CHAPTER - I

INTRODUCTION

1.1 Location and History

Factory Site
The sugar industry is essentially an agro industry and therefore should be
centrally located with the vast area of can cultivation: otherwise it will increase
cost of transport. THE SALEM CO-OPERATIVE SUGAR MILLS LIMITED
is locates at 2 kmfrom Mohanur town on the way of Velur of NAMAKKAL
[Link] agronomic conditions such as temperature, humidity, rainfall,
lad fertility and irrigation facilities are highly favorable for abundant growth
and supply of sugar cane with high yields per hectare.
History
Sugar cane the main crop on the northern bank of river cauvery. Till 1964
it was diverted for making [Link] on 24.07.60 THE SALEM CO-
OPERATIVE SUGAR MILLS LTD, MOHANUR was registered under Co-
operative [Link] of machinery was signed three days after with
M/s K.C.P. LTD., Madras for 1000 TCD(TonesCrushing per Day) capacity.
Crushing was started on 07.04.1964 an average of 9,000 acres of cane
cultivation per year was there. Subsequently the factory was permitted to
expand to a crushing capacity of 1750 TCD by the year 1973. And presently the
capacity 2500 TCD was started on 1977 under nearly 32,000 acres of cane
cultivation.
The special and unique feature of his sugar mill is with the desire of
diverting all beagle to the adjacent paper mill. Since from the inception of the
paper mill viz., TAMILNADU NEWS PRINT AND PAPERS LIMITED, (25
km from the sugar factory), as a raw material for paper. And in turn they give

1
steam for the process from their coal and biogases fired boilers situated inside
our factory premises.
Nearest Sugar Factories
1. EID PARRY INDIA LIMITED,Pugalur unit, Karur Dt. -20KM
2. EID PARRY SUGAR (1) LTD,Pettavaithalai, TrichyDt - 50KM
[Link] SUGARS LIMITEDPallipalayam, Namakkal Dt. - 50KM
4. SAKTHI SUGARS LIMITEDAppakudal, Periyar Dt. - 70KM
5. HARUR CO-OPERATIIVE SUGAR MILLS LTD Harur, -150 KM
DharmapuriDt.

1.2Present Status of the World Cane Sugar Industry

The total crystal sugar manufactured in the world is over1010 million
tones per annum, out of which the cane sugar accounts for 60-65% of the
production, the remaining being the share of the best sugar industry located
mostly in Europe, U.S.A. and some cold regions of the globe.
The cane sugar industry is widely dispersed indifferent regions of the
world like India, Australia, South America, Africa, U.S.A and many parts of
Asia, enjoying tropical warm climate. Based on the types of sugar produced the
cane sugar factories can be classified into two categories as under-

Process Flow Diagram

2
 Cane

Cane Weighment

Cane Feeding

Cane Preparation by
Leveler and Fibrizer

Milling

Mixed Juice Baggase to TNPL for

raw material for paper
Juice Weighment 6 MT making.

Temp 65 – 70*C
Raw Juice Heating
TNPL Boiler
Milk ofLime

Juice Sulphatation
Sulphur gas Ash Steam
R
E Turbine
Sulphited Juice
C Temp 102–105*C
Heating
Y Power Generation
C
L
I Clarification To all electrical
N power drives
G

Mud Clear Juice 12-15 Brix

Filter Clear Juice Heating

Juice Press mud Evaporation 55-65 Brix

Syrup
Temp 78-85* C

Syrup Sulphatation

Pan Boiling

3
 Pan Boiling

A - Pan B - Pan C - Pan

“A” Crystallizer “B” Crystallizer “C” Crystallizer

Batch Centrifugal “B” Continues “C” Continues

Centrifugal Centrifugal

White “A” Light “A”

Sugar Molasses HeavyMolas CF Sugar Final Molasses
ses
“C“ Light
Bagging A -Pan B -Pan Molasses To
Distillery
C -Pan

B -Seed “B” C -Seed For Spirit

HeavyMolas Production
ses
A -Pan C -Pan

Raw Material Input :-

Cane
Intermediates- By Products :-
a). Bagasse
b). Press mud
c). Final Molasses
Final Product Output:-
White Sugar

4
 1. Raw Sugar Factories- cum refineries- In these factories producing raw
sugar from sugar cane, small refining units are uncalled-for processing
the raw sugar and manufacture of refined [Link] refinery can operate
throughout the year even though the raw sugar production is confined to
the crushing campaign restricted to dry periods of the year.

2. Plantation White Sugar Factories-In India and some of the developing

countries white sugar is manufactured from cane for direct consumption
employing more complicated techniques in clarification of juice and also
in crystallization of sugar. The sugar produced is of 99.8% purity and
contains slightly higher amount of impurities than the refined [Link]
plants can also produce raw sugar either for export or supply to refineries.

1.3The Major Components of Sugarcane

1.3.1Sugars
(a) Sucrose- Commonly known as sugar in the popular parlance, this is the
major constituent of sugarcane and belongs to the family of carbohydrates
formed out of ‘C’ ‘H’ and ‘O’. The chemical formula for is C12 H22 O11.

In its pure form this sugar is crystalline in nature. Sucrose content in

fully mature can ranges from 12-15%. Under conditions of low pH or under
influence of certain enzymes like inverts sucrose is hydrolyzed into two
monosaccharide viz. Glucose and fructose in equimolecular proportions
according to equation:
C12H22O11+H2O C6H12O6+C6H12O6
Glucose Fructose
[Link]- Also known as dextrose, this monosaccharide has a chemical
formula [Link] two major monosaccharide viz. glucose and fructose or
laevulose are present in higher amount in the immature can but their percentage

5
decreases as can reaches maturity. In a sugarcane plant the presence of glucose
and laevulose is more marked in the cane tops than in the middle portion of
stalk.

Glucose is sensitive to alkaline condition and heat undergoing

decomposition under action of heat and alkali to from colored compounds. It is
less soluble in water than sucrose.
[Link]- Laevulose or fructose a laevorotatory monosaccharide is present
along with glucose in the growing portions and tops of cane more than in the
main stalks. The empirical formula of fructose is the same as for glucose is i.e.
C6H12O6. Out of the two monosaccharide i.e. glucose and fructose, the
proportion of fructose is less than that of the former.

It is highly soluble in water but less soluble in ethanol and at 30 0C

saturated solution of fructose contains 81.54% of this sugar.

Fructose has a kenotic group in its structure unlike glucose which has
aldehyde group. Being highly susceptible to heat and alkaline conditions it gets
decomposes under these conditions. Like glucose fructose reduces cupric salts.

1.3.2 Starch- Starch is formed by condensation of glucose molecules and is

present in cane juice in small amounts the percentage depending on the cane
varieties as also soil and other natural conditions.

1.3.3Fiber- This water insoluble portion of the sugar cane plant is present in
abundance and forms important component of sugarcane along with sucrose.
The principal constituent of the cane fiber is cellulose and the complex fibrous
structure of the plant is bound together by lignin, pectin and [Link]

6
cellulose is composed of chain of glucose molecules held together closely with
varying degrees of polymerization.

1.3.4Other Organic Polymers- Gums in sugarcane composed of six different

monosaccharide are soluble in water but insoluble in acidified ethyl alcohol.
Though removed in the process to some extent they persist till the final stage
and are present in molasses and to some extent in sugars.

1.3.5Organic Acids and Nitrogenous Compounds - Cane juice is acidic in

nature with pH of 5.0-5.5 stale, immature or frozen cane yields low pH juice
with high among of free acids. Out of the different organic acids aconite acid
claims the major share in the juice from normal cane. Deterioration of cane
after harvest or due to natural causes results ingeneration of acetic acid, lactic
acids etc.

1.3.6ColourForming Compounds and Pigments - Natural pigments like

chlorophyll, xanthophylls and carotene present in the cane plant are extracted in
milling but are eliminated in juice clarification and subsequent boiling
operations.

7
1.3.7 Inorganic compounds- Sugar cane plant during the period of growth
absorbs various minerals from the soils, which are partly dissolved in water and
to some extent are present as organic compounds. Prominent among them are
anions, phosphates, sulphate, chlorides and cations like silica, Iron, aluminum,
calcium, magnesium, potassium and sodium.

1.3.8Lipids- Sugarcane outer surfaces are coated with waxy lipids which are
discernible on the rind of the cane stalk as whitish coating. The fatty lipids and
wax are extracted in milling to the extent of nearly 40-50% and are eliminated
in the filter mud during clarification. These lipids consist of a mixture of
alcohols, free acids and esters. Crude wax extracted from filter cake contains
resins and soft portion or oils a part from hard wax.

1.4Process of Manufacture of Sugarfrom Sugarcane

White sugar by SulphitationProcess
The raw juice after being heated to 65-75 0C is treated with phosphoric
acid, sulphur dioxide and dilute lime solution for removal of impurities in
suspension in a continuously working apparatus.

The sulphur dioxide is generated by combustion sulphur, while lime is

either produced in Kiln from limestone or bought as such and stored in a
separate house. The treated juice on boiling is fed to continuous clarifier from
which the clear juice is decanted while the settled impurities known as mud are
sent to continuous vacuum filter for removal of unwanted stuff. The clear juice
with about 73-75% water is concentrated in a multiple effect evaporator under
vacuum to yield syrup with about 37-43% water content.

The syrup is again treated with sulphur dioxide before being sent to the
pan station for crystallization of sugar. It is at the vacuum pan boiling stage that

8
the sugar crystals appear. The crystal containing mass from the pan is dropped
in crystallizers and subsequently centrifuged in centrifugal machines for
isolating sugar crystals from mother liquor, which again is sent to pan for
boiling and recrystallisation.

Threestages of recrystallisation are adopted to ensure maximum recovery

of sugar in big crystal form. The final mother liquor referred to as final
molasses is sent out of the factory as waste being unsuitable for recovery of
sugar under commercial conditions from economic point of view.

Under conditions of Deccan Sugarcane processing yields-

(a) 27-30% bagasse containing around 46% fibers.
(b) 3.5% filter cake containing 30% dry matter and,
(c) About 4% final molasses containing 80% dry matter besides about
10.5 to 12% crystal sugar which is the principal product of manufacture.

1.5Usesof Sugar
1.5.1Sucrose commonly known as sugar has an important place in
humanlife not only as an article of food but also as an ingredient of various
medicinal preparations and even as a raw material for some products of every
day use. Sugar is thus consumed not only as sweetening agent in the human diet
but also in pharmaceutical, food and other industries.
1.5.2 Sugar which is formed by photosynthesis in plants from suns energy
is a natural food for all living beings. In the human system, when taken orally,
the sugar is attacked in the stomach by hydrochloric acid of the gastric juices
and converted into glucose and laevulose. In the small intestines these sugars
are absorbed through the intestinal capillaries in the portal vein whence they are
carried to liver and stored there.

9
 Sugar above a certain level in blood is converted into a polysaccharide
known as glycogen to be decomposed into simple dextrose and used whenever
sugars level of blood falls below certain limit. Energy required for any activity
of the brain or muscles is supplied by dextrose getting oxidized into CO 2 and
H2O. The sugar taken orally raises the blood sugar level in the human system
within five minutes. Sugar thus serves as a source of quick supply of energy to
the body for any physical or mental activity.

1.5.3Food products - Sugar serves as a good preservative for edible

products which can keep well in concentrate sugar solution for quite some time
without deterioration. Fruit preservation and canning is a big industry in
advanced countries of the world. It is widely used in beverages in tea, coffee
etc. In most of the countries and forms the principal raw material base for
candy as well as confectionery industries.

1.5.4Pharmaceutical and Other Industries - Sugar Syrups i.e.

concentrated sugar solution containing on of more medicinal ingredients are
quite common. In smaller amounts sugar is used for coating for medicinal
tablets or pills which are better in test, so as to make them palatable. Apart from
these, following products can be manufactures with sugar as base?

(a) Sorbital used in diabetic food and for producing ascorbic acid.
(b) Lactic acid which forms an important chemical intermediate in food
pharmaceutical and leather industry is produced by action of lime on
sucrose and hightemperature 240ºC.
Oxalic acid is manufactured by oxidation of sucrose by nitric acid.
(c) Sucroseoctaacetate produced by the action of acetic anhydride and
sodium acetate is used as adhesive, plasticizer etc.

10
 (d) Nonionic surfactants are manufactured from sucrose and fatty acidic.
These surfactants with good wetting properties are widely used in food,
pharmaceutical industries and cosmetics. As detergents these
surfactants have gained wide acceptance in the market.

CHAPTER-II
AIM AND SCOPE

The project is about “Role of Heavy ChemicalsUsed in Sugar

Industery’’
In terms of

11
  Treatment of cane juice.
 Chemical used in sugar manufacturing process.

2.1 Chemicals Used Are:

 Phosphoric Acid: To promote physico chemical reaction.
 Lime as milk of lime: Maintaining clear Juice pHaround 7.0.
 Sulphur as SO2 gas: Used as a bleaching agent and maintain the pH range.
 Flocculent: Used to increase the mud-setting rate in clarifier.
 Mill Sanitation Chemicals: Used to avoid microbial inversion loss in
mills.

These chemicals are used to improve the clarification.

CHAPTER - III
REVIEW OF LITERATURE

 Lime is still they only chemical used in making raw sugar, as was true
twelve centuries ago in Egypt. Lime and sulfurous acid, or lime, sulfurous
and carbonic acids are used in making plantation – white and near – white
sugars. These three reagents are the only ones that enter directly into the

12
 current processes. It is probable that more than 90 percent of the world’s
cane sugar made with lime as the only chemical entering the process.
([Link], 1923)

 The mixed juice from extraction is preheated prior to liming so that the
clarification is optimal. The milk of lime, calcium hydroxide or Ca(OH) 2,
is metered into the juice to hold the required ratio and the limed juice
enters a gravitational settling tank: a clarifier. The juice travels through
the clarifier at a very low superficial velocity so that the solids settle out
and clear juice exits. (Joachim [Link] et al, 2006)

 The evaluating various liming techniques, namely fractional, intermediate

and hot liming involving milk of lime and lime saccharate, the results
indicated that intermediate liming was more effective(53%) than
fractional liming with hot liming giving the lowest juice turbidity. In
addition all saccharate liming produced with clear juice (51%) than milk
of lime methods.(K.T.K.F Kong Win Chang et al, 2006)
 A number of commercial flocculants – both anionic and cationic ones –
and their effect on clarifier underflow (clarifier mud) filtration rate were
measured. Contrary to some previous reports, the high molecular weight
anionic flocculants were found superior to the cationic flocculants. The
same flocculants that are effective in the juice clarification stage were
found also effective for mud conditioning at 10 mg/L mud. At that
addition level, the filtration rate is increased with respect to the no –
flocculants case by up to five-fold. (Michael Saska, 2006)

 The filtration of muds formed by the defecation of cane juice is an

important step in manufacture of raw sugar. In the effort to obtain a good
filtration rate by the addition of excess quantities of milk of lime to the

13
 mud, the fact that the percentage of harmful impurities – namely, lime
salts and colloids-will be increased in the filtered juice by this practice. Is
frequently over looked. Considering all factors, it was concluded that the
muds should be limed to a pH value not exceeding 7.8, and that the
properly filtered juice may be added to the clarified juice without
detrimental effect and sent directly to the evaporators. ([Link] et al,
1928)

 The sulfiter and the treatment of the juice play a very vital role in
clarification of the juice. To get better results the juice is shock – limed a
pH of 9.0/9.2 and then neutralized to 7.1/ 7.2 pH by the addition of SO 2.
The use of a continues film – type sulfur burner has provided the
advantage of maintaining a very uniform SO 2 gas concentration. With the
use of refrigerated air for the burning of sulfur, sublimation of sulfur is
eliminated, there by avoiding choking of the gas pipes normally
experienced with most conventional sulfur burners. The system of juice
sulphitation has given good reaction of the juice with the reactants like
milk of lime and SO2 used in the process of sulphitation, resulting in a
better clarification efficiency and improved clarity of juice.
(MullapudiNarendranath, 2006)

 The direct determination of plant – food ingredients in cane juices is

suggested as a logical and easily applicable means of getting an
approximate idea of fertilizer requirements of cane soils. A large number
P2O5 determination in crusher juices indicated that this element was fairly
constant for a given field and, in general, for a given elevation, although
marked differences existed between canes grown at different elevations,
the lower fields producing juice containing the most P2O5. As a
preliminary standard 0.020 % P2O5 (g /100 cc. crusher juice) is suggested.

14
 Fields averaging probably contain sufficient available P2O5 for maximum
cane yields; a lower figure calls for field experiments. Where juices run
less than 0.010 %, some phosphate should be applied as a precaution,
even in the absences of experimental proof that it is needed.(Herbert.
Walker, 1923).

CHAPTER – IV
ROLE OF HEAVY CHEMICALS USED FOR PROCESS

1. Lime
2. Sulphur
3. Phosphoric acid
4. Flocculent (settling Aid)
5. Mill Sanitation chemicals

4.1 Lime
Lime Stone

15
 It is kind of stone available in nature. The stone is in the form of rocks
and rich in calcium carbonate and it is the (CaCO 3) Calcium Carbonate, which
is systematic burning kiln, produces quick lime or CaO, which is useful for
juice clarification.

CaCO3 + Heat CaO+CO2 (endothermic reaction)

A good lime stone should contain with the following specification.

1. Calcium Carbonate - 95% (minimum)

2. In soluble matter - 20% (maximum)
3. Magnesium Oxide (MgO) - Below 1%
4. Iron Oxide and Alumina (Sesquiodixe) - Below 2%
5. Silica - below 1.0%
6. Sulphates - below 0.5%
7. Moisture - below 2.0%

The above impurities from lime stone passes one to quick lime in spite of
very systematic burning in the lime kiln. Therefore in the limestone burnt the
factory in the own kiln it should confirm with the above standard.

Many factory purchase quick lime directly from lime manufacturer. The
prominent being as under.

1. Non-availability of assured supply of good quality of steam coal.

2. Non-availability of skilled labor at reasonable cost to carryout limestone
burning operation.
3. Non-availability space in the factory premises for erecting limekiln.

16
 4. Preparation of the lime kiln result in the air pollution due to emission of
CO2 gas and therefore the risk of attracting profusion from the anti air
pollution authority.

In the case of these factories, which purchase of quick lime (or) hydrated
lime from the supplier. The lime should confirm with the following
specifications.

Preparation of Milk of Lime or Lime Cream

Preparation of lime cream requires careful supervision. The milk of lime
should be prepared 3-4 hrs before its use.

The formation of Ca(OH)2 from quicklime is exothermic reaction.

CaO+2H2O Ca (OH) 2+ 63.6 KJ
Since only one part of dissolves is 79 parts of the result of lime slaking
process is portion (or) dispersion of finely divided Ca(OH) 2 particles in limed
water.

1Beaume = 1.8 Brix

Milk of Lime Storage Tank
Lime storage tank is a cylindrical tank in which vertical axis is provided
which is the part of the stirrer with a rake of a hanging chains which revolve
round and high rubbing against the bottom of the tank prevents any lime
accumulating at the bottom. The speed of the stirrer should be 8 to 10 RPM
(Revolutions per Minute).

Practical Consideration
(i) To ensure good slaking full time should be allowed for the reaction i.e.
it should be take 3-4 hrs to slake before use.

17
 (ii) Water should be pure and hot for this the condensates from the second,
third and fourth the bodies of the evaporator are suitable.
(iii) The slacker should rotate 6 to 8 RPM speed. Higher speed will
discharge the lime from the slacker, which will help complete slaking
of lime.

The grit from discharges lime coming out of the lime slacker is removed
by equipment called as “lime clarifier”.

The grit free lime from the lime clarifier is then screened on 14 mesh
sieve and its stored in a primary storage tank, were the density of lime is around
15 to 20 Beaume (1 Beaume = 1.8 Brix). This relatively high density of milk of
lime then flows into lime collection tank where after suitable dilution with pure
water the density is adjusted to 10 to 12 Brix and this lime from collection tank
is pumped to the lime proportionate device. This device regulates the dose of
lime, which is to be added in the heated raw juice in liming and sulphitation
tank.

4.1.1 Lime Analysis

Aim
To analysis the CaO% and grit % of the burnt lime.

Apparatus and Chemicals Required

 Burette
 Pipette
 250 ml standard flask
 250 g sub sample lime
 N/2.8 H2SO4

18
  Phenolphthalein indicator

Method of Sampling
The burnt lime sampling is being done normally from 15% of the total
bags of lime received and from each bag about 250g of lime taken out. The total
quantities thus collected in a backed us against sub sampled for 1 kg. Kept in a
polythene bag and tightly covered to avoid absorption of moisture.

Analytical Method
About the 250g sub sample lime is taken out and ground well in a pestle
and mortar 5g of lime powder is weighed accurately immediately after the
powdering is done and is dissolved in a 250 ml standard flask using to 100 ml of
freshly boiled distilled water. The flask is then heated and the lime solution is
boiled for 3minutes for the evolution of CO2 then it is cooled.

About 40-30g of white sugar is dissolved in about 50 ml of boiled

distilled water. The cooled sugar solution is added to the lime solution in 250 ml
standard flask (both the solutions should be in the room temperature).

The solution is mixed well and filtered 25 ml of filtrates and is pipette out
in a conical flask and titrates against N/2.8 [Link] had already been
standardized using the indicator phenolphthalein. The end point is
disappearance of pink colour. The titrations are repeated for the concordant
values.

Calculation:-
CaO% = 2 x T.V x Strength of acid
= 2x 36.1x1.105
= 79.78.

19
4.1.2 CaO Content in the mixed juice and Clear juice
Aim
To determine CaO content in the mixed juice and clear juice by EDTA
method.

a)Chemicals Required:
1. M/56 EDTA (ETHYLENE DIAMINE TETRA ACETIC ACID)
solution (6.6473 g di sodium salt of ethylene diaminetetra acetic acid
is weighed accurately, dissolved in distilled water and made up the
solution to 1000ml.
2. Ammonia
3. Lead subacetate: Horne’s dry lead.
4. Potassium Ferro cyanide (Merck quality) powder.
5. Erichrome Black T (weight 0.1 g of Erichrome Black T in 100 mL
rectified spirit or absolute alcohol).

b) Apparatus Required
1. Calibrated Brix Spindle.
2. Brix cylinder
3. 250 ml Conical flask
4. 100 ml Beaker and Funnel
5. Calibrate 10 ml pipette.
c) Procedure
Take the juice, syrup or molasses sampled as obtained from the factory.
In case of juices no dilution is require. In case of molasses, dilute to 5 Brix.
Transfer about 150 ml of the juice or diluted solution into a conical flask.
Clarify the solution by lead sub acetate as in Horne’s method (Add if necessary
some amount of active carbon).

20
 Transfer about 60 ml of the clarified solution into a dry conical flask or
flask previously rinsed with the clarified solution. Add powdered Potassium
Ferro cyanide little by little till not further precipitate forms. Shake thoroughly
and filter. Test the filtrate for absence of lead with potassium iodide. Clean
conical flask previously rinsed with distilled water and dried. Add 5 drops of
ammonia and add a few drops of the indicator solution of EBT when a pink red
colour appears. Titrate against EDTA solution shaking the contents of the flask
after additional of EDTA solution. The end point is indicated by the sharp
change of colour from red to blue know the volume of titrant.

Calculation:-
1. Observed (Un corrected Brix) =B
2. Titration reading =Vml

Formula:
Amount of Ca++ is expressed as CaO = Vx100 mg per liter of juice or diluted
solution.
= V x 100 mg per liter per 100 Brix.
B
Mixed juice Clear juice
= 8.7 x 100 = 15.7 x 100
10 10
= 870 mg/litre = 157 mg/litre

[Link] Mixed juice mg/litre Clear juice mg/litre

1. 870 1570
2. 930 1460
3. 830 1420
4. 700 1370
5. 850 21
1440
6. 950 1350
4.2 Sulphur
Sulphitation Process
Purification of juice employing SO2 gas and milk of lime is called as
sulphitation. This process was first invented in European beet sugar industry
and later was introduced in java by end on 19th century was operating
successfully than country before the II world war. When the java sugar industry
was a model of the other sugar industry of the world, on account of innovation
introduced the research were carried out and the technological advances
achieved. Almost 85 to 90% of white crystal produces by vacuum pan sugar
industry. In India is manufactured by sulphitation process of clarification.

Chemistry of SO2
Sulphur occurs as an element in USA, Sicily and to a smaller extends in
Japan and France. Sulphur also occurs in abundance in combined form as
sulphides of Lead, Iron, Zn and Cu.

As sulphate gypsum or calcium sulphate is of wide occurrence the main

use of sulphur is for the manufacture of H2SO4 one of the most important
chemicals used is various industry. Sulphur obtained can 99.9% pure.

Properties
Sulphur has an atomic weight of 32.06, which melts at 130 oC. It
vaporizes at 444oC when heated out of contact with air. One account of its self
sustained burning characteristic. A mass of pure sulphur once ignited burns
completely in air.

22
SulphurDiOxide (SO2)
Sulphur is available in two forms, namely rock sulphur and roll sulphur.
Roll sulphur is pure than rock sulphur.

Combustion of sulphur
SO2 is a gas resulting from combustion of Sulphur.
S+O2 SO2 +293 KJ
32 g+32 g 64 g

Hence 1kg of sulphur requires1kg of O2. The reaction releases us 293KJ

or 221k. Calories 1kg of sulphur-di-oxide Combustion takes place of a
temperature about 360oC. If the combustion were it take place with theoretical
quantity of air would be 4.3 times the weight of sulphur. This is the quantity of
air required. (The air contains 23.15% of O2 by weight). Similarly the maximum
volume of SO2 in the combustion gases is about 21% (Air contains 20.84% of
O2 by volume).

However it is not possible to obtain complete combustion with this

amount of O2 and it is necessary to allowed excess of air above the theoretical
level. In actual practice pure SO2 obtained in the burner gas mixture would be 8-
14% on an average 10%. The remaining components of the burner gas are free
air, Nitrogen, Oxygen and a small extend SO3.

Precaution
In the presence of moisture sulphur burns to give sulphuric anhydride i.e.
SO3 instead of sulphurous anhydride. On reacting with moisture SO 3
immediately forms sulphuric acid. It is therefore absolutely necessary to

23
exercise greatest possible care to avoid introduction of water into the sulphur
furnace. The air to be used for burning of sulphur should always be dried. For
this the air is generally passed over a layer of quick lime which has got great
affinity for moisture and absorbs moisture from the air. It is advisable to renew
quick lime pieces in the air dried before it is completely saturated.
Preparation of SO2 Gas
Sulphur heated to 250oC is oxidized to sulphur dioxide with evolution of
heat which heats the sulphur in the burner and rises its temperature to the point
of oxidation in present of air. The molten sulphur is first vaporized and the
sulphurvapour in contact with air form sulphur dioxide. Vapour pressure of
sulphur increases with temperature and unless sufficient air is supplied,
complete conversion of sulphur to SO2 gas is not possible.

The mixture of sulphur dioxide and sulphurvapour when cooled results in

sublimation of sulphur. Secondary a small portion of SO 2 is gets oxidized to
SO3 (sulphur trioxide) as per the following reaction.

2SO2+O2 2SO3

This reaction is exothermic and more SO2 is in equilibrium at low

temperature second factor is supply of sufficient air for completion of SO 2
formation. Since in adequate O2sulphurvapour would remain unreacted and can
be carried with the gas.
Sulphur dioxide generation station consists of (a) a burner combustion
chamber (b) gas cooler (c) scrubber (d) air drier and air compressor is very often
located in close vicinity of the lime station.

A sulphur burner designed to work continuously is composed to three

parts.

24
 1. SulphurMelter
2. A Chamber for molten sulphur
3. The burner or a combustion chamber was Sulphur is converted into
SO2

The chamber for molten sulphur serves as feeding chamber to the

combustion chamber. A live steam of about 5.0 kg/cm (70-75 pounds per square
in gauge) is supplied to the steam chamber to melt the sulphur in the
sulphurMelter.

4.2.1 Analysis of Sulphur

Aim
To determine the purity of Sulphur.

Procedure
Percentage of Sulphur
a) Take 10 gm of properly mixed Sulphur sample in a beaker.
b) Add sufficient carbon disulphide to dissolve all the Sulphur.
c) Decant the carbon disulphide. Heat residue for half an hour in hot water
bath.
d) Now add more carbon disulphide and dissolved more Sulphur if possible.
e) Decant the CS2 and wash several times with the same.
f) Allow the beaker to stand for some time when the CS2 will evaporate.
g) Weigh the beaker and residue.

Calculation
Percentage of residue = weight of residue x 100
10
Percentage of Sulphur = 100 - (% moisture + % residue)

25
 = 100 - (0.04+0.06)
= 99.90.

4.3 Phosphoric Acid

Purpose of Addition of Phosphoric Acid in Raw Juice
The phosphate content of the juice is the most important factor in
efficient clarification. In sugarcane, the phosphates are inorganic as well as
organic. The inorganic phosphates exist as free phosphate ions, where as the
organic exists in the form of phospholipids, phospoproteins, nucleotides
phosphates and hexose phosphates.

It is understandable that only the free phosphate ions take part in juice
clarification. Therefore juice with adequate quantity of inorganic phosphates is
most desirable. Generally phosphate is most phosphorous content is sufficient
for better clarification. Since the phosphate content in juice is normally less that
the desired level. Orthophosphoric acid is added in raw juice to 350ppm. The
addition is about 0.0005% on cane.

Reaction Involved in Phosphoric Acid and Clarification

The Phosphoric acid presents in the mixed juice in the form of soluble
phosphor and has practical significance. The P2O5 reacts with lime to form
various calcium phosphate and tri-calcium phosphate.

CaO + H3PO4 CaHPO4 + H2O

CaHPO4 +2CaO+ H3PO4 Ca3(PO4)2 + 2H2O 3CaO +
2H3PO4 Ca3(PO4)2 + 3H2O

26
 Intermediate precipitation of CaHPO4 which later dissolves with great
slowness, the slowness and slow rate at which Ca3(PO4)2 precipitate the two
following reaction takes place simultaneously.

Ca2+ + HPO42- CaHPO4 ------ (1)

3Ca2+ + 2(PO4)2- Ca3(PO4)2 ----- (2)

The first reaction is more rapid because it is a second order reaction

involves two ions while the other is a higher order reaction involving five ions.
The probability of two ions coming together is much greater than five. As a
reaction approaches completion. The rate of the reaction (1) slows down the
reaction exceeds it. This result in further dissociation of second order reaction
Hand PO43- process which cause decreases in pH.

4.3.1 Phosphoric Acid Analysis

Aim
Determination of available P2O5 in Phosphoric acid.
Procedure
Take 20 g of well mixed sample of Phosphoric acid in 1000 ml standard
flask with 800 ml water and shake for half an hour then till the flask up to mark
and then used for titration.

100 ml (or) equivalent of 2 g prepared solution in conical flask add 3 to 4

drops of phenolphthalein indicator and titrate with 1N sodium hydroxide
solution and end point is colourless to pink.
As phenolphthalein show naturally as soon as the sodium salt is formed,
every ml of 1N NaOH is equivalent to 0.0355 gof P2O5.
1 N NaOH = 40 gms of NaOH 1000ml
% P2O5 = T.V x 0.0355 x 1000

27
 20
= 41.6 x 0.0355 x 1000
20
= 73.84%
4.3.2P2O5 Content in the Mixed Juice and Clear Juice
Aim
To determine P2O5 content in the mixed juice and clear juice by Uranium
Acetate method.

Uranium Acetate Solution

Dissolved 35 g of chemically pure uranium acetate in distilled water and
add 50 ml of chemically pure glacial acetic acid and made up to 1 liter.

Standardization of Uranium Solution

Dissolve 9.583 g of potassium phosphate (KH2PO4) in one liter of water.
Dilute 25 ml of this solution to 100ml. Add uranium solution from a burette to
the cold phosphate solution till a few drops drawn with a pipette given a brown
precipitate on a drop reaction plate dusted with potassium Ferro cyanide. Heat
the solution to 90-100oC and add uranium solution till a precipitated appears. 25
ml of uranium acetated till be required. Adjust to the corrected volume if
necessary.
When a 100 gm sample is titrated with each ml of uranium solution is
equivalent to 0.005% of P2O5.

Procedure
To 100 ml of juice and 1 ml of 10% NH 4OH solution and acetify with
acetic acid and add 10 ml of sodium acetate solution (100 gm of Sodium acetate
and 50 ml of glacial acetic acid per liter of distilled water).

28
 Titrate with standard uranium solution. Using powdered potassium Ferro
Cyanide as indicator. The solutions will usually settle sufficient to pipette of a
small portion of clear liquid for the end point determination nearly the whole of
the uranium solution should be added in the cold and the titration finished at 90-
100oC.

When the solution contains the slightest excess of Uranium the addition
of drop of solution to the Ferro cyanide on a drop reaction plate produced a
brown precipitate of uranium Ferro cyanide.
Calculation:-
P2O5 volume used = Vml
Weight of juice = w gms
i.e. 100 ml of juice = 100 gm of juice
Before addition:
The Amount of P2O5 = 0.005 x V x 1000
100
= 0.005 x 4.6x 1000
100
= 230 mg/lit.
After addition:
The Amount of P2O5 = 0.005 x V x 1000
100
= 0.005 x 6.4 x 1000
100
= 320 mg/lit.

29
Phosphoric acid before addition and after addition in mixed juice and clear
juice
[Link]. Mixed juice mg/lit Clear juice mg/lit
Before After Before After
1. 185 285 110 150
2. 245 365 100 125
3. 230 320 95 140
4. 200 365 125 155
5. 270 325 85 105

4.4 Flocculants (Settling Aid)

Purpose of flocculent is to improve flocculation and increase settling rate
of mud in the clarifier. The basic chemical present in these flocculants available
in the market is called “Polyacryl amide”. Common brand of flocculent
available in market are.

1. Sedipure DF-2 German products

2. Sedipure AF 200
3. Seperan AP 300 American product
4. Mango floe LT 27 British product
5. Nalco
6. Tulsipar Indian Products
7. High floe
8. Dai-Idu-Indian-Japanese product

Properties
Some times normal practice and precautions followed in the process of
juice clarification do not give desired clarity in the clarified juice and also leads

30
to higher mud level in clarifier. Under such condition suspension or dispertion
of the chemical known as “flocculent” is applied to the boiled sulphited juice
entering the clarifier in adequate doses.

Now a day there are number of flocculants available in market. Some are
crystalline in nature and some of the semi solid nature in the jelly form. The
basic chemical underlined these flocculants is polyacrylamide. This chemical
facilitates better flocculation of the mud flocks from the sulphited juice which
increase the settling rate of mud floes in the clarifier. These are polymers having
very high molecular weight to the order of 0.15 to 0.3 million. Normal dose of
flocculent are in the rang of 2.6 ppm (parts per million) as compared to juice.

Name of the Colouring Impurities Present in Juice

1. Chlorophyll
2. Xanthophylls
3. Crotone
4. Saccharetin
5. Tanin
6. Anthocyanin

4.4.1 Methodsof PreparingFlocculent Suspension

1. Take necessary weight of flocculants.
2. Generally to separately cylindrical tanks of 1-2 m.t (millitonnes) capacity,
are connected to each other having mechanical stirrer and common outlet
piping is used both the tanks are provided with hot water connection.
3. Then hot water in one of the tank to 1/3 level sprayed the flocculent
powder in the hot water of the tanks in installment and allow the stirrer to
mix the content thoroughly for about 10-50 min.

31
 4. Take same more water in the tank and add second installment of the
flocculent when the contents are continuously being stirred.
5. In this way dissolve all the flocculent dose in hot water until the tank full
at desired level. Take one precaution essentially that no lumps of
flocculant should be formed during mixing as they may block the pipe
lines.

When one tank is being prepared the flocculant solution from other tank
should be used. The cost of flocculant is approximately Rs.165/ kg.

4.5 Mill Sanitation Chemicals

The prevalence of micro organisms in freshly extracted cane juice their
ability to induce losses of the recoverable sucrose having in greater Delong
study of means the reduce in loses by the addition of some ‘biocide’. As
delivered to the mil, the sugarcane states contain high concentration of bacteria.

There are eight species in freshly extracted cane juice.

1. Saccharomyces- carlsbergensis
2. S. cerevisiae
3. Alcoholophila
4. Sichiamembranafacious
5. Candida krusia
6. Torrulopsisstellada
7. C. Guilliermondi
8. [Link]

The sugarcane rings to the mill high concentration of vibal micro-

organism but most of them are washed off in the extracted juice where if the

32
temperature level with in the growth limit microbial development in gently
occurs.

The application of modern biocides for the prevention of mill loser is

justifiable and may prove especially effective when grinding damaged cane.
The interaction between the microorganisms various sugars present in juice
reduce sugar recovery as well as cause various problems in juice clarification
due to increased viscosity and turbidity.
By good house keeping of the mills station the application of steam and
water jets at the joints and chain links can be 60% effective. The remaining
bacterial concentration i.e about 40% can be deactivated by applications of
appropriate biocide.

The biocide i.e. nowadays commonly used as the following composition.

1) Disodium cyanodithiocyanodiamido carbonate

2) Ethylene diamide
3) Potasium “N”- Methyl dithio carbonate
Indion9053 used in the salem-co-operative sugar mills Ltd, Mohanur. It
cost is approximately Rs. 45/kg.

4.5.1 Mill Sanitation Chemicals Analysis

Estimation of Active Content for Biocide
(Di ThioCarbomate Base)

33
Aim
To estimation of active biocide in mill sanitation chemicals.
Procedure
Sample:
Take 4-5 g of biocide is added to 200 ml of distilled water and add 2-3
drops of phenolphthalein indicator. Incase of pink colour formed add 0.1N
H2SO4 till colourless. Then add 50 ml of 1N H 2SO4 and this solution is boil for
30 minutes and cool and titrate against 1N NaOH. The end point is the
appearance of pink colour.
Blank:
Take 200 ml of distilled water is added to 2-3 drops of phenolphthalein
indicator and add 50 ml of 1N H2SO4 and the solution is boil for 30 minutes and
cool and titrate against 1N NaOH. The end point is the appearance of pink
colour””””””””””””””””””"Calculation
Active biocide in mill [Blank – Sample] x Normality of NaOH x7.18
=
Sanitation chemicals Weight of sample
(25.9-0.6) x 1 x 7.18
=
5
= 36.33 %

CHAPTER – V
PROCESS INVOLVED IN SUGAR PRODUCTION

34
5.1 MAXWELL BOULOGNE
Juice Weighing Scale
Juice weighing the most common type of prevailing in Indian sugar
industry. Maxwell Boulogne design operating for levers and counter weights.
It’s consist of
1. Over head juice receiving tank.
2. Weighment tank
3. System of levers, counter weight and valves for the two tanks
4. Weighed juice receiving tank.

The top rectangular tank receives the juice continuously which flows into
cylindrical weighment tank provided with small vertical baffle at the conical
bottom with a hole, which retains certain amount of juice. After the weighing
tank is discharged and this arrangement help to maintain a constant weight.

As soon as the completely discharged and the tare weight of weighing

tank is reached, the counter weight which is in the raised position caused tilting
of the weigh beam. There by raising the empty weighing tank. The two valves
of the top juice tank and weighing tank are fitted to a common steel rod in such
a way that when upper one get open the lower one is closed and vice versa and
are operated only by the upward and downward movements of the weighing
tank. When the weighing discharged the inlet to the same is closed.

A scale of this type is usually designed for 25-28 discharge tips/ hr. a
totalizer or a digital counter is attached to all modern scales for indicating the
number of tipping. The tare chamber has to be maintained free function
properly and the juice weight in accurate.

35
5.2 Juice Clarification
The raw juice (or) mixed juice obtained from the mills is weighed in
automatic juice weighing scale and required quantity of O-Phosphoric acid is
added into the weighed raw juice so as to get phosphate level in juice 300-350
mg/liter. Weighed raw juice is heated to the temperature of 70-75°C in a raw
juice heater, which is heated by, normally vapours from Second body of the
Evaporator.

The heated raw juice is then passed into a liming and Sulphitation tank
which is also called as juice Sulphitor via so2 gas absorption tower. The vent
pipe of juice Sulphitor is connected to the gas absorption tower at the bottom so
that the residual SO2 gas left after its due absorption in the juice Sulphitor finds
its way in the stack gases which enters in the gas absorption tower. The heated
raw juice enters the gas absorption tower from the top and travels downward
through and over the baffle plates fitted in zigzag manner in the tower.

The milk of lime enters the outlet juice of gas absorption tower at a
suitable point so the pH of the limed juice remains in the range 9.5 to 10.5 of
about 10 to 15 seconds before it is neutralized by SO 2 gas entering the juice
Sulphitor at the bottom. The incoming SO2 gas comes out through the gas
spargner for uniformed distribution of gas in juice. The commonest spargner is
designed are
 Perforated coil type
 Perforated cross type.
The perforation on the coil is cross should face downward. The following
physico chemical reactions take place in juice sulphitor.

5.3 Physico Chemical Reactions

36
  Most of the colloidal non sugars from juice get coagulated due to hest
and addition of milk of lime. Most of the colloidal non sugars are
coagulated.
 Ca from juice and Ca from milk of lime react with phosphates from
juice to form insoluble precipitate of tricalcium phosphate (Ca3
(PO4)2).
 Some of the coloring impurities are absorbed by the tricalcium
precipitate.
 Calcium from juice and calcium from milk of lime reacts with SO 2 gas
to form insoluble ppt of calcium sulphate (CaSO3). Due to reaction
with SO3 which is always present in Sulphur burner gas in a small
proportion forms calcium sulphate (CaSO4)
 Due to action of SO2 gas some of the colouring impurities from juice
are bleached off.
 Due to action of SO2 gas viscosity of the juice is reduced.

The treated limed and Sulphured juice is then heated to 102°C to

104°C in Sulphured juice heaters. The primary heating is done by means of
vapour from 1st body or vapour cell of the Evaporator to the temperature of 900C
to 950C and in secondary heating of the Sulphured juice the temperature is
raised to 1020C to 1040C by means of exhaust steam of 7 to 9 psig (Psig -
pounds per square in gauge).

The heated Sulphured juice is then released into continuous juice clarifier
via flash tank. The heated Sulphured juice enters in the juice clarifier firstly in
the flocculation chamber in tangential manner. The juice then decant down the
clarifier through the centre tube called as ‘recess’.

37
 Firstly the bottom most compartment gets filled and than the above
compartment. In this manner the entire clarifier gets filled with juice. The bed
plate of the each compartment is stopping towards the centre. There is juice box
and mud box situated at the top of the clarifier. In some clarifiers there are to
two juice boxes and one mud box. The mud from the mud boots of different
compartments in conveyed to the mud box by individual pipes with value to
control the mud flow.

Similarly clarified juice is drawn from the upper most portion of each
compartment and is conveyed to the juice box by means of separate pies and
valves. The mud from the mud box overflows into adjoining compartment of
the box which is conveyed to the Rotary vacuum filter section by separate
piping. This mud is mixed with specific quantity of bagacillo and is the mixture
is fed the Rotary vacuum filters which separate the filtrates from the mud solid.
The combined filtrates, which are about 15 to 20% of the juice quantity, are
recycling into weighed raw juice.

The mud solids get accumulated over the perforated screen of the
[Link] (Rotary vacuum filter) in the form of filter cake. The filter cake
detached from this screen by means of scrapper plate, which falls into screw
conveyor or belt conveyor which conveyed the filter cake trolley. This filter
cake important by product of the sugar factory, which have get very good
manure value.

The clear juice emerging from juice box of the clarifier has the
temperature of 900C – 950C and the pH of 6.8. to 7.0.

Juice Heater

38
5.4 Construction of Juice Heater:
The tubular juice heaters are cylindrical cells fitted with two plates and
both ends, the tube plates are provided with baffles beyond the tubes so as to
divide the two end portions of the heater into compartment.

The compartment of juice entry and exit have only one pass and the
remaining compartment have two passes i.e. are upward and downward flow.
Multiple circulation of juice is achieved by providing double the number of
juice in each compartment i.e. for 12 tubes per pass the compartment will be
fitted with 24 tubes. The shell heaters and tube plates are of mild steel
construction. But stiffeners are welded to the covers to enable than to withstand
high pressure of circulating juice. These covers are hinged to the body of the
heater and closed by hinged bolts of sufficient strength.

In the case of vertical heaters the doors are balanced by counter weighs.
The juice heaters are equipped with two double beet valves. According to
practice followed in India and usually the same heaters are operated for Raw
and Sulphured juice on alternate days to prevent accumulation of scales. The
doors are provided with corks one for each compartment. The corks and the
corks provided on the bottom cover are called as drain corks.

Solid drawn brass tubes of 42mm ID (Inner Dia) and 1.5mm thickness are
common Indian sugar industry. The length of the tubes varies from 3 to 4
meters. Many factory they are using S.S. tubes instead of brass tube. The juice
velocity is about 1.8 to 2.0 meter/sec. Higher velocity of juice is conductive to
higher rates of heat transmission.

39
 The steam or vapour connection is provided in the upper half of the shell
about ¼ the height from top of the heater, in the case vertical juice heaters to the
facilitate drainage of the condensates.

With horizontal heaters the steam entry is close to one end of the shell.
The incondensable gas vent is open to atmosphere when steam is the heating
medium bleed vapour are to be used the vent pipe has to connected to a vacuum
system. The incondensable gas should be drawn from top as well as from
bottom of the shell.

The heat transmission from heating vapour or steam to juice is affected

adversely by scale on the heating surface of the heater, which gradually
develops during running. The total installed heating surface of juice heater in
modern plants in around 6.5 to 7.0m i.e. to five heaters one of which is always
under cleaning.

Vapour line juice heater is installed of the vapour line of the last body of
the evaporator, before the condenser for cold raw juice heating. Since the
temperature and pressure with consequent small temperature difference between
cold juice and vapour rise in temperature of 10-15 0Ccan be achieved in the
vapour line heater if the heater is properly designed.

5.6 Dorr Clarifier:

40
 The first successful modern continuous system of mud settling was
introduced in Cuba in 1918 and gained Rapid favour through the world. The
latest design produce by the company is known as Rapi- Dorr- 444.

41
 The Rapi - Dorr - 444 consists of 4 compartments with separate provision
for free over flow take off and mud withdrawal system allowing the unit to
operate as 4 totally independent clarifier enclosed in a common housing.

As in ordinary old Rapi Dorr model juice is introduced at the top centre
of the each compartment through the hollow rotating centre tube. As the feed
entered each compartment its strike the reflector baffle and flows out wards at
the decreasing velocity creating minimum turbulence rotating rake arms or the
stirrer arm in each compartment moves the settled mud to the mud discharged
boot at the centre of the tray where from the mud is drawn separated by a
combination of pipe and valves leading to the mud box situated at the top. Each
compartment has its own overflow pipeing to remove the clarified juice at the
multiple points around the periphery.

A single over flow box collects the clarified juice from all the
compartments with more uniform juice takes off; the potential stagnant pockets
are eliminated.

The juice clarifier is free from excess vapour and volatile gases. This
prevents the disturbance of settling mud in the clarifier.

5.7 Vacuum Filters

The typical and more widely used filter of the class is the Oliver campale
filter. The filter consists of a hallow drum rotating about its horizontal axis and
partly submerged in the liquid to be filter. The periphery of the drum serves as
filtering surface. It is divided in 24 independent sections, each occupying 15
angles on the circumference and extending along the full length of the drum.

42
Each of these sections are connected individually to a vacuum system by a
small middle pipe terminating into a distribution valve called as “Trunion
valve” situated at one end of the drum and carrying three differing sectors.

 One with connected to the vacuum but connected to the atmosphere.

 The second connected to the chamber were the low vacuum of the
order of “6 to 12” of Hg (i.e. 150 to 300 mm of Hg) is maintained.
 The third connected the chamber were a high vacuum is maintained of
the order “15 to 20” of Hg

The exterior surface of the drum consists of a sheet of stainless steel with
very fine perforation i.e. 0.2. to 0.4 mmdia hole.

5.8 Working of R.V. Filter:

Before starting the R.V. filter the vacuum system must be checked by
filling water for possible leakage.

Necessary quantity of muddy juice should be taken from the mud box of
the clarifier in the mud [Link] should be taken into the mud
bagacillo mixture by starting the air blower at the mills.

After ensuring paper mixture of mud and bagacillo, the mixture or feed
should be taken Oliver filter tray until the tray is just full. The filter drum should
be put into motion and its speed should be kept in the range 4-6
minutes/Rotation.

To begin with the vacuum pump is started and the valves connecting to
the low vacuum zone should be operated firstly on one side of the trunion valve

43
and secondly other side trunion valve. (When one side valve is opened half the
surface area of the filter drum is covered with filter cake).

When entire surface of the filter drum is properly conversed with filter
cake open the vacuum valve near the trunion valve pertaining to high vacuum
zone simultaneously apply wash water from atomizers and then through drip
pipes.

Once the desired vacuum gets established you will notice is that the wash
water properly penetrates through the filter cake and washes the cake perfectly
desugarising it to the maximum extend. (Pol% F.C. 1.5% to 2.0) Primary
washing of filter cake is accomplished by atomizers and secondly washing by
drip pipes. Adjust the water spray from the drip pipe in such a way that water
does not overflow the cake nor it washes away the cake. Vacuum gets
disconnected from the drum surface few feet before the cake come in contact
with the scrapper plate. So that the dried cake easily gets discharged into belt or
screw conveyor through which the filter cake is conveyed into weighting trolley
CHAPTER –VI
RESULT AND DISCUSSION

Analysis of lime, sulphur and phosphoric acid, CaO& phosphate content

in the mixed juice and clear juice and estimation of active Biocide in mill
sanitation chemicals were carried out in the laboratory under conditions
specified.

Table: 1
CaO % in lime stone

44
 [Link] CaO%
1 79.78
2 75.44
3 72.13

Table: 2
CaOcontent in the mixed juice and clear juice.

[Link] Mixed juice mg/ litre Clear juice mg/litre

1 830 1420
2 700 1370
3 850 1440
4 950 1350

Table: 3
P2O5 % in Phosphoric acid.

[Link] P2O5 %
1 73.84
2 75.60
3 66.56

Table: 4
Phosphate content in the mixed juice and clear juice.

45
 [Link] Mixed juice mg/lit Clear juice mg/lit
Before After Before After
1 185 285 110 150
2 245 365 100 125
3 230 320 95 140
4 200 365 125 155
5 270 325 85 105

6.1 CaO
The results of the CaO % in lime stone and CaO content in the mixed
juice and clear juice are given in table 1 and 2.

CaO % in given sample (lime stone) = 75-85%

Amount of CaO in mixed juice = 850 to 950 mg/ lit
Amount of CaO in clear juice = 1200 to 1400 mg/ lit

Cane juice is acidic with pH of around 5.2. In the acidic medium,

Sucrose is inverted into glucose and fructose. So we added to milk of lime to
cane juice increase the pH 7.0. The aim should be to use the minimum of lime
which will give good clarification and good settling, with a pH of clarified juice
close to 7.0. Since any excessive lime is harmful and results in an increase in

46
the content of lime in clarified juice. The CaO content of mixed juice to clear
juice should not exceed 400 mg/lit.

6.2 P2O5
The results of the P2O5 % in phosphoric acid and phosphate content in the
mixed juice and clear juice are given in table 3 and 4.

P2O5% in Phosphoric acid = 62-64%

Amount of P2O5 in mixed juice
Before adding Phosphoric acid = 250- 300 mg/ lit
After adding Phosphoric acid = 300- 350 mg/ lit
Amount of P2O5 in clear juice
Before adding Phosphoric acid = 75-90 mg/ lit
After adding Phosphoric acid = 100-125 mg/ lit.

The mean phosphate content of normal juice is approximately 250mg

P2O5 per liter. It is not sufficient for efficient clarification it is a very poor. One
so we increase the range to 300 to 350 by adding phosphoric acid. The P 2O5
increase the juice clarification.

Role of phosphate in clarification is considered to be most important from

the point of view of clarification and further settling operations. The
Tricalciumphosphate precipitate formed by the reaction of lime with phosphoric
acid which not only removes the colloidal matter by its sweeping action but also
removes the colouring matters by adsorption. The P2O5 content of 300 to 350
mg / lit is essential for good clarification.

6.3 SO2
The purity of Sulphur (in sample) = 99.9%.

47
 1. SO2 neutralizes excess quantity of lime added to produce the CaSO 3
which adsorbs colour and colloidal particles.
2. It blocks the carbonyl group of reducing sugar which is responsible for
colour formation.
3. SO2 decreases the viscosity of juices.
4. It acts on bleaching agent and disinfectant.
6.4 Flocculent
Flocculent is a settling Aid.
This chemical facilitates better flocculation of the mud flocks from
thesulphited juice which increase the settling rate of mud flocks in the clarifier.

6.5 Mill Sanitation Chemicals

Active biocide in mills sanitation chemicals = 40.2%.

Since the cane juice provides ideal media for the growth of innumerable
types of microorganisms. It is pertinent to expect deterioration of cane juice in
it is passage through the milling process resulting in loss of sugars. The
quantum of sugar loss in mills due to microbial action, the microbial growth if
not checked effectively increases reducing sugars acids and non sugars at the
expends of sucrose and reducing sugarno sugars thus formed not only reduce
the recoverable sugar. But also create problems in the boiling house operation,
so we are adding mill sanitation chemical in the Imbibitions water.

48
 CHAPTER - VII
CONCLUSION

From the laboratory scale analysis the following conclusion can be

drawn.

 Firstly the phosphoric acid is used to increase the phosphate level in

juice for efficient clarification.
 Secondly the milk of lime and SO2 gas is used to maintain naturalpH
7.0 of the juice. SO2 is used for another purpose to act as
bleachingagent.
 Flocculent is used to increase the mud settling in clarifier.
 And mill sanitation chemical used to avoid microbial inversion loss in
mills.
 The amount of P2O5andCaO is determined in mixed juice and clear
juice for good clarification.

49
 The percentage of CaO, P2O5 and SO2 are determined in the given
sample for judgment of required quantity.
 If we used atomization equipments, we reduce the chemical cost.

CHAPTER - VIII
REFERENCES

 P. Honig., Principles of Sugar Technology, 1853.

 E. Hugot., Hand book of Cane Sugar Engineering, 1972.
 [Link]., Cane Sugar Manufacturing in India.
 [Link]., Chemical Progress in Cane – Sugar
Manufacture, Vol.15, 1923.
 Joachim [Link]., Peter C. Toebe., Clemens Starzinski., Cane Juice
Purification processes, 2006.
 Herbert . Walker., Industrial and Engineering Chemistry, 1923, 15(2):
164-165.
 K.T.K.F. Kong Win Chang., [Link] Ah Wing., Cane Juice
Purification Processes, 2006.
 [Link]., M.A.A McCalip., H.S. Paine., Industrial and Engineering
Chemistry, 1928, 20(4): 372-376.
 Michael Saska., Cane Juice Purification Processes, 2006.

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 [Link] ., Hand Book of Cane Sugar Technology, 1975.
 MullapudiNarendranath., Cane Juice Purification Processes, 2006.
 [Link]., Vasantdata Sugar Institute, Pune Project Book.
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 [Link]., Processing Sugar Technology Association of India.

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