crystllization therefore is very poor in case of C
massecuite boiling resulting into longer boiling period for the same.
 As Massecuite viscosity increases, it affects the mobility of sucrose
molecules and thus decreases the rate of crystallization
3) Temperature
 Lowering the boiling temperature of the massecuite the rate of
crystallisation gets retarded
 Sucrose crystals grows faster in the higher temperature
 Con’t
3) Super saturation :-
 It is established that the rate of deposition of sucrose over the
crystal grain is proportional to the square of the super saturation.
 Therefore the growth of a crystals takes place as the coefficient
increases. But coefficient 1.44 is not to be exceed.
 This is known as the critical value, beyond which the
crystallisation would become out of control giviing abundant false
grain.
 Boiling Scheme(Systems) for Batch Sugar
Crystallization
 Crystallization has to be carried out in several stages (or boiling’s) with the
molasses and crystals being separated at the end of each boiling.
 Two boiling, three boiling, and sometimes four boiling schemes have been used.
 In each case, for the last (low-grade) boiling with the lowest quality molasses,
fine seed crystals are used.
 The crystal product from this boiling is used as seed crystals for the earlier (purer
liquor), high-grade boiling’s.
 The crystal products produced from these boiling's are mixed and become the
final raw sugar product.
Basic Diagram of Three Systems for Batch Sugar
Crystallization
In Figure, a Three Boiling Scheme (A,B,C) is indicated
diagrammatically.
 The syrup enters the A pan together with the seed crystals from
the C boiling.
 After evaporation of water and crystal growth, the crystals are
separated in a centrifuge and pass to product while the liquor
(termed A molasses) passes to the B boiling which is seeded from
the C boiling pan. Product crystals from the B pan are again
produced.
 The liquor from the centrifuge after the B boiling (B molasses) is
used as the feed to the C pan, together with fine seed crystals
produced elsewhere in the factory, e.g., by grinding sugar crystals
in an alcohol slurry.
 After the C boiling the molasses-crystal mixture (massecuite) is
usually cooled to affect a final recovery of sugar (exhaustion of
molasses) before centrifuging» Such cooling crystallization is
always a slow process.
 The recommended pan boiling to be maintained for
efficient operation is as Following:
 Boiling time of various massecuites (Single Pan):
A massecuite : 2- 2 ½ hours
B massecuite : 4-5 hours
C massecuite : 6-8 hours
 Average brixes and purities of various massecuites :
A massecuite : 92-93 & 84-88
B massecuite : 96-97 & 66-70
C massecuite : 100-101 & 50-55
 Average crystal size in low grade massecuites:
B massecuite : 0.30 -0.35 mm
C massecuite : 0.18-0.20 mm
 Massecuite Circulation In Vacuum Pans

The circulation of the Massecuite is most important for the

following reasons;
• To prevent caking of the sugars on the heating surfaces
• To move the crystals freely on the mother liquor so that they face
new sucrose molecules and grow regularly
• To exhaust final molasses at the maximum possible.
• The circulation is promoted by the bubbles of vapour due to
heating in the tubes . These bubbles tend to rise , growing and
agitate the mass and lift it towards the surface .
• Circulation by heating is proportional to the degree of heating. If
the heating is stopped circulation also decreases
 Advantages of Mechanical Circulator
For low grade Massecuite at the end of the strike, the brix becomes high so

that circulation by heat only is not enough and hence the circulation is

assisted by mechanical circulator equipped with pan.

 Maximum temperature reached by the Massecuite substantially lower

 Saving time for the strike

 Less colour formed in the pan and reduced risk of sugar local over heating

 Crystals better formed more sharply and more regularly

 Less deposit on the tubes due to the abrasion effect by the friction of the

circulating crystals and etc

Pan with Mechanical
Circulator
 5.2. Centrifugal Separation
 The various grades of Massecuite after completion of
crystallization process in Vacuum Pans/Crystallizers contain Sugar
Crystals together with Mother Liquor.
 Hence the next operation is separation of this Crystalline Sugar

from Molasses which is thick liquid

 The process of operation is said to be purging or curing or

Centrifuging or centrifugal ling or fugal ling effected by

centrifugal machine
 Con’t

 The centrifugals separate the crystals and the mother liquor as

such that due to high speed of the centrifugation
 the light particles (molasses) centrifuged to the outer shell
 the crystals remain in the inner centrifugal disk
• BY-Products (Molasses)
 The first massecuite is called the A massecuite, and the mother

liquor obtained from the centrifuges is called A molasses and

crystal separated from mother liquor is A sugar

 the mother liquor (A molasses) from the centrifugal is returned

to the vacuum pan

 re-boiled to yield a second massecuite (B massecuite), that in

turn holds a second batch of crystals

 The B massecuite is transferred to the crystallizers and then into

centrifuges,

 the raw sugar is later separated from molasses

 The so-called B sugar from the B massecuite is only

half as pure as that obtained from the first strike

 The raw sugar is combined with the first crop of

crystals

 The molasses from the second boiling (B molasses) is

much lower in purity than the first molasses

 It is re-boiled to form low grade massecuite (C

massecuite), which goes to a crystallizer and then to

centrifuges
 This low grade sugar is mix with syrup and sometimes is

used in the vacuum pans as “seeding” solution

 The final molasses from the third stage (“blackstrap

molasses”) is a heavy, viscous material used primarily as a

supplement in cattle feed

 The cane sugar from the combined A and B massecuite is

dried in fluidized bed driers and cooled

 After cooling, the cane sugars is transferred to packing

bins and then sent to bulk storages and distribution centers

 Types of Centrifugal Machines
 Two Types of Centrifugal Machines are employed for the purpose
of separating Molasses from the Sugar crystal.
These are;
I. Batch Centrifugal
II. Continuous Centrifugal
 Batch Centrifugal
The general assembly/construction of Batch Machines contain:
1) Basket
 The basket are made of special steel and are of sufficient
thickness to with stand the centrifugal force to which they are
subjected
 It is pierced with numerous holes to allow the molasses to
escape
 The basket is open partially at the top to allow Massecuite to be
feed in to it, and bottom opening allows the sugar to be
discharged when the machine is stooped
Basket of Centrifugal
 Con’t

2) Spindle
 The basket is supported at the bottom by the spindle which has its
top head connected to the system of drive through suitable coupling
3) Drive
 Batch centrifugals are high speed machines directly driven by
vertical variable frequency drive electric motors which through
the coupling transmit the rotary drive of the shaft of electric motor
to the centrifugal spindle which carries the basket
4) Plough
The process of scrapping the sugar from the basket screen is
termed as ploughing
 General Operation Principle of Batch
Centrifugal
 The entire operation of centrifugal separation in purging of

Massecuite involves the following steps:

I. Taking charge

II. Running at intermediate speed

III. Running at full speed

IV. Ploughing and discharging

V. After ploughing stages, one complete cycle of

operation is over and the machine is ready for
restarting the next cycle
Batch Centrifugal
 Factors Affecting Centrifugal Separation

 Work at crystallization stages particularly at the pan station has a

great bearing on centrifugal performance.
 Generally the performance of centrifugal machines are affected
by:
 Viscosity of the Massecute
 Uneven Size of the Grain
 Continuous Centrifugal
 In continuous centrifugal a constant stream of Massecuite is charged and sugar
flows out continuously
 These centrifugal work essentially on thin layer principle and efficient molasses
separation is obtained even from mixed size grain
 These are conical basket vertical machines being perforated and lined with
screens
 The drive for the machine is provided with electrical motor mounted behind the
machine with V- belts.
 The top of the machine is open while the bottom shaped like cylinder is closed
Continuous Centrifugal
 Sugar Drying
 Sugar discharged from centrifugal machine is having
 0.2 – 0.4% moisture
 60-80OC temperature
 This moist sugar is not suitable for bagging because
 the sugar crystal forms linkage with each other and leads to
lumps formation
 Some dried lumps are very hard and difficult to break
 so the sugar should dried to a safe limit i.e. up to 0.04%
moisture
 Also hot sugar has tendency to absorb the moist from

atmosphere which results with the formation of lumps

 To avoid these draw backs, sugar should be cooled to

ambient temperature (35 – 40OC)

 The drying of sugar is done by varies equipments

which are as follows

1) Fluidized Bed Driers and coolers (FBD)

2) Rotary cascade Driers and coolers

3) Rotary Louver Driers and coolers.

Grading
 The main aim is particle size classification which is
done by screens
 The classification is usually achieved by using wire
mesh or perforated plate through which
 particles smaller than screen aperture may pass,
 while largest fraction is carried over the surface
Raw Sugar
 The A and B sugars from the centrifuges comprise
the raw sugar of world commerce and stored for
several years
 During bulk storage, the raw sugar undergoes quality
deterioration in the form of increased colour
 Increased colour is the result of sucrose degradation
caused by
 Chemical rxn b/n amino acids and degraded invert
sugars, known as Maillard rxn
 Sugar Handling
• After A-Massecuite double purged in batch
centrifugal, the wet A-sugar is allowed to
feed in rotary dryer – cooler for the
purpose of drying and then the dried sugar is
screened/graded and stored in sugar bins.
• Finally dried white sugar is weighed in
weighing machine and packed by bagging
machine for commercial distribution
• Transportation of wet/dry sugar from one
unit operation to another is handled by :

a) Sugar Conveyors like Screw Conveyor,

Belt Conveyor

b) Sugar Elevators ( Bucket Elevator)

Sugar Processing
Technology
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