SOME THOUGHTS OF SUGAR

REFINING PROCESS

PRESENTED BY –
M.K.YADAV
J.T.O. (SUGAR TECHNOLOGY)
N.S.I. KANPUR

6-SEP-17 National Sugar Institute, Kanpur 01

 Indian Sugar Scenario

India is the largest consumer and second largest

sugar producer in the world after Brazil.

Climatic
Climatic fluctuations cause surplus and shortages
over alternate years which creates havoc for
planning.
planning.

The
The majority of India’s output is direct plantation
white sugar which is inferior to refined sugar and
has quality implications especially for industrial
customers.
customers.

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 Introduction

Demand
Demand for high quality sugar by local and multi
nationals is growing at a steady rate.
rate.

Sulphitation
Sulphitation and other plantation white
processes were phased out in many countries and
this trend continues in countries like china,
Indonesia etc

India
India by virtue of its needs, is slowly introducing
back-
back-end and stand-
stand-alone refineries.
refineries.

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 Sulphitation

 Sulphitation has been the back bone of the

sugar industry for many years.
years.
 The process produces a direct consumption
white sugar and being used for more than 100
years.
years.
 Over the years, we have made a remarkable
journey of perfecting this process.
process.
 Using new materials of construction and
automation, it has become a robust and
predictable process.
process.
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 Consumption Pattern

House
House hold is 35%
35%
Institutional/
Institutional/ Bulk consumers 65%
65%
Sweet
Sweet makers
Confectionaries
Confectionaries and Bakeries
Beverages
Beverages
Pharmaceutical
Pharmaceutical Industry
Ice
Ice cream, Dairy, and canned food etc.
etc.

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 Demerits of Sulphitation

Sulphitation has some disadvantages which

have not been solved so far:------

 Lime consumption 1.5 – 1.8 times more than

defecation.
defecation.
 Higher lime salts in juice resulting in evaporator
tube fouling.
fouling.
 Corrosion problems due to low pH.
pH.
 Higher molasses losses due to chemical losses.
losses.
 Inferior sugar quality as compared to Refined
sugar.
sugar.
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 Refined & Plantation White Sugar

The following parameters are indicative of

difference of.
of.
 Colour
Colour of sugar shows undesirable
impurities present in the sugar crystal.
crystal. The sugar
colour of plantation white sugar varies in between
90-
90-200 I.U. where as Refined sugar EEC grade-
grade-I is
below 22 and Refined sugar EEC grade –II is below
45 IU .
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 Refined & Plantation White Sugar

Insoluble
Insoluble Impurities:
Impurities:-
Insoluble’s are the substance present in the sugar crystal as
contaminants, which are insoluble in water.water. As plantation white
sugar process does not have any filtration process, insoluble level
is very high, this varies in a large from 100to
100to 250 ppm where as in
Refined sugar this is below 20 ppm.ppm., Insoluble’s and turbidity not
only effects the appearance of sugar solution but also unsuitable
for many bulk consumers.
consumers. As plantation white sugar do not pass the
floc test.
test. The insoluble matter is often considered as important
criteria as regards the suitability of sugar for bulk consumers

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 Refined & Plantation White Sugar
Sulphur
Sulphur Content
The sulphur content varies in between 20-20-70
ppm in Plantation white sugar as sulphur is
used as a clarifying cum bleaching agent,
where as sulphur is not used in refined sugar
making process so it is always less than 5
ppm ( negligible ). Calcium sulphite and
hydrogen sulphite are occluded to sugar
crystals during crystallization or are present
in the syrup film creates various difficulties
when used in food processing industry .
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 Refined & Plantation White Sugar

Ash
Ash Content
Ash content is the inorganic components
remaining after complete incineration of
organic material mainly consists of
Potassium, Sodium, calcium and iron salts.
salts.
Plantation white sugar this is almost around
0.10 % but in refined sugar this is less than
0.03 %.
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 Refined & Plantation White Sugar

Invert
Invert Sugar
Invert sugar is a mixture of two reducing
mono saccharides D- glucose and D-
fructose, The invert sugar content is a factor
of in its storability.
storability. The invert content of
plantation white sugar is around 0.10% 10%
where as in refined sugar this is around
0.03%
03%. This inhibits the sugar storage.
storage.
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 Process Technology Should be…

If Sugar is Import Raw Sugar

Refine in Integrated Feed Domestic
Refinery Market
Short

If Sugar is Process Produce 45 IU Export in

Surplus Sugarcane Sugar Global Market

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 Technological Advances

Refinery Process

Secondary Boiling Condensing

Clarification Energy
Decolorization Scheme System

Carbonati Straight Water Steam

GAC Transformer
on Boiling Cooled

Melt
Phosphat Back Air Concentration
IER with extensive
ation Boiling Cooled bleeding

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 Refined Sugar Advantages Vs Plantation Sugar

Keeping Sulphur Life of

Demand Use
quality Content Equipments

Life of refinery
Refined Demand from Multiple plant equipment
Up to 24 sulphurless Institutional value added is more reliable
Sugar months sugar buyer (Coke, product can due to
Pepsi etc) operations at
be made neutral pH

Plantation
Sugar Life of plant is
Contains 40-
Direct/ Table Conventiona less due to
6-7 months 50 ppm
consumption l use operations at
sulphur
low pH

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 Integrated Sugar Refinery
Value addition by managing domestic sugar cycles
• Produce raw during campaign and refine during off-
campaign
• Make refinery working for over 300 days/year
Round the year • Generate surplus power (cogeneration route)
operation: The best • 100% capacity utilization can be achieved irrespective of
utilization of capital
and resources sugarcane availability

• Set up raw sugar plants around a large nucleus

refinery/integrated complex.
Future: Cluster • Operate integrated complex for longer duration using raw sugar,
manufacturing
approach
molasses and Bagasse.
• Resultant savings in fixed costs and capital around 20%
• Minimize per unit of conversion cost by 15%

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 Refining advantages

Produce
Produce raw and/ or refined sugar or mix of both
for market depending upon the market conditions
Import
Import Raw and refine during off- off-campaign
periods.
periods. Do the tolling depending upon the
location from port
Carry
Carry out export based business initiatives.
initiatives.
Premium
Premium in domestic and global markets.
markets.
Initiate
Initiate specialty sugar production facilities for
Premium
Premium market .
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 Criteria for Refining
Criteria process
for Refining selection
process selection

Capital
Capital cost
Operating
Operating cost
Process
Process capabilities
Environmental
Environmental concern
Availability
Availability of process
chemicals/Polymers/technologies/equipments
Raw
Raw sugar quality
Refined
Refined sugar quality

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 Unit Operations in Sugar Refinery
•Raw Sugar Storage / Handling
•Affination
•Melting
•Clarification
•Decolourisation
•Filtration
•Crystallization & Centrifuging
•Recovery
•Drying, Cooling & Packing
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 Option for Refining raw sugar

The process involves for making refined sugar in two

basic stages, Pre-
Pre-treatment of Raw Sugar Liquor and then
De-
De-colorization of treated sugar liquor.
liquor. Thus basically,
colour removal occurs in two stages.
stages.

FIRST STAGE:
STAGE:
 Pre-
Pre-treatment of Raw Sugar Liquor-
Liquor- It is classified in to
two main clarification steps:
steps:-
i. Carbonation process.
process.
ii. Phospho-
Phospho- floatation Process.
Process.

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 Contd.........

SECOND STAGE:
STAGE:
 Secondary Decolourization Process-
Process-
It is through Granular activated carbon, Powdered activated carbon &
Ion exchange resin.
resin.
The main Objective of above both clarification steps are the removal
of turbidity and colour.
colour. The choice of the process, whether Carbonation or
Phosphatation is dependent on several factors:
factors:
Raw
Raw Sugar Quality.
Turbidity
Turbidity Removal.
Colour
Colour Removal.
 Process Capability.
Capital
Capital cost.
Operating
Operating costs.
Sugar
Sugar loss & Environmental concerns.
Refined
Refined sugar quality.

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 DESCRIPTION OF THE CARBONATION PROCESS

Process
Process involves precipitation of Calcium Carbonate with addition of Ca(OH)2
Ca(OH)2
& Carbon Dioxide.
Dioxide.
Carbon
Carbon dioxide can be scrubbed from Flue gas & then compressed to fed to
Carbonators.
Carbonators.
Proper
Proper & effective distribution of CO2 gas for better precipitation.
precipitation.
Carbonation
Carbonation can be followed in three stages & in some refineries within two
stages.
stages.
Carbonator
Carbonator -1, pH drops from 10.
10.6 to 9.6 & Retention time in all saturators – 55
to 60 minutes.
minutes.
Carbonator
Carbonator -2, pH drops up to 8.4-8.5
Carbonator
Carbonator- 80-850C.
Carbonator-3, pH drops to 8.0 – 8.2 at 80-

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 Process Flow diagram

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 Melting and carbonation:

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 Saturators with the arrangement of CO2, MOL
& Steam

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 Saturators / Carbonators

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 Carbonators Arrangement

To ensure the completion of reaction, it is normal practice to use two saturators

in series. 85% of the reaction is completed in Ist vessel & remaining 15 %
series. About 85%
in second vessel.
vessel.
The arrangements are made as per the capacity & reaction condition requires.
requires.
•Line
Line A only (A1& A2)
•Line
Line B only (B1& B2 )
•Line
Line A and B
•Line
Line AI,AII and BI only
•Line
Line BI,BII and AI only

The first vessel operates at out let pH of 9.5-9.6 & second vessel at 8.1 to 8.2.
The higher pH leads to higher Cao in liquor & it is observed that the soluble
bicarbonates are formed below pH 8.0, which not only increase the ash % but
also detrimental to the filtration.
filtration.

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 Gas Distribution

The proper mixing of the CO2 CO2 gas & limed liquor is the very
essential need of the reaction.
reaction. So the good gas distributor ( Richter
tube) must fulfil the following conditions.
conditions.

Distribute the gas uniformly over the cross-

cross-sectional area of the
saturators.
saturators.

Distribute gas in the form of very small size bubbles & more nos.
nos.
since the smaller the size of the bubble larger area for mass
transfer.
transfer.

Sufficient agitation in the vessel is to be provided to ensure the
uniform condition in the vessel & to keep the boundary layer
between gas bubble & liquid as thin as possible.
possible.
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 View of Richter Tube

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 CONTINUED…..
CONTINUED…..

Ca (OH)2 + CO2 = CaCO3 + H2O

 Lime is added to melt liquor immediately ahead of the saturator.
saturator.
 Boiler flue gas is used as source of CO2 required for the reaction
to form calcium carbonate.
carbonate.
The
The concentration CO2 gas is about 12- 12-14%
14% in scrubbed flue
gases.
gases.
General Observation on Impurity Removal from Melt during Carbonation
Colour 60
Turbidity 90
Starch 93
Gums 29
Sulphates 86
Phosphates 100
Magnesium 67

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 Co2 Scrubbing System From Boiler flue gases

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 Step Wise Colour & Turbidity Removal in Carbonation Process:

Color Turbidity Alkalinity

Particular Brix % Pol Purity pH
(IU) (NTU) (ppm, as CaO)
64.2 63.62 99.10 6.9 1250 50
Raw Sugar
Melted Liquor 63.3 62.72 99.08 6.9 1380 55
64.3 63.82 99.25 7.3 1360 54
Limed 61.9 10.4
Liquor (MOL 61.9 10.4
Ratio - 2.8 %
V/V ) 64.8 10.3
60.7 8.1
Carbonated
Liquor 60.0 8.2
61.3 8.2
59.6 59.22 99.36 8.0 445 4
Filtered Melted
Liquor 1 61.1 60.66 99.28 8.0 485 4
62.9 62.46 99.30 8.2 480 3
60.3 59.92 99.37 7.8 428 2 180
Filtered Melted
Liquor 2 61.1 60.64 99.25 8.0 470 2 203
60.0 59.58 99.30 8.0 402 2 190
60.8 7.8 220 1
Decolorized
Liquor 60.3 7.7 215 1
60.1 7.9 205 1

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 PRECIPITATE & CO2 CALCULATION BY ALKALINITY
METHOD

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 Precipitate & CO2 Calculation by precipitation Method

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Filtration:
Filtration:-

The
The separation of the clear liquor and the calcium carbonate is done by
pressure filtration.
filtration.

Carbonated
Carbonated liquor pressure filters.
filters.
Daistar
Daistar or candle filters.
filters.
Safety
Safety filter.
filter.

Filtering
Filtering elements are generally made up of polypropylene cloth.
cloth.
Monofilament polypropylene woven fabric cloth are used universally.
universally.

Periodic
Periodic cleaning of cloth with sulphamic acid with inhibitor is generally
followed.
followed.

Installed
Installed capacity of filters is designed so as to handle worst quality of raw
sugar liquor.
liquor.

Considering
Considering the minimum filterability of raw sugar, filter area requirement of
15 m2 filtering area per tone of melt per hour is considered to be standard.
standard.

On volumetric basis, filtration rate of 0.1 m3/ m2 / hour is acceptable.

On acceptable.

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 Flux calculation in filters

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 Flux calculation in safety filters

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 DESCRIPTION OF THE PHOSPHATATION
PROCESS

The process of floatation can be divided in three main steps:

steps:-
Phosphate
Phosphate flocculation.
flocculation.
Air
Air floatation.
floatation.
Scum
Scum production.
production.
Phosphate flocculation:
flocculation:- The objective of first step is to form a floccules that
would occlude, adsorb and absorb the greatest possible portion of impurities.
impurities.
This process is further classified in to three steps.
steps.
 Reaction of phosphoric acid and lime.
lime.
Primary
Primary flocculation.
flocculation.
Secondary
Secondary flocculation.
flocculation.

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 DESCRIPTION OF THE PHOSPHATATION Contd...

 The reaction between lime and H3PO4 produces a precipitate of tricalcium

phosphate, to which is added a flocculent to coagulate it.
it.

3Ca (OH)2 + 2 H3 PO4 = Ca3(PO4)2 + 6H2O.

 The precipitate is very fine & therefore, the liquor is aerated by dispersed air to
flotation in a clarifier.
clarifier.
The
The precipitate and other debris are scraped off as a scum.
scum.
The
The scum is de-
de-sweetened in several ways, the most popular of which is a series of
two or three counter current clarifiers.
clarifiers.
The
The clear liquor underflow is led to one or two filtration processes where any carry
over is removed.
removed.

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 Measurement of effectiveness of reaction

Residual phosphate in the clarified liquor is most important

parameter to measure the completion of reaction.
reaction. Hence frequent
measurement of phosphate content will give the indication about the
performance of the reaction / system.
system.
Aeration:
Aeration: The aim of this stage is to achieve complete floatation of
the floccules formed in the first stage.
stage.
With the aeration we introduce the greatest possible population of
minute air bubble uniformly distributed in the liquor.
liquor. The performance
of floatation is largely depends upon the sufficient no.
no. Of suitable size
of air bubbles.
bubbles.
 Air bubble parameters

As air bubbles provides the lifting force for floatation of the solid floccules, there size and
no.
no. Have great influence on the stability and velocity of floatation.
floatation.
following equation will help in knowing this phenomenon.
phenomenon.
Force F1 casing a body to float in the liquid is
F1 = v.(d2
(d2-d1)
Where v = Volume of the body.
body.
d1=Density of the body.
body.
d2=Density of the liquid.
liquid.
The resistance F2 to a body to float is given by-
by-
F2 = c.d2.A.V2/2g
Where c is the coeff.
coeff. Of motion resistance and is further defined as c = 24/Re,
24/Re, (Re= Reynolds
no.
no.), A= Sectional area of the body, V=moving velocity of the body.
body.
 PROCESS CAPABILITY

1.% Removal of impurities : The table given below have been drawn on the basis of
observations made and data collected with regard to % impurity removal in the two
processes, Phosphatation & Carbonation:
Carbonation:
Analysis % removal of impurities
Carbonation (0.60% CaO) Phosphatation(0.050% P2O5)
Colour 55 35
Turbidity 95 88
Starch 93 95
Polysaccharides 91 62
Sulphate 86 28
Phosphate 100 88
Magnesium 67 35

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 2.Chemical Consumption:
Consumption: The details with respect to requirement
of primary and secondary process chemicals for the processing
house are indicated in the following table:
table:

Particulars Doses Chemical consumption % on raw sugar

(ppm) Phosphatation Carbonation
Phosphoric acid 500 0.059 0.0
Flocculent 10 0.001 0.0
Colour precipitant 150 0.015 0.0
Calcium oxide Neutralisation 0.060 0.60
Alfa-Amylase 8 0.00 0.0008
enzyme

Overall, the Carbonation process is a more efficient in

removal of impurities with lower chemical requirement as indicated
in the above table.
table.
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 Colour Transfer

The
The term colour transfer is used to describe the incorporation of
colour into the sucrose crystal during crystallization.
crystallization.
 Lionnet reported the results of two refineries operating
Carbonation:
Carbonation: Ion Exchange and Phosphatation:
Phosphatation: Ion Exchange.
Exchange. He
reported data that showed that the colour transfer of Carbonation
was superior to that of Phosphatation as shown in table.
table.
Feed colour Crystal colour
Carbonation Ion-Exchange Phosphatation Ion-
Exchange
200 12.00 17.00
400 17.50 22.00
600 22.00 27.00
800 26.00 31.00

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SEP-17 National Sugar Institute, Kanpur 41
 Colour Transfer Contd......

It
It is believed that the higher operating pH of liquors
reduces inversion.
inversion. Invert, especially fructose, is one of
many pre-
pre-cursors of colour.
colour. Phosphatation refineries
show higher invert gain, about 0.025% 025% compared to
carbonation refinery liquor gain of 0.012%
012%.

Carbonation
Carbonation is thus considered as superior to
Phosphatation with respects to colour transfer.
transfer.

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 COST COMPARISON OF CARBONATION &
PHOSPHATATION PROCESS

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 COST COMPARISON OF CARBONATION &
PHOSPHATATION PROCESS Contd............

Total
Total chemical & electrical cost in Carbonation process= 973.
973.22
Rs/Ton of Raw Sugar.
Sugar.

Total
Total chemical & electrical cost in Phosphatation process =
1044.
1044.56 Rs/Ton of Raw Sugar.
Sugar.

Profit
Profit by increasing 1.15%
15% yield on raw sugar in carbonation
process = 460 Rs/Ton of Refined Sugar.
Sugar.

 Net profit in Carbonation process = 460 + (1044.

1044.56-
56-973.
973.22)
22) =
531.
531.34 Rs/Ton of Refined Sugar.
Sugar.

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 Conclusion

Carbonation appears to be the most effective technical and

commercial solution in sugar refining.
refining. Today, the situation has
changed as the costs of energy and chemicals have increased
tremendously.
tremendously. Phosphoric acid prices are linked to the price of
fertiliser and food;
food; both are expected to remain high in the future.
future.
The quality of raw sugar has improved as well and there are more
stringent quality norms for Refined Sugar.
Sugar. Thus, the choice of a
suitable process would depend on the economics taking into
account all such factors and also the size of the sugar refinery
proposed to be set up.
up.

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 THANK YOU

6-SEP-17 National Sugar Institute, Kanpur 46