Sryup Clarification Kuma Nacho

ADDIS ABABA UNIVERSITY
INSTITUTE OF TECHNOLOGY
SCHOOL OF CHEMICAL AND BIO ENGINEERING
SYRUP CLARIFICATION USING FLOTATION SYSTEM WITH

OPTIMIZED DOSAGES OF PHOSPHATE AND CATIONIC
FLOCCULANT: THE CASE OF WONJI SUGAR FACTORY
A Thesis Submitted in Partial Fulfillment of the Requirements for the Degree of Master
of Science in Biochemical Engineering
By: Kuma Nacho

Advisor: Adamu Zegeye (Ass. Professor)
May, 2018
Addis Ababa, Ethiopia
I
Syrup clarification using flotation system with optimized dosages of phosphate and
cationic flocculant.
The undersigned have examined the thesis entitled „Syrup clarification using flotation
system with optimized phosphate and cationic flocculant: The case of Wonji sugar
Factory‟ presented by Kuma Nacho, a candidate for the degree of Master of Science and
hereby certify that it is worthy of acceptance.
Mr. Adamu Z. (Ass. prof)
Advisor Signature Date
Internal Examiner Signature Date
External Examiner Signature Date
Chair person Signature Date
MSc Thesis Page 1

Undertaking
I certify that research work titled ‘Syrup clarification using flotation system with
optimized dosages phosphate and cationic flocculant: The case of Wonji sugar
Factory’ is my own work. The work has not been presented elsewhere for assessment.
Where material has been used from other sources it has been properly acknowledged /
referred.
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TABLE OF CONTENTS
TABLE OF CONTENTS ................................................................................................... 3
ACKNOWLEDGMENTS .................................................................................................. 6
LIST OF TABLES .............................................................................................................. 7
LIST OF FIGURES ............................................................................................................ 8
LIST OF ACRONYMS……………………………………………………………... ..... 10
LIST OF APPENDICES…………...…..………………...………...…………….…… .. 11
ABSTRACT ....................................................................................................................... 13
CHAPTER 1 INTRODUCTION ............................................................................... 14
1.1 Background of the study ...................................................................................... 14

1.2 Statement of the problem ..................................................................................... 18
1.3 Objectives ............................................................................................................. 20
1.3.1 General objectives ......................................................................................... 20
1.3.2 Specific objectives ........................................................................................ 20
1.4 Significance of the Study ..................................................................................... 20

CHAPTER 2 LITERATURE REVIEW ................................................................... 21
2.1 The Sugar Industry general overview .................................................................. 21

2.2 General overview of Wonji Sugar Factory .......................................................... 22
2.3 Clarification as a unit operation ........................................................................... 24
2.3.1 Object of clarification ................................................................................... 25
2.3.2 Chemical reactions of clarification ............................................................... 26
2.4 Syrup clarification using the floatation method ................................................... 27

2.4.1 Syrup clarification process ............................................................................ 30
2.4.2 Benefits of syrup clarification ....................................................................... 32
2.5 Principals involved in syrup clarification............................................................. 33

2.5.1 Effect of operating parameters ...................................................................... 33
2.5.2 Effect of added chemicals ............................................................................. 36
2.5.3 Effect of aeration of syrup ............................................................................ 39
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2.6 Harmful effects of SO2 consumption with sugar ................................................. 41

2.7 Carbonatation and Phosphatation process ............................................................ 44
2.7.1 Phosphatation process ................................................................................... 45
2.7.2 Carbonatation Process ................................................................................... 47
2.7.3 Coagulation and Flocculation ....................................................................... 49
2.8 Froth flotation fundamental principles ................................................................. 53

2.8.1 Types of Flotation ......................................................................................... 54
2.8.2 Hydrophobicity/hydrophilicity ..................................................................... 54
2.8.3 Particle/Bubble Contact ................................................................................ 56
2.8.4 Collection in the Froth Layer ........................................................................ 57
2.8.5 Reagents ........................................................................................................ 57
CHAPTER 3 MATERIALS AND METHODS ........................................................ 60
3.1 Site of the experiment .......................................................................................... 60

3.2 Materials ............................................................................................................... 61
3.3 Sample Preparation .............................................................................................. 62
3.4 Analytical methods ............................................................................................... 63
3.4.1 Color: ............................................................................................................ 63
3.4.2 Turbidity ....................................................................................................... 63
3.4.3 The pH .......................................................................................................... 64
3.4.4 Sulphur Dioxide (SO2). ................................................................................. 64
3.4.5 Determination of Brix in syrup (dilution 1:3 m/m) ...................................... 65
3.4.6 Determination of Pol in Syrup Clarification ................................................. 65
3.4.7 Determination of Soluble Phosphate content ................................................ 66
3.5 Experimental Design ............................................................................................ 68

3.6 Statistical analysis ................................................................................................ 70
CHAPTER 4 RESULTS AND DISCUSSION .......................................................... 71
4.1 Results of the Syrup analysis from Wonji Sugar Factory .................................... 71
4.2 Results of syrup clarified at different level of combinations of phosphate and
flocculation. ..................................................................................................................... 72
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4.3 Color of clarified syrup ........................................................................................ 73

4.4 Turbidity of clarified syrup .................................................................................. 76
4.5 Viscosity of clarified syrup .................................................................................. 79
4.6 Optimum point for combined color, turbidity and viscosity reduction ................ 82
CHAPTER 5 CONCLUSIONS AND RECOMMENDATIONS ............................ 85
5.1 Conclusion............................................................................................................ 85
5.2 Recommendation .................................................................................................. 85
REFERENCES .................................................................................................................. 86
APPENDICES ................................................................................................................... 89
Appendix A. Table of Least Squares fit to results of color, turbidity and viscosity for
clarified syrup .................................................................................................................. 89
Appendix B. figures ........................................................................................................ 93
Appendix C. photos ......................................................................................................... 96
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Acknowledgments
Frist I praise my Lord Jesus Christ who was and is with me by helping and keeping me with
all his eternal graces. Next I want to express my sincere appreciation to my advisor
Asso.prof. Adamu Zegeye; for his guidance, professional suggestion and support during all
the work times. All the students and staffs of Chemical and Bioengineering School
especially members of the Biochemical Engineering are greatly appreciated for the
studying atmosphere during my stay throughout the program duration. Finally I am
grateful to Ethiopian Sugar Corporation Research center (ESCRC) who invited me to the
governmental sugar plan and transformation research and helped me in all idea
exchanging and all laboratory facilities.
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List of Tables
Table 3.1 Coded and corresponding actual value of the factors used in the central composite
design
Table 3.2 Central composite design (CCD) for coded levels of the two factors
(phosphatation and flocculation)
Table 3.3 Calibration of phosphate concentration against its optical density
Table 4.1 Laboratory analytical results of syrup from wonji sugar factory
Table 4.2 Average results obtained from syrup at different level combinations of phosphate
and flocculation.
Table 4.3 The optimum phosphate and talodura for syrup clarification.
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List of figures
Figure 1.1 process of the cane juice from the cane stalks and subsequent removal of the
non-sugars.
Figure 1.2 Wonji syrup clarification plants.
Figure 2.1 Satellite image of wonji sugar factory.
Figure 2.2 Wonji shoa sugar factories.
Figure 2.3 Turbidity removals in syrup as a function of flocculent dosage.
Figure 2.4 Effect of temperature on turbidity removal.
Figure 2.5 Viscosity of syrup and molasses (adjusted to 73 Brix and 40°C) with and
without syrup clarification. (Rein 1988)
Figure 2.6 DAF Process Schematic.
Figure 2.7 Mode of interaction of Talofloc with colorant.
Figure 2.8 Typical flotation vessels.
Figure 2.9 Diagram of flocculation
Figure 2.10 The flotation system includes many interrelated components and changes in
one area
Figure 2.11 Selective attachment of air bubbles to hydrophobic particles.
Figure 2.12 Contact angle between and air bubble and a solid surface immersed in liquid.
Figure 2.13 Simplified schematic of a conventional flotation cell.
Figure 2.14 Adsorption of anionic collector onto a solid surface.
Figure 3.1 Wonji Sugar Factories.
Figure 4.1 Diagonal lines within 95% confidence limit region.
Figure 4.2 The actual by predicted plot for color points.
Figure 4.3 Response grid slider shows variation in color.
Figure 4.5 The actual by predicted plot for turbidity points.
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Figure 4.6 Response grid slider shows turbidity variation.
Figure 4.8 The actual by predicted plot for viscosity points.
Figure 4.9 Response grid slider shows viscosity variation.
Figure 4.10 The desired point for optimum clarification.
Figure 4.11 Superimposed contour plots for optimum point.
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List of Acronyms……………………………………………………………………...IX
PWS………………………………………………………………..plantation white sugar
DOE…………………..……………………………………………design of experiments
ICUMSA……………………………………………............……International Commission
for Uniform Methods of Sugar Analysis
USD……………………………………………………..……………..United states dollar
GTP………………….………………………………….Growth and Transformation Plan
MWh……………………………………...........………………………Megawatt per hour
TCD…………………………………………………………….……..Tons of cane per day
DAF……………………………………………………………........Dissolved air flotation
DS………………………………………………………………..………………Dry solids
CD……………………..……………………………………………..……Drag coefficient
CHM..……………………………………………...………...…...Crystal habit modifiers
CCD………………………………..………………………….Central composition design
CFD………………………………………………….…….Computational flood dynamics
SASTA…………………………………...South African Sugar Technology Association
VHP………………………………………very high pool
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List of Appendices…………...…..………………...………...…………….…………..X
Appendix A. Table of Least Squares Fit to results of color for clarified syrup
Appendix table 1. Model fitting to results of color for clarified syrup
Appendix Table 1.1 Summary fit for results of color for clarified syrup
Appendix Table 1.2 ANOVA for results of color for clarified syrup
Appendix Table 1.3 Lack of fit for results of turbidity for clarified syrup
Appendix table 2. Model fitting to results of turbidity for clarified syrup
Appendix Table 2.1 Summary fit for results of turbidity for clarified syrup
Appendix Table 2.2 ANOVA for results of turbidity for clarified syrup
Appendix Table 2.3 Lack of fit for results of turbidity for clarified syrup.
Appendix table 3. Model fitting to results of viscosity for clarified syrup
Appendix Table 3.1 Summary fit for results of viscosity for clarified syrup
Appendix Table 3.2 ANOVA results of viscosity for clarified syrup
Appendix Table 3.3 Lack of fit for results of viscosity for clarified syrup.
Appendix B. figures
Appendix Figure 1. Prediction profiles
Appendix Figure 2. Interaction profiles
Appendix C. Figures
Appendix Figures 1. Cane loading in the field
Appendix Figures 2. Flotation system syrup clarification plant
Appendix Figures 3. Flotation system syrup clarification plant
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Appendix Figures 4. Sample of the syrup taken from wonji factory
Appendix Figures 5. The talodura flocculant
Appendix Figures 6. The CaCO3 used to precipitate the phosphate
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ABSTRACT
Syrup is a clarified juice evaporated to approximately 65% dry solids in a stepwise

evaporation process. This concentrated syrup is needed to clarify further before the final
fractionation. All Ethiopian sugar factories are designed for the production of plantation
white sugar (PWS) by double sulphitation system which is the main source of an increased
residual sulphur dioxide in the final product. There is a significant interest in many sugar
producing countries towards producing a higher quality plantation white sugar with lower
color and lower residual sulphur dioxide content. A sugar with a lower color and lower
residual sulphur dioxide values is achieved by replacing the syrup sulfitation process with
syrup phosphatation and flocculation. The study was conducted to optimize the syrup
clarification as the result of the effect of Talodura and Phosphate on reducing color,
turbidity and viscosity using flotation system and there by modifying or reducing the sulfate
content in the sugar. This increased sulfate is due to syrup double salfitation during syrup
clarification at Wonji Sugar Factory. Since degree of clarification is dependent on the dose
of Phosphate and Talodura flocculant, optimization of the doses was carried out against
color, turbidity and reduction of viscosity. Design Expert 7 and JMP13 software were used
to determine the common optimum doses. The range of levels of the P2O5 used was 117.8 -
680 mg/L, and that of the Talodura was 7.2 - 12.8 mg/L. The optimum levels, 668 mg/L of
P2O5 and 12 mg/L of Talodura gave color and turbidity values of 9772 and 4669 ICUMSA
respectively and a viscosity reduction of 39 %. Practicing the above optimum conditions at
Wonji Sugar Factory could increase productivity and sugar quality.
Keywords: Color, Phosphate, Syrup clarification, Talodura, Turbidity, Viscosity,
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CHAPTER 1 INTRODUCTION
1.1 Background of the study
The production of raw sugar from sugarcane consists of a series of units of operations,
which begins with the extraction of the cane juice from the cane stalks and subsequent
removal of the non-sugars. This process is summarized in figure 1. Sucrose is first
extracted from the cane by the addition of water through counter current milling or
diffusion. Extracted juice then undergoes an extensive process of cleaning which
involves screening, heating and addition of milk of lime (calcium hydroxide) to adjust
pH and enhance flocculation. The limed juice is then allowed to settle out suspended
particles in a clarifier. Following the juice cleaning process the clear or clarified juice is
then evaporated to approximately 65% dry solids (DS) in a stepwise evaporation process.
Then the juice, which is now concentrated syrup, is formed and need to be further
clarified before put through a final fractionation of sugars from non-sugars by
crystallization in vacuum pans via evaporation and concentration and in crystallizers by
cooling. (Broadhurst, 2002)
It is expected that the increasing interest in the production of both plantation white sugar
and raw sugar of high quality will focus attention on raw syrup quality in the factory.
Having identified undesirable impurities of raw syrup, steps can be taken in the factory
to reduce the levels of these impurities in the pan feed syrup. The nature of impurities
determines the methods of clarification to choose. In the case of process generated
colorants', preventative measures such as inhibition of color formation by juice
sulphitation are likely to prove increasingly attractive. Levels of other impurities such as
insoluble and gums which, although present in relatively small quantities, affect sugar
quality and factory recovery can be reduced at reasonable cost by clarification of the raw
syrup. The removal of such impurities has proved attractive to factories producing
plantation white sugar. Improvements in recovery indicated from the viscosity reducing
effect of syrup clarification; is also likely to generate interest in the industry. (Bennett,
et.al 1977)
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Figure 1.1 Process of the cane juice from the cane stalks and subsequent removal of the
non-sugars, Broadhurst, 2002.
They are two ways of obtaining low color syrup that leads low color sugar. One way of
obtaining low color sugar which is conventional is operating sulfitation on evaporator
syrup (syrup taken from evaporator after clarified juice evaporation). Lime or lime
saccharate is added, and then sulfur dioxide. Adding sulfur dioxide on syrup is called
double sulfitation because ones sulfur dioxide is added to the juice clarification to
achieve better color of sugar juice. By this time Ethiopian sugar factories are designed
and working for production of plantation white sugar (PWS) by double sulphitation
system which produces the traces of sulfur remain in these food product (sugar) and
hazardous to human health.
In double sulfitation system the raw juice is heated to 75°C and pre limed to PH 9.2.
Sulfur dioxide is first applied which neutralizes the alkalinity reacting with lime and
forming calcium sulphite precipitate in the clarification process. In the second phase
sulfur dioxide is again added in syrup treatment to PH 5.4 to reduce the viscosity of the
syrup and massecuite and improve molasses exhaustion. But the treated syrup is left
acidic during its retention time in take case and the crystallization process in vacuum pan
is carried out in turn affects sugar recovery. The treatment of the syrup with SO2 is
known also to reduce sugar color by just 6-15% (kulkami, 2009)
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Syrup sulphitation also doesn't remove suspended solids and impurities like bagacillo and
colloidal matter that may have escaped screening process, which adversely affect the
crystallization, curing of massecuite and quality of sugar. This realization encouraged the
development of an alternative technology that would avoid at least syrup sulfitation and
help in producing good quality PWS sugar. (Bennet, 1971)
The second method which is new technology or alternative technology is Syrup

clarification using flotation process. The basis of this process is based on the
Phosphoflotation and froth flotation, conveniently termed as 'phosphoflotation' process
applied in sugar refineries. Since the syrup liquor is very viscous, at about 65ºBrix,
clarification is done by flotation. Air is used to aerate the flocculated particles so that they
float and are removed at the top of the clarifier as scum. The treated syrup is drawn from
the bottom of the clarifier and sent to vacuum boiling pans to crystallize out the sugar.
The mechanism involves physical capture of the air bubbles within the floes and
intermolecular attractions across the air/liquid interface. Scum can be floated off with
bubbles in the clarifier. The degree of separation achieved depends on the surface
properties of the solid particles.
Laboratory and factory scale trials on syrup clarification conducted by sugar research
institute of Australia dated back 1960 assess the benefits of phosphitation clarification of
syrup to improve the sugar quality. It was demonstrated that a process of heating syrup
76°C to 86°C and addition of phosphoric acid and lime would cause precipitation of
calcium phosphate scum that included fats, waxes, proteins and ash constituents. This is
done by investigated the use of specialty chemicals like Talofloc (cationic color removal
agent) and Taloflote (polyacrylamide flocculant). A similar flocculant, Talodura was
subsequently developed for use in syrup clarification.
Like other Ethiopian sugar factories Wonji Shoa Sugar Factory is also using the syrup
double sulfitation even though two types of syrup clarification plants; syrup clarifier
using flotation method and that of clarifier using sulfitation were planted. The second
method which is syrup clarification using flotation system has installed in Wonji case and
has many advantages over that of syrup sulfitation but it doesn't start working in this
sugar factory yet.
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The efficiency of syrup clarification using flotation system highly depends on optimized
dosages of factors like: flocculants added and phosphates to get good results on reduction
of color, turbidity and viscosity. The variability in the composition of the juice as a result
of differing geographical location, cane variety and seasonal influence as well as the
conditions to which the cane is subjected during harvesting and transportation makes the
nature of the research to be area specific; hence, there is no universal dose of phosphate
and flocculent so as to produce the best possible quality clear syrup. Each factory is
therefore essentially unique and adopts a system of clarification based on their own
process with modifications usually determined by a combination of research and
experience.
Figure 1.2 Wonji syrup clarification plants
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1.2 Statement of the problem
Increased export prospects, increasing consumer awareness for hygiene and the changing
habits by small packs are becoming more popular and are changed from time to time. Save
for the right price consistently superior quality sugar is vital to securing a long-term
advantage for the sugar industry. The insoluble matters content with large variations makes
the sugar unsuitable for consumption by specialty consumer. Sugar cane juice is composed
of various constituents like chlorophyll, xanthophyll, antherocynines & cynines etc. Most
of them are removed during processing but some of them passes through syrup like
colloidal substances, color causing impurities, gums, dextran, polysaccharides, bagacillo, in
organic precipitates etc. This increases viscosities & resulting losses. The presence of
sulfur di-oxide, calcium oxide, ash & reducing sugars makes it unacceptable for export
purpose. Poor keeping quality and low color removal are common problems for double
sulphitation.
There is also loss which is higher when double sulphitation is practiced to make mill-white
sugar, due to the low pH reached in the syrup sulphitation stage. Syrup sulphitation is the
process in which the pH of the syrup is reduced to a value of about 5, or in extreme cases,
to as low as 4. Because of the high sensitivity of observed color to pH the resulting low pH
syrup has lower color and, in addition, some insoluble material is dissolved under these
acid conditions. However, the sugar produced from such low pH syrup has poor keeping
quality and the color increases rapidly during storage. Furthermore, process losses through
inversion are high. (Bennett, et.al 1977)
Sulfur dioxide (SO2) is toxic gas. When it is used during the manufacture of any food
product residual traces of sulfur remaining in such food product is hazardous to human
health. In the sulphitation process, the use of sulfur burner is difficult as it causes the
toxic (SO2) to be released into atmosphere, leading to serious environmental pollution
because of this potent greenhouse gas. It can also create health problems for the workers
handling the sulfur burners. The cost of repair of sulfur burner plant is so high due to
corrosion effect of sulphur. (Biotech, 2009)
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Syrup sulphitation end up significant amounts of sulfur and hence it affects the
fermentation of the molasses by inhibiting the growth of the yeast. Moreover, traces of the
sulfur that gets into the alcohol make it unsuitable for use as a fuel supplement, liquor, and
pharmaceutical industries, unless further refinements are carried out. Thus the use of SO2 in
syrup does not provide any significant benefit. Further, whatever benefit does result lasts
only for a short period of time. (Bennett, et.al 1977)
Currently, all Ethiopian sugar factories were designed for the production of plantation white
sugar (PWS) by double sulphitation system which is the main source for the increased
residual sulphur dioxide in the final product. There is significant interest in many sugar
producing countries towards producing a higher quality plantation white sugar with lower
color and lower residual sulphur dioxide content due to this residual sulphur dioxide is
harmful in consumption. (Mohammed, 2013)
This realization prompted the development of an alternative technology that would avoid at
least syrup sulphitation and help in producing good quality sugar. One option to replace the
second sulfitation process is to use syrup clarification based on the phosphoflotation
process. The phosphoflotation process can reduce color compounds that are produced
during the factory processes. Such color and color precursor groups include melanoidins,
caramels and alkaline degradation products of fructose and glucose. This research project
was initiated to investigate the best working dosages of Talodura flocculant and phosphate
on the benefits and methods of improving syrup clarification and to looks at the results thus
far in the review of syrup clarification as a possible technology for better sugar quality,
specifically sugar color, reduced turbidity, viscosity.
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1.3 Objectives
1.3.1 General objectives

 To study syrup clarification system using flotation process with optimized
phosphate and cationic flocculants in Wonji Sugar Factory.
1.3.2 Specific objectives

 To analyze the raw syrup from Wonji Sugar Factory prior to clarification.
 To conduct the syrup clarification process using flotation system on the laboratory
scale.
 To determine the dosage of phosphate and cationic flocculants that should be added
for better clarification.
 To analyze the clarified syrup (color, turbidity, viscosity reduction) with the syrup
clarification technology.
 To Optimize the effect of phosphate and cationic flocculants using centeral
composite design using the DOE and JMP software.
1.4 Significance of the Study
The syrup clarification process is low cost solution both from the capital costs point of view
as well as sugar operational costs in relation to the gains to be made by the sugar refinery
factories. Syrup clarification system using flotation process ends with: Improvement in
sugar quality with lower ICUMSA value and lower SO2 contents, reduction in viscosity of
syrup which in turn improves the pan flour working and these results in better exhaustion of
molasses, increased boiling house capacity, reduction of final molasses % cane, rise in
purity from unsulphered syrup to clear syrup. Which means: Faster boiling, leading to
increased pan equity, faster purging to increased centrifugal capacity, reduction in non-
sugars % leading to lower final molasses quantity and rise in purity, leading to higher
boiling house recovery.
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CHAPTER 2 LITERATURE REVIEW
2.1 The Sugar Industry general overview
Sugar is produced from cane and beet in over 130 countries in which sugar produced from
sugarcane contributes about 65 to 70 % of global production. Brazil, India and China are
leading countries and 85 percent of production was contributed by the top 15 producer
countries. Moreover, in the last 50 years these countries were leading the industry. Ethiopia
is one of sugar producing country from sugarcane and contributes about 0.18 % of the
global sugar production. The use of improved technologies developed through research in
different sugar producing countries had increased their production and productivity. In
Ethiopia the cane productivity was not maintained from year to year and the potentials are
not yet exploited mainly due to the inability to optimize cane production and sugar
manufacturing process through the application of improved technologies. (Girum Asfaw,
2015)
Commercial sugar production in Ethiopia was started in 1954 with the establishment of
Wonji Sugar Factory. Since then, sugar is produced from irrigated and semi-mechanized
sugarcane farms owned by the sugar estates and some out growers‟ scheme. Currently
Ethiopia has about 45,000 ha of cultivated sugarcane farm that supplies cane only for three
operating sugar factories (Wonji, Metahara and Finchaa) to produce annually about 460,000
tons of sugar. Finchaa and Metahara also produce about 20,000,000 and 15, 000, 000 liters
of ethanol respectively and blended at 10 % with benzene for transport sector. The sugar
industry is self-sufficient in term of its thermal and electric demand from cogeneration.
The sugar industry contributed to the country‟s socioeconomic benefit by creating more
than 28,000 employees. (Girum Asfaw, 2015)
In recent years the increasing local demand of sugar cannot be met through the existing
production system. As a result the government was forced to import annually 150,000 ton
which is valued at 50 to 60 million USD. To solve this problem the government was
undertaking expansion programs on the three sugar state, namely Wonji, Metahara and
Finchaa. Moreover, a new factory in Afar regional state, Tendaho Sugar factory, has begun
to produce raw sugar as raw material for back end factory for refined production. The
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countries five years Growth and Transformation Plan (GTP) which was launched in 2003
E.C. has given paramount emphasis to the sugar industry which demands huge technology
development, dissemination and manpower training. At the end of the five years, it is
planned to produce 2,250,000 tons of sugar and out of this to export 1,246,000 tons by
establishing eight or nine huge sugar factories. The plan also targeted to produce 304,000
m3 ethanol and 606,943 MWh electric powers from cogeneration. (Girum Asfaw, 2015)
2.2 General overview of Wonji Sugar Factory
The factory is found at Oromiya regional state near Nazareth city at 110 kilo meters from
Addis Ababa. Commencing production in 1954; it is the oldest and the pioneer in the
history of Ethiopia‟s sugar industry. Shoa Sugar Factory constructed in 1962 is the second
oldest and both being obsolete have stopped production since July, 2012 and July, 2013
respectively. The two factories constructed by the Holland Company known as H.V.A had
a capacity of producing 750,000 quintals of sugar a year. The sugarcane plantation land of
these two factories was 7,000 hectares out of which 1,000 had been planted by out growers.
Figure 2.1 Satellite image of wonji sugar factory
In a bid to replace these two oldest factories with a new and modern one, an expansion
project had been carried out both in the cane cultivation field and the factory since 2010.
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And the factory plant expansion project was come into its completion in July, 2013.
Accordingly, the newly built and modern Wonji/Shoa Sugar Factory has currently a design
capacity of crushing 6,250 tons of cane a day and producing over 174,000 tons of sugar per
annum which with further expansion will reach up to 12,500 TCD maximizing its
production to 220,700 tons of sugar a year. The new ethanol plant planned to be built, will
have a capacity of producing 12,800 meter cube. The Factory is currently contributing 20
megawatt electric powers to the national grid in addition to satisfying its own demand
which is around 11 megawatt. Its agricultural expansion project is currently being carried
out around the areas known as Wakie Tiyo, Welenchiti and North Dodota areas. The
factory with the help of this agricultural expansion project will have 16,000 hectares of
sugarcane plantation field in total.
Figure 2.2 Wonji shoa sugar factories.
The total cane cultivation field of the factory has currently reached 12,800 hectares. And,
the 7,000 hectares of the factory‟s sugarcane field cultivated with the agricultural expansion
project is owned by out grower farmers of the surrounding area. There are 32 sugarcane
growers association; which has in total 9,100 member farmers. The Factory, beyond
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supplying the farmers with selected seeds, and rendering professional as well as technical
support to them, has made irrigable land available to all. (Whayman and Crees, 1974)
2.3 Clarification as a unit operation
The sugar cane juice as expressed from the cane contains not only sucrose but also
numerous other dissolved substances, as well as cellulose or woody fiber. Sugar cane juice
is an extremely complex liquid medium, containing many organic and inorganic
constituents in soluble, suspended or decant and suspended/colloidal form. The percentage
of sugar (polarization) in the cane varies from 8 to 16 per cent and depends on a great
extent on the variety of cane, its maturity, the condition of the soil, the climate and
agricultural practices followed. Cane sugar for human consumption is produced by means
of clarification of sugar cane juice. A critical step in the manufacture of any sugar (raw,
plantation white, or refined) is clarification of the sugar juice. Clarification is the process of
removing the constituents of the juice other than sucrose and at the same time minimizes
loss of sucrose and color formation. Clarification is therefore an essential step to obtain
high yields and high quality sugar. Several clarification methods are currently used
including cold liming, hot liming and fractional liming with double heating, liming while
boiling, calcium saccharate treatment and Java method. (Hugot, 1986)
Sulphur dioxide (SO2) has been used for centuries to minimize color in food processing and
fruit and vegetable storage. Sugarcane processors throughout the world use SO2 to produce
plantation white sugars. It consists of SO2 absorption by the hot limed juice, reducing its
basic pH to about 7.0. To improve floc formation, soluble phosphate is added to the juice.
The soluble phosphate produces an insoluble calcium phosphate primary floc that traps
other suspended impurities. In the cane sugar factory, the major role of sulfur dioxide has
been to make white sugar rather than raw sugar through inhibition of color forming
reactions including enzymatic browning reactions. However, periodic spikes in sulfur
prices and sugar quality issues have stimulated efforts to reduce or even eliminate its use.
With that in mind, a carbonation process has been tested and compared with standard
sulfitation and defecation. Besides eliminating the use of sulfur, carbonation would also
provide a means to utilize and take away some of the excess CO2 that may be available
cost-free in some sugar factories from molasses or juice fermentation. Among sugar cane
processors worldwide, there is mixed interest in usage of sulfitation. (Godshall, 2002)
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In Ethiopia, all sugar factories employ sulphitation process for the manufacture of
plantation white sugar (PWS). In the United States (US), sulfitation has rarely been used in
cane raw sugar factories since the 1950's. Today, there is renewed interest in the
effectiveness of sulfur dioxide as a color retardant as many US factories are considering the
production of high quality low color raw sugar to be sold as a food grade sugar . To
improve decolorization without using an excessive amount of lime that would raise scale
problems, phosphatation can be supported by a flocculating agent. Rapid flocculation and
sedimentation of suspended particles in primary cane sugar juice is achieved using a high
molecular weight anionic polymer flocculant (Doherty et al., 2003).
Flocculation is the agglomeration of fine particles suspended in solution in to a flocculent

mass. Flocculation removes insoluble suspended particles and colloidal impurities by
aggregating them into flocs. A typical size range for pre-flocculation impurities in mill-
extracted mixed juices at Louisiana raw sugar factories is 0.1 - 22 microns. In many cane
sugar producing countries, the standard sugar product has a very low color in the range 80
to 250 IU. This sugar which is used in Ethiopia is commonly referred to as plantation white
sugar (PWS). On the other hand, the standard for white (refined) sugar is considerably
higher, requiring a color below 45 IU for EU No 2 or even 22.5 IU for grade 1 white sugar
(Rein, 2008). The methods employed to produce PWS usually involve sulphitation of the
juice and/or the syrup (Steindl, 2005). Plantation white sugar has been produced at raw
sugar mills for many years without refining or re-crystallization (Rein, 2008).
2.3.1 Object of clarification

The term clarification is defined as a process by which all insoluble and some soluble
impurities are removed from the juice or syrup. These impurities impart dark color to the
juice and contain sucrose, reducing sugars, organic and inorganic matter in the solution. It
also contains insoluble matter in suspension such as bagacillo (fine bagasse) and soil. The
main object of clarification of mixed juice is as follows: Removal of maximum non sugars;
elimination of suspended and colloidal impurities; removal of color forming compounds; to
obtain brilliant, light colored, transparent clear juice free from any suspended impurities.
(Whayman and Crees, 1974)
To obtain high quality clarified juices or syrups, removal of components other than sucrose
should be maximized, and losses of sucrose and formation of color should be minimized.
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Proteinaceous and waxy matter, some silica acid (hydrated SiO2), and sesquioxides can be
removed by heating, while liming neutralizes acids, forms calcium phosphates, and
coagulates colloidal particles. Colloids are known to be responsible for higher or lower
turbidity of sugar products and to have an adverse effect on the entire process (Rodriguez et
al., 1977).
Cane juice is a poly dispersed irreversible colloidal suspension in which the suspended
particles carry a large negative charge. According to established theory of colloid stability,
small particles are attracted one another by Van der Walls forces and therefore always tend
to aggregate together but they are kept apart by electrostatic forces arising from their
electrical charges. The measures of these repellent force is called Zeta potential and has
been defined as a measure of net electrical potential (in millivolts) carried by particles in
size ranges of 10 A° to 10 μm. The aggregation process is aided by the addition of simple
electrolytes like Ca(OH)2 to the juice. The negatively charged colloidal calcium phosphate
is formed by liming. This interaction results in coagulation and sedimentation of the
particles (Rein, 1977).
2.3.2 Chemical reactions of clarification

The chemical reactions that occur during cane juice or syrup clarification are not fully
understood. It is fundamental however that those reactions with lower free energy content
would take place preferentially, with reactions requiring lower energy completing first.
Defecation as an example is the most used method of clarification; therefore in looking at
the reactions in clarification, defecation will be the clarification method of choice. The
solubility of calcium oxide in water is about 0.12% at 25°C, but it is greatly increased in a
solution of sucrose. The solubility however decreases with an increase in temperature.
Calcium hydroxide being a relatively strong base of a divalent metal ionizes in solution to
give CaOH+ and OH-. (Saska, 2002)
The secondary ionization is low, with less than 10 % of calcium as Ca++. The reaction of
lime and phosphate in juice or syrup precipitate calcium phosphate. This reaction is rather
complex due to the reactions of phosphoric acid, calcium hydroxide, and the presence of
other organic and inorganic compounds. Calcium phosphate reaction rate has been shown
to be very low and the precipitate formed in two forms, tri-calcium phosphate in sucrose
solution containing 0.3-0.5 % calcium oxide Ca3(PO4)2, and calcium hydrogen phosphate
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CaHPO4. The formation of calcium hydrogen phosphate has been shown to have a faster
reaction rate, and as it approaches completion the rate of the formation of tri-calcium
phosphate increases. The rates of both reactions are greatly increased at high temperatures
and result in an increase in the hydrogen ion (H+) concentration, which has been suggested
as a contributor to the drop in the pH observed when juice is heated. (Honig, 1963)
Approximately 80-90% of the phosphate present in juice is precipitated with lime. It was
shown that at a pH of about 8.5, about 99% of the phosphate present in juice are
precipitated. Other calcium salts are precipitated in clarification; these may include sulfate,
aconitate, and oxalate, tartrate, and citrate salts. These salts are normally precipitated in
small quantities, but variations do occur depending on the quality of the juice. The sulfate
content of cane juice is highly variable and approximately 20% is removed by liming to pH
in the range 7-8 (Rundel, 1977).
The organic acids in juice are responsible for the natural pH of the juice (5.2 - 5.4) as well
as the buffering capacity of the juice, which is mainly due to the juice aconitic acid content.
The presence of other organic acids such as lactic, formic, acetic, propionic, and butyric
acids are generally a result of microbial or chemical decomposition of sugars (Saska 2002).
Another component of cane juice is silica. Silica is present in the juice in the form of
dissolved silica, colloidal or suspended silica or as silicates. On average it is 0.42% of
solids in mixed juice. Most of the suspended silica is removed by liming (Honig, 1963).
2.4 Syrup clarification using the floatation method
Syrup clarifiers use the floatation method unlike the juice clarifiers, which utilize a settling
method. The settling method would not be possible with syrup because of the high density
and viscosity. The mechanism of syrup clarification involves the trapping of air bubbles
within the flocs and intermolecular attraction across the air/liquid interface. Syrup
clarification occurs by heating the syrup, then aerating it to trap the fine particles, which are
finally coagulated by a low molecular weight flocculant. The scum will float to the top of
the clarifier where it is scraped off and returned to the mixed juice tank. The factors that
directly influence the syrup clarifier are temperature, flocculant mixing and dosage, air and
syrup flow rates. (Rundel, 1977)
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Syrup clarification is an old technology that is being used to good effect especially in South
Africa, Australia, Belize, India and Mauritius. It was first tried in South Africa in 1974 at
Noodsberg with the following results: improved sugar quality, reduction in massecuite
viscosities, no boiling house improvements. This process was discontinued at Noodsberg
because the emphasis was not on quality. At Tonga at Hulett Sugar Limited, Felixton
several trials were undertaken and they have shown good results with respect to; insoluble
solids, color reduction, better boiling house recoveries. (Hon- Jun, 1990)
Then trials were undertaken at Belle Vue Sugar Mill in Mauritius with the following
results; sugar quality was improved, massecuites were found to be less viscous and easier to
cure, a 67% reduction in the syrup turbidity, no improvements on final molasses, there was
an increase in color. In 1960 the Sugar Research Institute of Australia commenced its first
syrup clarifier project and has since constructed syrup clarifiers in Australia, India and
China to give a higher quality raw sugar. Syrup clarification is being done at Tower Hill
Sugar Mill to reduce the insoluble solids for direct consumption sugars. Guysuco provided
drawings and additional information for the syrup clarifier that was built at Tower Hill Mill
in 2001 and a 73% reduction in turbidity was reported in 2001.
There are a few key parameters, which must be controlled before proper results can be
obtained. Those key parameters are; air supply, heating of syrup, syrup flow, flocculant
dosage and concentration, air supply. Air is applied to the syrup clarifier by air diffusers.
The air is used for two reasons in the clarifier. Aerating the syrup is done so that the air
bubbles cling to the precipitates in the syrup and it aids floating the floc to the top of the
syrup clarifier. When starting up the clarifier the air must be added at a higher rate (15-20
p.s.i) than during operations. This is to create bubble formation at the top of the clarifier. It
was found that excess air promotes faster scum formation. During operations the air should
be regulated so that the minimum air is used to float the floc to the top of the clarifier and
produce the lowest possible turbidity. This range is between 5-15 p.s.i. (Rein and Cox,
1987)
Heating of the syrup is essential to the coagulation of the flocs. A shell and tube heater,
which uses 2nd vapor as the heating agent, heats the syrup. Studies from (Rein and Cox,
1987) have shown that changes in temperature will affect the turbidity removal of the syrup
MSc Thesis Page 28

and it peaks at a temperature of about 85oC, hence no specific trials were undertaken.
(Rundel, 1977)
The flow of syrup is very important to obtain constant turbidity from the clarifier. Excess
flow or low syrup brix conditions will cause syrup to overflow into the scum take off and
returned to the mixed juice tank, thereby affecting the performance of the juice clarifier.
There will be an increase in color and the juice clarifier will also become disturbed. If the
syrup flow is not maintained within a range the ratio of syrup to flocculants will change and
hence the turbidity will be affected unless there is an automatic link between the syrup flow
and flocculent dosage. If the station is manned then the operator will need to change the
flow of flocculant to get the desired turbidity, but it would be best if a flow controller is
installed to more accurately control the flocculant dosage as the flow changes. At present a
flow controller is not installed but one is being acquired to monitor the flow and ultimately
control the dosage. (Hon- Jun, 1990)
The flocculant dosage and concentration affects the clarity of the syrup and this was evident
from the scum at the top of the clarifier. The best results were obtained at concentrations of
0.1% and dosage of 15 ppm on brix. The flocculants used was Talodura with other
flocculants. The sequence of air and flocculants additions affected the operation of the
syrup clarifier. It was found that better results were obtained when the syrup was aerated
before the addition of flocculants, but syrup clarifiers at other factories operate with the
reverse. The flocculants is added into the syrup line by the use of a variable speed mono
pump just before a specially designed mixer situated about 6 feet before the clarifier. The
mixing system for the flocculants is very important because if there are lumps in the
flocculants, it will affect clarification. It must be noted strict guidelines should be followed
before the flocculent can work effectively. These include the mixing temperature and the
aging of the flocculent before usage. The flocculent is mixed by air with a funnel used to
distribute the flocculent at small quantities into the mixing tank, but this inevitably creates
lumps. A new flocculant mixing system equipped with a venturi is being installed to
improve flocculant mixing. (Rundel, 1977)
An SMRI turbidity meter is installed to monitor the turbidity as it changes. This is

displayed on a chart recorder, which also records the temperature of the syrup going into
the clarifier. These results can be downloaded to a computer for analysis. This is done on
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daily basis. The laboratory does a turbidity analysis on none clarified and clarified syrup on
alternate hours so that the reductions can be monitored. Also an insoluble solids analysis is
done on a shift basis for the composite sugar samples.
Major components of the syrup clarifier station, includes;
 Clarifier
 Syrup heater
 Air diffusers
 Syrup pump
 Flocculant Tank
 Flocculant pumps
 Inline Turbidity meter and Recorders
 Inline mixer
In addition, improvements in the final molasses purities will result in increased sugar
production, for example it is estimated that if the final molasses purity drops two unit this
factory should recover a further hundreds tons of sugar per year, which is equivalent to
huge money per year increased revenue. With the addition of lime and phosphates to the
syrup better clarification will be achieved because of the formation of more agglomerates,
which will further trap the insoluble particles and hence a greater reduction in color and
insoluble solids will result. (Pottage, 1977)
2.4.1 Syrup clarification process

Syrup clarification is not a standard operation in all raw sugar mills. It is becoming more
widely used and gradually replaces the double sulphitation process, particularly in the
production of sugars for direct consumption, either to remove suspended solids or color or
both. Because of the viscosity and greater density of the syrup, it is not possible to settle out
the fine suspended solids. Flotation clarification does, however, work effectively when
applied to syrup, without any sophisticated process requirements. The aerated phase is
stable and does not require the extensive use of chemical to form and stabilize the scum
layer as, for instance, flotation in mineral processing requires. As an alternative to filtration,
flotation clarification can be considered as a simpler and cheaper option. It can be
augmented with either sulphitation or phosphatation to achieve particular sugar quality
criteria. Normally, the color index of clarified syrup is from 1600 to 1800 IU depending on
MSc Thesis Page 30

some factors such as cane varieties, qualities of sugarcane, capacity of factory, etc. If
factories would like to have good quality sugar products, they have to meet such color
index. (Rein, 2007)
Flotation clarification is a process which has found extensive use in water treatment and in
the mineral processing industry. The process has also been used for many years in sugar
refining in the form of phosphitation. Until recently flotation separation has received little
fundamental attention. Schofield (2001) remarked as follows: "The lack of fundamental
design criteria in 1991 painted a rather depressing picture of DAF (dissolved air flotation)
design expertise and whilst DAF had existed as an art form far-over 30 years, as a science it
was much less developed".
It has since been the subject of more intensive study using CFD techniques. Application of
flotation clarification in raw sugar mills was pioneered by Tate and Lyle (Bennett et.al,
1977). The process was substantially improved by the development of efficient
polyacrylamide flocculants and a number of installations clarifying syrup have been
installed throughout the world. Systems have been installed in Hawaii, Taiwan, Louisiana,
The Philippines, India, Colombia, South Africa, China, Mauritius and many other countries.
It is attractive because it is a simple process carried out in inexpensive equipment.
Subsequently flotation clarification has been applied to filtrate from rotary vacuum filters
as well. As an alternative to filtration, flotation clarification can be considered as a simpler
and cheaper option. It can be augmented with either sulfitation or phosphatation to achieve
particular sugar quality criteria. In this process, very fine suspended is agglomerated and
floated to the surface by fine air bubbles. (Bennett et.al, 1977)
Separation by flotation does not depend so much on size and relative density of particles
being removed as it does on their surface properties. The process can be considerably
enhanced through the use of appropriate chemicals. In the mining industry selective
flotation of particular types of particles is possible through the addition of chemicals which
change the surface properties. The use of flocculants in flotation has a substantial effect on
the process, leading to mechanical entrapment of air bubbles in the floe particles and
greatly assisting separation.
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The mechanisms involved in the formation and flotation of floe particles are complex.
Little work has been done to elucidate the mechanisms involved, and the process has
evolved through empirical investigations to a viable process. Optimization invariably
requires onsite testing using the particular syrup to be treated. An important aspect
therefore is the method for a suitable laboratory test to simulate the process in practice and
optimize conditions which may vary depending on location. (Rein, 2007)
2.4.2 Benefits of syrup clarification

Syrup clarification is characterized by the stable scum which is obtained. The process is
simple, requires little supervision and the operating cost is low since it requires only the use
of flocculent and may not require any additional chemicals. A further advantage is that the
scum can be directed back to raw juice or perhaps to clarifier mud. If the latter option is
employed, care must be taken to prevent an increase in the pol of the filter cake, but this
can be minimized by optimizing the operation. The major benefits to be obtained from
syrup clarification are an improvement in sugar quality and a reduction in massecuite
viscosities. (Haarof and Edzwald, 2001)
The advantages of this application are greater when the quality of cane being processed is
poor. From being in the position where the mill was regularly unable to produce VHP sugar
in South Africa, Empangeni mill with syrup clarification was able to produce consistently
good quality sugar meeting VHP specifications and for the first time was able to achieve
good molasses exhaustion (Rein 1987). Although these benefits should help to achieve an
improvement in overall sugar recovery, the small improvements anticipated have never
been proven in the face of normal recovery variations. The best way of assessing the
efficiency of syrup is still from turbidity removal results. A large number of syrup samples
tested from many different mills have always shown the potential to achieve a reduction in
turbidity of 80 to 95%. (Rein, 1987).
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2.5 Principals involved in syrup clarification
2.5.1 Effect of operating parameters

Clarification of syrup from a raw sugar mill leads to a very stable scum layer and a high
turbidity removal can be achieved merely with the addition of polyelectrolyte flocculants.
Microscopic examination shows that the majority of the particles in unqualified syrup are in
the range 1-10µm. In the scum the floe sizes are very much larger, comprising air bubbles
and solid particles held together by the flocculent. Laboratory trials show that there is no
significant purity improvement and that the ash removal is small. In addition, the
improvement in syrup color is small. Perhaps because of the high syrup color however, the
removal of turbidity is dramatic. The use of anionic flocculants, high molecular mass
polyacrylamides is essential. The effect of flocculent dosage rate on turbidity removal is
shown in Figure below. (Edzwald, 2001)
This indicates that a dosage of around 15 mg/kg DS is optimum. With very poor quality
syrups, higher dosage rates of up to 30 mg/kg DS are required for best results. It has also
been established that polyelectrolytes with a higher degree of hydrolysis and lower
molecular mass give better results in this application. This generally means that the
optimum flocculent for syrup clarification will be different to that used in juice
clarification. Clarification of refinery melt on the other hand is more efficient if flocculent
with a low degree of hydrolysis is used (Rein, 1988).
Temperature was found to have a significant effect on turbidity removal. This is shown in
Figure below which indicates that a progressive improvement is obtained up to 85 °C after
which the effect of temperature levels off. From Figure it can also be inferred that turbidity
removal is independent of the Brix and viscosity of the syrup. The viscosity of 65 brix
syrup is; about 60 % higher than that of the 60 brix syrup. See in next Figure. Therefore,
viscosity values in the range encountered do not have any effect on this process, and the
better results at higher temperatures are not due to viscosity reduction but due to the effect
on the formation of flocs or on the intermolecular attractions across air/liquid interfaces.
Other work confirms that the viscosity of the syrup does not affect the removal process
(Rein et al. 1987).
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Results of tests on boiling both clarified and unclarified syrup in the laboratory are
described by Rein et al. (1987). The viscosities of molasses produced were measured and
the results are shown in Figure. The viscosity of the clarified syrup and molasses after
boiling was lower by up to 25%. A reduction in molasses viscosity is a significant
advantage, since the viscosity affects centrifuging and the ultimate molasses exhaustion is
generally controlled by the viscosity of massecuite. (Edzwald, 2001)
Figure 2.3 Turbidity removals in syrup as a function of flocculent dosage.
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Figure 2.4 Effect of temperature on turbidity removal.
Figure 2.5 Viscosity of syrup and molasses (adjusted to 73 Brix and 40°C) with and without
syrup clarification. (Rein, 1988)
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2.5.2 Effect of added chemicals

The original Tate and Lyte patent claimed that it is essential to form a primary floc of
calcium phosphate prior to forming a secondary floe with the addition of air and flocculent.
Phosphate addition rates of around 300 mg P2O5/ kg DS are recommended. Other work has
shown that the process can be operated without phosphate addition (Rein et.al 1987) and
that addition of lime and phosphate does not improve the results compared to the standard
process adding only flocculent. (Bennet et al, 1980)
Steindl and Doherty (2005) showed in laboratory tests that color removal is less than 10 %
and is affected by the final PH. They showed that increasing the P2O5 dose from 250 to 500
mg/kg DS gave no benefit. However a number of installations do use phosphoric acid and
lime. One of the problems in using additional phosphate in practice is the drop in pH which
occurs as the reaction of calcium and phosphate goes to completion. A pH drop of about 0.5
units can be allowed for, but the danger of incomplete reaction leads to the possibility of
post-precipitation and additional turbidity generation. Instead of using air, gassing with CO2
and SO2 has been tried (Rein, 1988). Use of CO2 proved to have no advantage, but &
significant improvement could be obtained with SO2 gassing, (i.e.Sulflotation). In this case,
best results were obtained by adding 0.3 kg lime/100 kg DS and 300 mg phosphate/kg DS
and gassing with SO2 to a pH between 6.0 and 6.5 before flotation. (Rein, 1988).
2.5.2.1 The application of cationic flocculants as decolorizing agents

Cationic surfactants (Bennett et al., 1971) can be used to precipitate colorants and other
anionic impurities from sugar liquors. They have a strongly basic center coupled with a
long chain hydrocarbon residue. The cationic center serves only as a means of attaching the
hydrocarbon to the impurity or colorant anion. It is the hydrocarbon that renders the
colorants repellant to water and which causes the color molecule to be precipitated from
solution. The relationship between the molecular structure of cationic surfactants and their
activity as color precipitants have been studied extensively. The most active cationic
surfactants were found to be the di alkyl quaternary ammonium compounds containing two
C6 or two C18 hydrocarbon chains. One product that has been developed for the sugar
industry is Talofloc (dioctadecyl dimethyl ammonium chloride). The mode of interaction of
Talofloc (Bennett, 1982) with colorant molecules is shown in Figure below. (Bennett et al.,
1971)
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Figure 2.6 Mode of interaction of Talofloc with colorant.
Bennett et al. (1971) also found that color can be precipitated from solution with the use of
primary or secondary amines. The addition of 100-200 ppm on cane of Talomel (acyclic di
methylamine polymer) to a syrup clarifier was found to increase the de colorization by 20-
30%. Residual Talomel in final A-sugar should be found below detectable levels. (Trot,
1988)
Talocarb (dimethylamine polymer), an FDA approved color precipitant, when dosed to

final carbonated liquor immediately before filtration at a dosage rate of about 200 ppm on
liquor solids, was found to increase the de colorization over carbonatation by 25-30%.
Talocarb reacts with negatively charged color molecules, neutralizing their charges and
causing precipitation. The precipitated color is subsequently removed during flotation or
filtration. Talocarb in the addition of the flocculants improves the color of both the
carbonated liquor and the liquor from the secondary acrylic resin station by about 20%. In
pilot plant work on melt phosphatation, found that the refined sugars produced from melt
treated with either polyamines or dioctadecyl dimethyl ammonium chloride were of similar
quality and could meet the specifications needed for the soft drink and food industries.
(Mochtar, 1989)
In South Africa, Matic et al. (1977) found that the addition of cationic flocculants during
melt phosphatation improved liquor de colorization as well as phosphate and starch
removals. Rein (1988) found that the addition of 10 ppm of cationic flocculent improves
color removal during refinery sweet water clarification. Getaz and Bachan (1989), in their
MSc Thesis Page 37

work on syrup sulphitation/clarification, found that the addition of a water treatment

flocculants (polyacrylamide) improved the de colorization quite significantly. Polyamines
(copolymers of dimethyl amine and epichlorohydrin) and other chemicals with cationic
properties are used extensively as flocculants in the clarification of potable water. (Getaz
and Bachan, 1989)
In the clarification according to Baxter et al. (1992), flocculants destabilize colloidal

matter by the formation of physical bridges between two or more particles, uniting the solid
particles into a random three-dimensional structure which is loose and porous. In the sugar
industry these cationic chemicals do not act as flocculants as described above but behave
more as decolorizing agents.
Flotation clarification of syrup has been in operation at a few South African mills over the
past 20 years. The original motivation was to enable production of VHP quality sugar at
mills that received poor quality cane. Use of flotation clarification processes has
subsequently been extended to meet like Reduction of insoluble matter in direct
consumption brown sugars; Further reduction of VHP sugar color and Low-cost
purification of melt in a back-end refinery. (Bennett et al., 1971)
Figure 2.7 Typical flotation vessels.
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2.5.3 Effect of aeration of syrup

Separation of particles either in clarification by settling or by flotation clarification is
determined by the terminal velocity of the particle. This is obtained by equating drag and
buoyancy forces. Using the Stokes law relationship for the drag coefficient for spherical
particles of diameter d at low Reynolds numbers (CD =24/Re), the equation for terminal
velocity Ut is:
Where Δp is the difference in density. The viscosity of syrup µl is considerably higher than
that of juice, which means that separation by settling is more difficult in syrup. The density
is also higher, so that the density difference between liquid and solid is insufficient to
achieve settling in practice. However in flotation, the density of the aerated floe is low and
the density difference is large, making separation feasible. Work reported by Echeverri and
Rein (2006) suggests that the density difference is of the order of 800kg/m3 and the average
floc velocity 1.4mm/s (5m/h) from equation the average floe size is 183µm. Considerable
variation around these average values was observed. In practice the particles being floated
are not spherical and Haarof and Edzwald (2001) report that the constant in equation is
higher than 18 and could be as high as 33. Thus the numerical value of the terminal velocity
will be affected by both the shape and size of the aggregates. Since the terminal velocity is
proportional to particle diameter squared, it is desirable to achieve large floe sizes. Three
methods of aeration are possible: (Doherty, 2005)
1. Electro flotation: Uses electrolysis at submerged electrodes to produce very small

bubbles less than 50 µm.
2. Dissolved air flotation (DAF) where bubbles are produced by aerating under pressure
(450- 500 kPa) and releasing the pressure on the supersaturated solution. Bubble sizes are
generally very uniform with an average size between 20 and 60 µm.
3. Dispersed air flotation where air is dispersed mechanically and entrained into the liquid.
Bubble sizes may be somewhat larger and display a wider size range.
MSc Thesis Page 39

Electrolysis is generally not practical on a full scale. Experience in water treatment and
sugar refining has indicated that dissolved air flotation gives better results than the simpler
aeration by dispersed air flotation (Saranin, 1972). In refining, claims that the air bubbles
are occluded within the calcium phosphate floes as they form, and so must be small and
preferably < 30 µm. Thus calcium phosphate formation and aeration should take place
simultaneously and not sequentially. In the case of syrup clarification, larger bubbles are
quite adequate since there be a total absence of calcium phosphate floe, and the attachment
of bubbles to particles is clearly by a different mechanism. (Honjun, 1990)
When processing syrup, dissolved air flotation shows no advantage and if anything, gives
worse performance than dispersed air flotation (Rein et al. 1987). This is evidence of the
stable foam formed in this application is the interests of simplicity and cost, dispersed air
flotation is a better option. Zeng Sixian et al. (1998) have shown that an improvement in
turbidity of the clarified liquor is possible by applying ultrasonic vibration to the liquor
after the addition of flocculent. With the low and variable solids load in syrup, instead an
air to solids ratio is not meaningful. An air to syrup ratio of 0.04 m3/m3 syrup is commonly
used. (Rein et al. 1987)
2.5.3.1 Dissolved Air Flotation (DAF Flotation)

Flotation is described as a gravity separation process in which gas bubbles attach to solid
particles to cause the apparent density of the bubble-solid agglomerates to be less than that
of the water, thereby allowing the agglomerate to float to the surface. (Baxter et al. 1992),
Dispersed air flotation involves the formation of bubbles by diffusers, spargers, and other
mechanical means. Large bubbles are formed and can be effective in treating suspensions
containing large particles such as mineral separation and industrial waste treatment.
Dispersed air flotation is generally unsuitable for liquid or syrup treatment as the bubble
size is large and because of high turbulence and use of undesirable frothing and surfactant
chemicals. However, the French Ozoflot® system applies ozone-rich air as a pretreatment
oxidation process for waters high in algae using diffusers to achieve dispersion. (Doherty,
2005)
In dissolved air flotation, air bubbles are produced by the reduction in pressure of a water
stream saturated with air. The three main types of dissolved air flotation are vacuum
flotation, micro-flotation, and pressure flotation. (Alemayehu, 2000)
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Figure 2.8 DAF Process Schematic
Factors that affect DAF performance are as the followings: Proper coagulation, should
produce destabilized flocs, floc characteristics, small and low-density floc is preferred,
bubble size and rise velocity, 10-100 mm floc bubble size, laminar flow regime, air loading,
ensure dense bubble cloud, floc-bubble attachment, important to know the mechanisms for
floc-bubble attachment, solubility of gases, ensure sufficient air delivery. (Alemayehu,
2000)
2.6 Harmful effects of SO2 consumption with sugar
Sulphur dioxide has traditionally been used in food processing and produces storage to
minimize color formation due to browning reactions associated with amino acids
interacting with invert sugars in the Maillard reaction. Sugar beet processors routinely use
sulphur dioxide in process streams for the same purpose. Among sugar cane processors
worldwide there is mixed interest in usage of sulfitation. In the United States, sulfitation
has rarely been used in cane raw sugar factories since the 1950's. Today, there is renewed
interest in the effectiveness of sulfur dioxide as a color retardant as many US factories are
considering the production of high quality low color raw sugar to be sold as a food grade
sugar. (Anonymous, 1996)
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Under normal ambient temperature and pressure, sulphur dioxide is a colorless, pungent
smelling, nonflammable gas. In very low concentrations this gas can cause extreme eye and
respiratory irritation, thus must be used in a controlled environment. The Egyptians and
Romans burned sulfur to form sulfur dioxide (SO2) as a means of sanitizing wine-making
equipment and today SO2 is used to treat most light colored dehydrated fruit and vegetables
to prevent undesirable enzymatic and non-enzymatic “browning” reactions. Sulfur dioxide
provides the added benefit of acting as a food preservative and functions as an antioxidant.
Sulfite additive has been used extensively in the food industry to retard Maillard reactions.
(Weeny, 1981)
The two main groups of reaction between sugars, ascorbic acid and their dehydration
products and bisulfite, are primarily the hydroxy sulfonate and organo sulfur compounds.
Browning reactions, of whatever type, are caused by the formation of unsaturated, colored
polymers of varying composition. Compounds that engender browning usually contain a
carbonyl or potential carbonyl grouping (Hodge, 1953). Browning can be inhibited by
compounds that block or eliminate or combine with carbonyl groups. The multiplicity of
studies regarding browning reaction theories is reviewed thoroughly in Hodge‟s (1953)
review article. The purpose of sulfiting purified and clarified thin juices are 1) to control
juice color formation; 2) to improve the boiling properties of the juices; and 3) reduce the
excess alkalinity (Ginnis, 1982).
Two methods of sulfuring are: by sulfur stove, burning elemental sulfur for production of
sulfite and bubbling sulfur dioxide through process streams and produced during these
processes is the undesired sulfate ion that can interfere with crystallization causing an
increase in molasses purity and production. The oxidation of sulfite to sulfate is greatly
retarded as the sugar concentration is increased. Sulfitation can control juice color by
interfering with chromophoric molecular groups include carbonyl (ketones), carbonyl
(aldehydes), carboxyl, and amido. “These compounds are characterized by an electron
imbalance, an electronically excited state, a molecular resonance, an absorption of specific
bands of transmitted light, and to the beholder, color” (Ginnis, 1982). Color compounds in
cane and beet sugar products include naturally occurring pigments along with a large
heterogeneous variation of color compounds produced during processing.
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It has been estimated that for a 98.5o pol raw sugar, colorants account for approximately
15-20 % of the weight of non-sugars. In granulated refined sugar the estimate is
approximately 30 ppm (Clarke, 1988).
In the cane sugar factory, the major role of sulfur dioxide has been to make white sugar
rather than raw sugar through inhibition of color forming reactions. This is achieved by
addition of SO2 to the alkenic double bond in an α, β- unsaturated carbonyl intermediate as
well as to the carbonyl group, which yields β-sulfonated aldehydes that are of
comparatively low reactivity in reactions leading to the production of browning compounds
by the Maillard reaction and degradation of invert sugars (Shore, et al., 1984). Sulfur
dioxide also has the ability to inhibit or retard enzymatic browning reactions. Sulfur dioxide
added as 300-500 ppm to raw beet juice resulted in minimal (5%) color reduction (Shore, et
al., 1984). Onna and Sloane (1978) reported that 300 ppm decreased color in syrup and
whole raw sugars by about 25% with crystal color reduced by 46%. Final refined
granulated sugar from this process had 35% less color. (Shore, et al., 1984)
During processing and storage at elevated temperatures, sugar products will darken. All
industries that use sugar products are in turn susceptible to color changes in their products
which may or may not be desirable (Zerban, 1947). When cane and beet juices are heated
and limed during clarification, invert sugar disappears and the color of juices increases with
the amount of lime added. Much of this color is bound to calcium precipitate in the
defecation process. Color changes additionally occur during heating and evaporation
processes, since the juices are exposed to continual heating (70-75o C) over several hours at
slightly alkaline pH in the beet industry and slightly acid pH in the cane industry. The
higher the alkalinity of clarified beet juice, the greater the color increases. The color of
clarified cane juice also increases during evaporation and crystallization even though it is
kept on the slightly acid side. (Zerban, 1947)
In cane and beet processing, there are many variations in procedure for adding sulfur
dioxide. There is cold sulfitation with SO2 added to cold raw juice then limed; alkaline
sulfitation where juice is limed then sulfited and again sulfite added to syrup prior to pan
boiling. Hot sulfitation is where juice is heated first then sulfited and limed; this method is
used to reduce the solubility of calcium sulfite. Other modifications of these procedures are
used according to plant capabilities etc.
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In Northern Europe, a method of combining sulfitation with preliming of diffusion juice

was developed. Small additions of SO2 to an acidic (PH 5.5-6.0) diffusion juice improved
filtration and sedimentation, as well as reduced juice color development. Effect on sucrose
recovery was not discussed. Indonesian cane processors have developed a similar process
using sulfitation with lime with the production of a high standard quality white
consumption sugar for export (Marches, 1953).
This plantation white sugar is the result of two sulfitation procedures, first at original
clarifier when added with lime and second as syrup sulfitation prior to vacuum pan.
Sulfitation in Louisiana is a very old process, possibly originating with French or English
settlers (Spencer, et al., 1945). Cold raw juice was pumped through a sulfur tower with a
countercurrent of sulfur dioxide to produce a fairly good, irregular, near or off-white sugar.
By the late 1930's use of sulfur dioxide was on the decline and was then mainly used for
production of direct consumption molasses. This study was undertaken to determine the
effect of sulphur dioxide on model and real cane process streams. This work is part of
SPRI‟s continuing research on determining the effect of invert and pH on sucrose recovery
and color formation. (Andrews, 2002)
2.7 Carbonatation and Phosphatation process
It is now almost universal for sugar refineries to use either carbonatation or phosphatation
process to clarify the melt liquor. These chemical processes, as well as removing the finely
divided particles of insoluble and semi-colloidal matter, also eliminate significant amounts
of color and other non-sucrose impurities which would otherwise have to be removed at
greater expense in the subsequent decolorization or crystallization processes. Recent
improvements to the traditional refining processes using new chemicals, techniques and
equipment are described and discussed below. (Bennett et al., 1971)
Basically, the process consist of precipitating insoluble calcium phosphates of variable

composition in hot melt liquor by first adding phosphoric acid, or an acid phosphate,
followed by calcium hydroxide, either as slurry with water (milk of lime) or dissolved in
sugar syrup as lime sucrate, to give a final pH of 7.2 – 7.4. This treatment produces a
calcium phosphate floc that is filtered with difficulty. Consequently, air flotation is
commonly used to separate the precipitated solids from the liquor; such systems are called
MSc Thesis Page 44

frothing clarifiers. During the flocculation and in the course of rising through the liquor, the
floccules collect most of the fine suspended impurities in the solution. Impurities such as
gums, waxes, and fine are swept from the liquor and appear at the surface as scums. In this
manner a rather complete separation of the precipitate and impurities is obtained without
resorting to settling or filtration. The scums are then removed from the liquor surface by a
skimming device. (Moodley, 1993)
2.7.1 Phosphatation process

One important modification to the phosflotation process is the application of color
precipitants, like talofloc or colorgone to refinery remelt liquors whereby anionic high
molecular weight color and other impurities are precipitated and subsequently removed as a
flotation scum. Also the replacement of the conventional clarifiers‟ type Jacobs or
Williamson with modern, new circular design, high yield clarifiers has greatly improved the
performance of the phosflotation process. Another advance is the extensive application of
highly efficient polyacrylamide flocculants e.g. taloflote, which not only speeds up
clarification, but also strengthens the floc against shearing forces mainly during the de
sweetening stage. (Bennett et al., 1971)
2.7.1.1 Color removal:

While phosphatation generally achieves a decoloration in the range of 25-30%, the addition
of these color precipitant or cationic surfactants, increases the efficiency of color removal
to a high level of about 70%. (Moodley, 1993)
2.7.1.2 Removal of insoluble solids:

While particles of size under 200 micron are, as a rule, successfully enmeshed in the
floccules and are removed in the process, insoluble solids such as bagacillo and fluff of
over 200 micron have poor floatability characteristics. Consequently, if not separated by
prescreening of the melter liquor, they are carried over with the clarified liquor, imparting
to it a cloudy appearance. Furthermore, if present in sufficient quantity they seriously
impede liquor flow over the char, by forming a mat on the surface layer. Removal of 50-
70% of solids present in the original melt is normally obtainable by the process. (Moodley,
1993)
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2.7.1.3 Secondary precipitation:

Formation of floc in phosphate-clarified liquor is usually referred to as the secondary
precipitation. The occurrence of this floc has been reported by a number of observers. It, of
course, creates problems in the processes subsequent to clarification. In a reasonably well
conducted flocculation process the residual P2O5 is well under 70 ppm and occurrence of
secondary precipitation is not likely. But if something can happen, early or later will it
happens. (Bennett et al., 1971)
2.7.1.4 Removal of ash:

Removal of soluble inorganic constituent from melter liquor is one of the objectives of
clarification. However, the level of removal obtained by any one of the three conventional
methods of clarification is only marginal. Phosflotation, it has been reported by various
writers, removes from nil to 20% of ash in the original liquor.
2.7.1.5 Sucrose inversion:

Exposure of liquor to temperatures ranging from 85 to 99 °C, depending on the type of
clarifier used, during the flotation period leads to inevitable inversion of sucrose. Most
observers reported inversion of the order of 0.01%. Scums from phosphatation systems are
generally sent to secondary clarifiers to reduce their sugar content. Two or three stage
flotation separators, using polyacrylamide flocculating agents as mentioned, permit
countercurrent de sweetening, more or less without filtration equipment. (Schuman, 200)
Nevertheless refineries using modern Phosphatation/Flotation process still have to deal

occasionally with some immanent drawbacks of the system, including high sugar losses,
cloudy clarifier liquors and wet scums muds of difficult disposal. Most operators of the
process admit having witnessed production of both excellent and poor liquors from a given
installation. With the notable exception of one or two refineries, conventional
phosphatation-flotation is found in practice to be a sensitive process. Relatively minor
changes can have a catastrophic effect on flotation characteristics, leading to the appearance
of heavy carry-over in the clarified liquor. If flotation is incomplete, the liquor not only
looks bad but is poor in quality and needs to be filtered before it becomes acceptable for the
char or ion exchanger treatment. The history of phosphatation for clarification of refinery
liquors may be summarized as follows. (Bennett et al., 1971)
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The advantages of phosphatation were recognized in the very early days of sugar refining,
but it was slow to receive acceptance because of the difficulties of floc separation The
reasons for the interminable evaluator debate may lie in the fundamental and inherent
difference that exists between phosflotation and the two other processes carbonatation and
diatomite filtration. This difference is that flotation, unlike diatomite filtration or
carbonatation filtration, has no element of positive separation of the insoluble solids.
Infiltration of the liquor, if the liquor passes through filter cake, it is free of solids of a
certain size. If not it does not pass through filter cake. In flotation the liquor passes through
a clarifier irrespective of whether complete or nil separation of coagulum is obtained.
(Smith and Schuman, 2000)
2.7.2 Carbonatation Process
Refinery carbonatation has been used for over 100 years for the refining of raw sugar. It is a
cheap and robust process. The process consists of adding slurry of calcium hydroxide in
water to the raw melt solution. Then carbon dioxide gas is bubbled into the sugar solution
in saturators, under controlled conditions of pH and temperature. Generally the carbon
dioxide is added to the saturators in two stages, with the major part of the gassing carried
out in the first saturator. The impurities are both absorbed by, and enmeshed in, the
conglomerated particles of the calcium carbonate precipitated by the reaction of the carbon
dioxide and calcium hydroxide.
New significant developments for the carbonanatation process, patented by Putsch Co. in
the last years, has brought the carbonatation, as the process of choice for updating existing
installation or for new refineries. Namely the introduction of Richter Tubes as efficient gas
distributors for carbonatation vessels and the utilization of modern Membrane Filter presses
for single stage filtration of carbonated syrup have given the conventional carbonatation
process an impulse to higher performance level. The ease of separation of impurity from
carbonated liquor in refinery practice is determinate by the filterability of the precipitated
CaCO3. Provided the design and operating conditions of the saturators follow well-known
principles of crystallization processes, the carbonatation system is relatively insensitive to
minor variations.
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It is considerably more dependent on the quantity of lime precipitated in the liquor. For any
liquor there is a particular lime dose at which the filterability will be greatest. The optimum
lime dose varies from below 0, 4 % CaO on solids in some liquors to over 1,2 % CaO in
others. Approximately 30 times more lime is precipitated as carbonate during carbonatation
than as phosphate during phosphatation. (Steindl and Doherty, 2005)
Separation of the clear liquor and the calcium carbonate is done by pressure filtration. This
filtration required expensive two-stage filtration plant for the separation and de sweetening
of the calcium carbonate precipitate. Now day single stage filtration is state-of-the-art. A
significant portion of the calcium carbonate cake is required to act as a filter aid and growth
of a suitable filtering carbonate cake is as important as color removal. One of the main
objectives of carbonatation is the removal of the impurities present in the raw sugar
entering the refinery. These impurities will have negative effects on some of the unit
operations in the refinery. Firstly certain impurities will have a profound effect upon the
nucleation and growth process involved in the formation of the calcium carbonate
conglomerate. As a consequence such impurities will impact upon the filtration processes in
the refinery. Secondly the presence of another impurity will adversely affect the sugar
crystallization process and lastly refined sugar quality will be influenced by this impurities.
Praxis have shown that carbonatation is very effective in the in the removal of the following
impurities: Results of impurity removal from melt during carbonatation (1,10 % CaO
addition on Brix): Color 55%,Turbidity 90%, Starch 93%, Gums 29%, Sulphates 86%,
Phosphates 100%, Magnesium 67%. The following comments can be made regarding the
results in the above: About 55% of the clour is removed, Most of the turbidity (90%),
starch (93%), sulphates (86%) and phosphates (100%) are removed, a small amount of the
gums is removed, and a high proportion of magnesium is also removed. (Smith and
Schuman, 2000)
In addition, it has been shown that during carbonatation glucose, fructose and aconitic acid,
if not precautions are taken, can be easily destroyed with increase in lactic acid and higher
molasses losses. Basically reducing the contact time of raw melt with lime at high
temperature noticeably reduces the invert sugar destruction. It has also been shown that
carbonatation removed floc-forming impurities and it has generally been accepted that
carbonatation refineries produce floc-free refined sugar.
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The two main components responsible for formation of floc are proteins and
polysaccharides, known as floc precursors, which are removed by carbonatation. In
addition it is confirmed that color removal during carbonatation is a function of the melt
color, amount of lime added and the final pH. (Steindl and Doherty, 2005)
2.7.2.1 Comparative quality

Being concerned with the problems of attaining maximum clarification at optimum costs,
technologists inevitably ask which one of three processes of melt clarification - diatomite
filtration, phosflotation or carbonatation - provides the best answer. This question arises in
planning a new refinery or when the existing process becomes unacceptable either for
technological or economic considerations. A complete answer to this question can only be
obtained by going through a close economic analysis of the alterative involving such factors
as cost of capital, labor, and materials used in the alterative processes, level of education of
the available labor, size of the plant etc. In the present context we can consider only the
technical effectiveness of the respective processes. Even though this appears to be a simple
question it is not easily answered.
There have been changes from one process to another since the 1950`s. Changes took place
from diatomite filtration either to phosflotation or carbonatation. There were also changes
from phosflotation to carbonatation. Of the newly built refineries the smaller sizes adopted,
as a rule, phosflotation, while the larger ones preferred carbonatation. (Smith and Schuman,
2000)
2.7.3 Coagulation and Flocculation

With the increasing demand to achieve efficient and cost effective removal of color in the
production of high quality white sugar, a number of processes and chemicals have been
investigated. Cationic flocculants such as polyamine chemistries are an example of
decolorizing agents used to precipitate colorants and other anionic impurities from sugar
liquors (Bennett et al., 1971; Moodley, 1993). Cationic polymers can be used to bind and
facilitate precipitation of color bodies from refinery melt liquor by way of the negatively
charged color bodies being attracted to the positively charged polymer, thus forming an
insoluble precipitate that can be easily removed from the refinery melt. (Moodley, 1993)
MSc Thesis Page 49

In this work, polymers were evaluated under laboratory conditions, utilizing refinery melt
liquor that was subjected to various refining processes. These include (i) carbonatation
where lime and carbon dioxide gas (recovered from boiler flue gas) form a calcium
carbonate precipitate that absorbs color particles, (ii) sulphitation, where sulphur dioxide
gas is reacted with lime to produce a calcium sulphite precipitate which adsorbs to the color
bodies, and (iii) phosphatation whereby lime and phosphoric acid are reacted together to
form a calcium phosphate precipitate, which absorbs and entraps the colour bodies. The
colour bodies are then removed either by filtration or by flotation in an air flotation unit
using a high molecular weight anionic flocculant to enhance the separation of the solids
from the melt liquor. (Bennett et al., 1971)
The cationic polymeric decolourisation agent is used to enhance rather than replace the
refining processes. Benefits include a greater performance efficiency as well as enhanced
colour removal during periods of exceptionally high colour loading.
Phosflotation (Phosphatation-flotation) is a widely practiced method for the defecation of a

raw sugar melt. The process involves the coagulation of impurities with a calcium
phosphate precipitate followed by the flotation of this coagulum to yield a clear liquor
underflow. In recent years, a number of new materials have been introduced in order to
improve the efficiency of the process. An upgrading in the through put of flotation clarifiers
have been achieved by the application of high molecular weight anionic polyacrylamides as
flotation aids. Due to their long chain length and negative charge in solution, these
polymers build up large flocs which can be floated at a much enhanced velocity. This
ensures a high throughput of turbidity free liquor. (Shephard, 1977)
One of the important developments has been the introduction of the Talofloc process which
aims at achieving a large measure of de colorization during defecation. A cationic
surfactant (Talofloc) is added prior to the precipitation of phosphate and the final aerated
suspension of calcium phosphate coagulum is flocculated by the addition of an anionic
polyacrylamide (Taloflote). The advantage of obtaining considerable de colorization in the
phosphatation process lies in the greater economy that can be achieved in the subsequent
decolorizing stage." The purpose of this study was to investigate the degree of impurity
removal that can be achieved with the aid of cationic flocculants. In addition, the effect on
the process of a polyacrylamide flotation aid was investigated. (Shephard, 1977)
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2.7.3.1 Coagulation:
Coagulation is the step where colloidal particles (similar to spheres of a diameter of less
than 1 micrometer) are destabilized. Coagulation comes from the latin word 'coagulare'
which means „to agglomerate'. Coagulation is the result of the addition of chemical reagents
to liquid suspensions where the dispersed colloidal particles are assembled in larger
aggregates called flocs or microflocs. Coagulation is an intermediary step, but it is essential
to the physico-chemical treatment process of juice and syrup. This is the first step in the
elimination of colloidal particles and its main function is to destabilize the particles. This
destabilization is essentially the neutralization of the electrical charge present on the surface
of the particle thus facilitating the agglomeration of the colloids. (Moodley, 1993)
Colloids are insoluble particles suspended in water. Their small size (less than 1 micron)
makes the particles extremely stable. They can have different origins: Mineral: silt, clays,
silica, hydroxydes and metallic salts and Organic: humic and fulvic acids, color,
surfactants. Micro-organisms such as bacteria, plankton, algae, and viruses are also
considered as colloids. The stability and consequently the instability of suspended particles
is a factor of different attraction and repulsion forces: ( Runggas, 1977)
 Van der Waals forces

 Electrostatic forces
 Universal attraction
 Brownian notion
Coagulation is both a physical and a chemical process. The reactions between particles and
coagulant will allow the formation of aggregates and their subsequent sedimentation.
Cationic coagulants neutralize the negative charge of colloids and form a spongy mass
called microflocs. The coagulation mechanism can be summarized of the two; charge
neutralization which is corresponds to the lowering of the electrical charges that have a
repulsion effect on the colloids and aggregation of the particles.
2.7.3.2 Flocculation:
Flocculation is the step where destabilized colloidal particles (or the particles formed
during the coagulation step) are assembled into aggregates. The flocculation step can only
operate on a water/wastewater where the particles are already destabilized. It is the logical
step following coagulation. (Bennett et al., 1971)
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Figure 2.9 diagram of flocculation
2.7.3.3 Destabilized particles:

The origin of destabilized particles is various and depends mainly on the origin of the water
to be treated. They can come from an initial coagulation step. The charge (+ or -) brought
by the flocculants will be selected according to the nature of destabilized particles in the
water. In general the selection follows the pattern as: Anionic flocculants (-) for mineral
particles and Cationic flocculent (+) for organic particles. (Runggas, 1977)
2.7.3.4 Flocculation mechanism:

Flocculants, with their very high molecular weights (long monomer chain) and their charge
content, fix the destabilized particles and aggregates along the polymer chain. There
follows, during the flocculation step, an increase in the size of the particles present in the
water phase resulting in the formation of flocs. The type of bonds between the destabilized
particles and the flocculant are mainly ionic bonds and hydrogen bonds. Amongst the 800
different flocculants of the Flopam range, two main categories of flocculants can be
distinguished.
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2.8 Froth flotation fundamental principles
Froth flotation is a highly versatile method for physically separating particles based on
differences in the ability of air bubbles to selectively adhere to specific mineral surfaces in
mineral/water slurry. The particles with attached air bubbles are then carried to the surface
and removed, while the particles that remain completely wetted stay in the liquid phase.
Froth flotation can be adapted to a broad range of mineral separations, as it is possible to
use chemical treatments to selectively alter mineral surfaces so that they have the necessary
properties for the separation. It is currently in use for many diverse applications, with a few
examples being: separating sulfide minerals from silica gangue (and from other sulfide
minerals); separating potassium chloride (sylvite) from sodium chloride (halite); separating
coal from ash-forming minerals; removing silicate minerals from iron ores; separating
phosphate minerals from silicates; and even non-mineral applications such as de-inking
recycled newsprint. It is particularly useful for processing fine-grained ores that are not
amenable to conventional gravity concentration. (Klimpel, 1995)
Figure 2.10 The flotation system includes many interrelated components, and changes in
one area.
MSc Thesis Page 53

Froth flotation is a good example of an engineering “system”, in that the various important
parameters are highly inter-related, as shown in Figure 2.11. It is therefore important to take
all of these factors into account in froth flotation operations. Changes in the settings of one
factor (such as feed rate) will automatically cause or demand changes in other parts of the
system (such as flotation rate, particle size recovery, air flow, pulp density, etc.) As a result,
it is difficult to study the effects of any single factor in isolation, and compensation effects
within the system can keep process changes from producing the expected effects. This
makes it difficult to develop predictive models for froth flotation, although work is being
done to develop simple models that can predict the performance of the circuit from easily-
measurable parameters such as solids recovery and tailings solid content (Klimpel, 1995).
2.8.1 Types of Flotation

Different methods of producing gas bubbles give rise to different types of flotation
processes. These are electrolytic flotation, dispersed air flotation, and dissolved air
flotation. The basis of electrolytic or electro flotation is the generation of bubbles of
hydrogen and oxygen in a dilute aqueous solution by passing a DC current between two
electrodes. The application of electrolytic flotation has been restricted mainly to sludge
thickening and small wastewater treatment plants in the range 10 to 20 m3/h and has limited
application to drinking water treatment. (Saranin, 1972)
2.8.2 Hydrophobicity/hydrophilicity
The basis of froth flotation is the difference in wet abilities of different minerals. Particles
range from those that are easily wet able by water (hydrophilic) to those that are water-
repellent (hydrophobic). If a mixture of hydrophobic and hydrophilic particles are
suspended in water, and air is bubbled through the suspension, then the hydrophobic
particles will tend to attach to the air bubbles and float to the surface, as shown in Figure 3.
The froth layer that forms on the surface will then be heavily loaded with the hydrophobic
mineral, and can be removed as a separated product. The hydrophilic particles will have
much less tendency to attach to air bubbles, and so it will remain in suspension and be
flushed away (Whelan and Brown, 1956).
Particles can either be naturally hydrophobic, or the hydrophobicity can be induced by

chemical treatments. Naturally hydrophobic materials include hydrocarbons, and non-polar
solids such as elemental sulfur. Coal is a good example of a material that is typically
MSc Thesis Page 54

naturally hydrophobic, because it is mostly composed of hydrocarbons. Chemical

treatments to render a surface hydrophobic are essentially methods for selectively coating a
particle surface with a monolayer of non-polar oil. (Kawatra, 1987)
Figure 2.11: Selective attachment of air bubbles to hydrophobic particles.
The buoyancy of the bubbles then carries these particles to the surface, leaving the
hydrophilic particles behind.The attachment of the bubbles to the surface is determined by
the interfacial energies between the solid, liquid, and gas phases. This is determined by the
Young/Dupre Equation,
where Ylv is the surface energy of the liquid/vapor interface, sv is the surface energy of the
solid/vapor interface, sl is the surface energy of the solid/liquid interface, and is the
“contact angle”, the angle formed at the junction between vapor, solid, and liquid phases, as
shown in Figure 4. If the contact angle is very small, then the bubble does not attach to the
surface, while a very large contact angle results in very strong bubble attachment. A contact
angle near 90° is sufficient for effective froth flotation in most cases. (Eisele, 1987)
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Figure 2.12: Contact angle between and air bubble and a solid surface immersed in liquid.
2.8.3 Particle/Bubble Contact

Once the particles are rendered hydrophobic, they must be brought in contact with gas
bubbles so that the bubbles can attach to the surface. If the bubbles and surfaces never come
in contact, then no flotation can occur. Contact between particles and bubbles can be
accomplished in a flotation cell such as the one shown schematically in Figure below.
(Eisele, 1987)
Figure 2.13: Simplified schematic of a conventional flotation cell.
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The rotor draws slurry through the stator and expels it to the sides, creating a suction that
draws air down the shaft of the stator. The air is then dispersed as bubbles through the
slurry, and comes in contact with particles in the slurry that is drawn through the stator.
Particle/bubble collision is affected by the relative sizes of the particles. If the bubbles are
large relative to the particles, then fluid flowing around the bubbles can sweep the particles
past without coming in contact. It is therefore best if the bubble diameter is comparable to
the particle diameter in order to ensure good particle/bubble contact. (Eisele, 1987)
2.8.4 Collection in the Froth Layer

Once a particle and bubble have come in contact, the bubble must be large enough for its
buoyancy to lift the particle to the surface. This is obviously easier if the particles are low
density (as is the case for coal) than if they are high-density (such as lead sulfide). The
particle and bubble must remain attached while they move up into the froth layer at the top
of the cell. The froth layer must persist long enough to either flow over the discharge lip of
the cell by gravity, or to be removed by mechanical froth scrapers. If the froth is
insufficiently stable, the bubbles will break and drop the hydrophobic particles back into
the slurry prematurely. (Kimpel, 1995)
However, the froth should not be so stable as to become persistent foam, as foam is difficult
to convey and pump through the plant. The surface area of the bubbles in the froth is also
important. Since particles are carried into the froth by attachment to bubble surfaces,
increasing amounts of bubble surface area allows a more rapid flotation rate of particles. At
the same time, increased surface area also carries more water into the froth as the film
between the bubbles. Fine particles that are not attached to air bubbles will be
unselectively carried into the froth along with the water (entrainment); excessive amounts
of water in the froth can result in significant contamination of the product with gangue
minerals. (Kawatra, 1987)
2.8.5 Reagents
The properties of raw mineral mixtures suspended in plain water are rarely suitable for
froth flotation. Chemicals are needed both to control the relative hydrophobicity of the
particles, and to maintain the proper froth characteristics. There are therefore many
different reagents involved in the froth flotation process, with the selection of reagents
depending on the specific mineral mixtures being treated. (Glembotskii et al. 1972)
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2.8.5.1 Collectors:
Collectors are reagents that are used to selectively adsorb onto the surfaces of particles.
They form a monolayer on the particle surface that essentially makes a thin film of non-
polar hydrophobic hydrocarbons. The collectors greatly increase the contact angle so that
bubbles will adhere to the surface. Selection of the correct collector is critical for an
effective separation by froth flotation. Collectors can be generally classed depending on
their ionic charge: they can be nonionic, anionic, or cationic. The nonionic collectors are
simple hydrocarbon oils, while the anionic and cationic collectors consist of a polar part
that selectively attaches to the mineral surfaces, and a non-polar part that projects out into
the solution and makes the surface hydrophobic. Collectors can either chemically bond to
the mineral surface (chemisorption), or be held on the surface by physical forces (physical
adsorption). (Eisele, 1987)
2.8.5.2 Chemisorption:
In chemisorption, ions or molecules from solution undergo a chemical reaction with the
surface, becoming irreversibly bonded. This permanently changes the nature of the surface.
Chemisorption of collectors is highly selective, as the chemical bonds are specific to
particular atoms.
2.8.5.3 Physisorption:
In physisorption, ions or molecules from solution become reversibly associated with the
surface, attaching due to electrostatic attraction or vandeerWaals bonding. The physisorbed
substances can be desorbed from the surface if conditions such as pH or composition of the
solution changes. Physisorption is much less selective than chemisorption, as collectors will
adsorb on any surface that has the correct electrical charge or degree of natural
hydrophobicity. (Glembotskii et al. 1972)
2.8.5.4 Nonionic Collectors:

Hydrocarbon oils, and similar compounds, have an affinity for surfaces that are already
partially hydrophobic. They selectively adsorb on these surfaces, and increase their
hydrophobicity. The most commonly-floated naturally-hydrophobic material is coal.
Addition of collectors such as fuel oil and kerosene significantly enhances the
hydrophobicity of the coal particles without affecting the surfaces of the associated ash-
forming minerals. This improves the recovery of the coal, and increases the selectivity
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between coal particles and mineral matter. Fuel oil and kerosene have the following
advantages over specialized collectors for froth flotation: 1) they have low enough viscosity
to disperse in the slurry and spread over the coal particles easily, and 2) they are very low-
cost compared to other compounds which can be used as coal collectors. (Kawatra, 1987)
In addition to coal, it is also possible to float naturally-hydrophobic minerals such as

molybdenite, elemental sulfur, and talc with nonionic collectors. Nonionic collectors can
also be used as “extenders” for other collectors. If another, more-expensive collector makes
a surface partially hydrophobic, adding nonpolar oil will often increase the hydrophobicity
further at low cost.
2.8.5.5 Anionic Collectors:

Anionic collectors are weak acids or acid salts that ionize in water, producing a collector
that has a negatively-charged end that will attach to the mineral surfaces, and a hydrocarbon
chain that extends out into the liquid, as shown in Figure below. (Eisele, 1987)
Figure 2.14: Adsorption of anionic collector onto a solid surface.
The anionic portion is responsible for the attachment of the collector molecule to the
surface, while the hydrophobic part alters the surface hydrophobicity. (Kawatra, 1987)
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CHAPTER 3 MATERIALS AND METHODS
3.1 Site of the experiment
The experiment was held at Wonji Shoa Sugar Factory‟s laboratory. The laboratory is
found at Oromiya Regional State near Nazareth City at 110 Kilometers from Addis Ababa.
Any research related to the sugar cane production and sugar processing technologies are
held mainly in this laboratory.
The experiment was conducted based on syrup produced from the mixed cane varieties and
taken from the factory as a sample. The syrup clarification experimental work and the
determination of the response variables were done at the research laboratory service of the
station.
Figure 3.1 Wonji Sugar Factory
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3.2 Materials
Sample for the experiment was:
 Raw syrup from evaporator
The equipment and materials:
 Measuring cylinder,
 Conical flask,
 PH meter,
 Stirrer
 Precision refractometer, Buchner funnel,
 spectrophotometer,
 1cm cell,
 Whatman No. 5 filter paper
 membrane filters
 glass electrode
 1-liter beaker
 Volumetric flask
Chemicals and Reagents:
 Talodura,
 Phosphate,
 CaCO3
 NaOH solution,
 HCl solution,
 Kieselguhr filters aid.
 Sodium thiosulphate
 Lime saccharate
 Potassium dichromate
 Potassium iodide solution (For standardization)
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3.3 Sample Preparation
Syrup of 16 L was collected from evaporator for one run. Laboratory scale experiment was
conducted on syrup clarification by Talodura process in contrast to the conventional syrup
sulphitation system. The experiment was conducted on samples of syrup collected from the
final effect of evaporators, at five levels of phosphate concentration (as Hussein
Mohammed, 2013 states the gap is good if the dosages start from a hundred and seven
hundreds,) (117.8, 250, 350, 450, 550 and 682.8mg/kg) using phosphoric acid of food grade
neutralized with lime saccharate to PH 7.0 and treated with Talodura solution of
concentration 7.2, 8, 9, 10, 11 and 12.8mg/kg of solid. The experiment conducted was
analyzed using central composition design (CCD) and JMP13.
Talodura flocculants solution of 0.1% strength was prepared from powder by feeding in to
spray water of 10-55°C and mixed by stirring. The solution then kept for a minimum of 2
hours after preparation to allow complete hydration of the polymer. The thick syrup from
the last effect of evaporator was heated to 85°C and then treated with each level
combinations of phosphoric acid and the PH was adjusted to 7.0 using lime saccharate. The
treated syrup was aerated in the system that ensures the correct size distribution and
volumetric concentration of the air bubbles. The aerated syrup is dosed with solution of
Talodura as per the CCD run order.
The secondary flocculation of primary flocs and air bubbles were developed. The
flocculated syrup was now kept in clarifier of 1 Liter graduated measuring cylinder for 20
minutes. Such treatment was done for the rest CCD combinations of phosphate and
Talodura. The flocculated impurities separate as floc scum, which was removed from the
surface of the syrup by scraping mechanism.
The samples of syrup clarified by Talodura process was compared with that of the one
treated by sulphitation method and subjected to laboratory analysis for the following
parameters: Color, turbidity, reducing sugars, conductivity ash, insoluble matter, residual
SO2, viscosity of the syrup suspended matter, lime salts and purity of syrup.
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3.4 Analytical methods
The quality of syrup like color, sulfur dioxide content, and turbidity was calculated as the
following.
3.4.1 Color:
The ICUMSA color method 4 using a wavelength of 420nm was applied for testing the
color of light colored syrup, as usually made on clarified juice to measure effectiveness of
clarification. Apparatus used for the purpose were; spectrophotometer equipped with 10, 5
and 1cm cells, membrane filters of 47mm diameter, pore size 0.45 µm, precision
refractometer and reagents used was 0.1M TEA solution and 0.05M HCl, 0.05M NaOH.
Procedure: A diluted solution of sample to be tested, (50 brix solution) was prepared. For
the brix of syrup was 65, then 100g of 50 brix solution was weighed 100/65 x 5 = 7.69g of
syrup, made up to 100g and mixed. The pH of the solution was adjusted to 7.0 ± 0.2 with
TEA buffer solution and mixed. (The use of TEA buffer solution is better than a 1M HCl or
1M NaOH solutions). The solution was filtered through a membrane filter with pore size
0.45µm. The solution was placed in an optical cell and measure absorbance, at 420nm in a
spectrophotometer using distilled water as reference standard of zero color. (The cell length
was chosen so that the instrument reading was between 20-80% transmittance and 0.1, 0.7
absorbance.)
e) The result was expressed as the following.
ICUMSA 420 color unit =
Where: b. Cell length (cm)

c. Concentration of total solids (gm/ml)
3.4.2 Turbidity
The turbidity of clarified juice or syrup is a measure of the effectiveness of the clarification
process. The ICUMSA Colors of unfiltered and filtered samples was measured at 420nm
and the difference between the readings was the turbidity of the sample. Apparatus used
were: Precision refractometer, pH meter, Buchner funnel, spectrophotometer, 1cm cell,
Whatman No. 5 filter paper and the reagents were NaOH 1M solution, HCl 1M solution,
Kieselguhr filter aid.
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Procedure: The original brix of the clarified syrup was determined and prepared a 65 brix
solution. The original brix = 60, then for 100g of 65 brix solution, the weight of the original
clarified syrup taken for dilution = 6.5/60 x 100 = 10.833g. The amount of clarified syrup
was weighed out necessary to make 65 brix solutions (in this case 10.833g of clarified
syrup) in a beaker and made up to 100g with distilled water. The solution was divided into
equal portions in two 100ml beakers. The first portion of the sample was taken and filtered
through Buchner funnel with Whatman No 5 filter paper using kieselguhr filter aid. The
first 10ml running was discarded. The pH of the filtrate was adjusted to 7.0 ± 0.2 using
either 1M NaOH. Absorbance (A1) in 1cm- cell at 420nm was measured against distilled
water blank.
ICUMSA 420 Color C1 =
Concentration of total solids (g ml-1) = Brix x true density/100. The 2nd portion of the
sample (do not filter) was taken and adjusted to the pH to 7.0 ± 0.2 using NaOH.
Absorbance (A2) was measured in 1cm cell at 420nm against distilled water blank.
ICUMSA420 Color C2 =
The result was expressed as the following:
Turbidity of Clarified syrup= C2-C1 =
3.4.3 The pH
PH of sugar solution (50g/100g concentration) was determined using glass electrode
attached to pH meter after calibration at pH 4.00, 7.00 and 9.00 at 20°C following
ICUMSA method GS1/2/3/4/7/8-23 (1994)
3.4.4 Sulphur Dioxide (SO2).

The Iodometric method is convenient for routine factory control for clear juice, syrup as
well as plantation white sugar which is accurate enough for the purpose and the analysis,
take little time. SO2 exists as sulphurous acid (H2SO3) in aqueous solutions. Starch solution
forms an intense blue absorption compound with the presence of Iodine. When titrating
with iodine in the presence of starch the end point is determined from the appearance of
permanent blue color with excess of one drop of Iodine solution. The method was used for
clear juice, syrup and plantation white sugar for routine factory control. Reagents used for
MSc Thesis Page 64

this specific experiment was: 0.01N iodine solution, starch solution, HCl (1:3), 0.1N
sodium thiosulphate solution, potassium dichromate, 20% potassium iodide solution (For
standardization)
Procedure: 200ml of syrup sample was taken and diluted by adding 400ml distilled water.
The burette was filled with this diluted syrup solution. 25ml of 0.01N iodine solution was
Pipette into porcelain dish and 5ml of (1:3) diluted HCl solution was added. The Iodine
solution with the diluted syrup sample from the burette was titrated till the brown color
begins to disappear. Then a few ml of starch solution was added and continued titration till
the blue color disappears. The volume of syrup taken for titration was read (ml) from the
burette.
The result was calculated as the following.
From the reducing and oxidizing property of H2SO3 and I2 respectively,
1ml 0.01 N I2 oxidizes = 0.32mg SO2
25ml 0.01 N I2 oxidizes = 25 x 0.32 mg SO2
V ml diluted syrup (burette reading) oxidizes = 25 x 0.32mg SO2
600ml diluted syrup = x 25 x 0.32mg SO2
1lit. (1000ml) undiluted syrup = x x 25 x 0.32 mg SO2
= 24000/V mg SO2,
Where: V is the burette reading of diluted syrup.
3.4.5 Determination of Brix in syrup (dilution 1:3 m/m)

A 200 g of syrup was weighed out in a 1-liter beaker. Distilled water was added and
brought to 600 g stirred and mixed well. About 200 ml of the diluted sample was filtered
through fluted Whatman No. 91 filter paper. The 1st 20 ml of filtrate was rejected and
sufficient filtrate in a beaker was collected. The refractometer Brix as close to 200C as
possible was determined. Expression of the result was Brix of syrup = refractometer
reading x 3
3.4.6 Determination of Pol in Syrup Clarification

Determination of the Brix of syrup was as described above. About 200 ml (1:3) m/m
diluted solution of syrup in a beaker was taken. Minimum quantity of Horne‟s dry basic
lead acetate (about 0.5g/100 ml) was added and mixed well. Filtered through Whatman
No.91 filter paper or equivalent, discarded the first 25ml of the filtrate was discarded and
MSc Thesis Page 65

the rest was collected. The clear filtrate was polarized without de leading and without delay
at 20°C; in 200 mm pol tube and the pol reading was taken. From the brix obtained, the pol
factor from table was found. Expression of the result was (pol %syrup) Pol % syrup = pol
reading x pol factor x 3 was registered.
3.4.7 Determination of Soluble Phosphate content

Phosphate content of juice or syrup is the most important factor for efficient clarification. In
sugarcane the phosphates are inorganic as well as organic. The inorganic phosphates exist
as free phosphate ion taken part in juice clarification. Therefore, juice with adequate
quantity of inorganic phosphate is desirable. If inorganic phosphate level in juice less than
300ppm w/v the juice cannot be properly clarified and addition of phosphate may be
required. The amount of inorganic phosphate left in clarified juice should be not less than
10ppm, which converts calcium and magnesium into non-scaling form in the proceeding
evaporation process. Hence this method is for determination of soluble orthophosphate.
Principle involved calculating the syrup phosphate was: Ammonium molybdate reacts in an
acid medium with dilute solutions of orthophosphate to form molybdophosphoric acid,
which can be converted by reducing agent like stannous chloride or ascorbic acid to the
intensely colored molybdenum blue.
Apparatus used for the experiments was: pH meter spectrophotometer, pipettes 50 ml

beakers, 150 100ml, volumetric flasks of 50, 100ml and reagents and materials used were:
0.1M H2SO4 Potassium hydrogen phosphate, 0.1M Na OH ammonium molybdate solution,
ascorbic acid Kieselguhr, Whatman No. 91, Phosphate in mixed Juice, clear Juice and
syrup.
Procedures: A 100ml of syrup brix diluted to the juice level was mixed with some filter aid
and filtered through Whatman No. 91 filter paper. A 50ml of filtered juice was pipette into
a 100ml beaker and adjusted the pH with 0.1M H2SO4 or NaOH. Then it was transferred
quantitatively to 100ml volumetric flask and made up to mark with distilled water. An
aliquot of the diluted juice was pipette into a 150ml beaker. Distilled water was added to
about 40ml. 4ml ammonium molybdate solution was added and mixed. A 0.1g ascorbic
acid was added and covered with watch glass and boiled gently for exactly 1 minute. The
solution quickly cooled and transferred into the solution of 50ml volumetric flask and made
up to mark with distilled water. The optical density of the blue color was measured in
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spectrophotometer using 1cm cell at 650nm against a blank of distilled water.

Corresponding to the optical density the P2O5 concentration was found from the standard
curve.
3.4.7.1 Preparation of Standard Curve for phosphate (P2O5)

Stock Phosphate solution was prepared by dissolving 0.1916g potassium dihydrogen
phosphate (KH2PO4) in a 1litre of water. This solution contains 100 mg P2O5/liter, i.e.
0.1mg P2O5/ml. Standard phosphate solution was prepared again by pipette 25ml stock
phosphate solution and diluted to 250ml in a volumetric flask. This solution was contains
0.01mg P2O5/ml. For calibration 0, 5, 10, 15, 20 and 25ml standard phosphate was pipette
solution into six 150ml beakers and added distilled water to about 40ml. To each beaker
4ml ammonium molybdate solution was added and mixed. 0.1gm ascorbic acid was added
and covered with watch glass, heated to boiling and boiled for exactly 1min, cooled the
solution quickly, transferred quantitatively to 50ml volumetric flasks and made up to mark
with distilled water. These solutions were containing: 0, 0.05, 0.1, 0.15, 0.20, 0.25mg
P2O5/50ml test solution. The optical density was measured of the blue color in a
spectrophotometer using 1cm cell at 650nm against distilled water blank. In our case:
Table 3.3 Calibration of phosphate concentration against its optical density
From the measured optical density of each test solution and phosphate concentration, a
graph of optical density against P2O5 concentration was plotted by noticing whenever a new
batch of reagent is used a standard curve should be prepared.
Expression of the result was like the following:
Ppm P2O5 in juice =
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3.5 Experimental Design
The effect of two factors (phosphitation and flocculation dosages) on the optimization of
syrup clarification was evaluated and Central Composite Design (CCD) for two-factors was
employed to conduct the experiment. Central Composite Design (CCD) with 8 center points
and a total run of 16 in triplicates was used at constant temperature of 85°C investigate the
effect of levels of factors on the response variables. The main variables considered here
are: Turbidity, color, sulphur dioxide content, reducing viscosity. Then the optimum
clarification level combinations of the factors were determined. JMP™ Software was used to
provide experimental designs, generate second degree polynomial models and make
statistical evaluations. The experiment was conducted using a lower and upper real value of
7.2 and 12.8 pH values for Talodura flocculent and the lower real levels of Phosphitation
was 117.2 and the upper real value will be 682.8 The lower and upper real values were
coded as -1 and +1 respectively and that of the center points was coded as 0. The lower and
upper axial points were coded by –α and +α respectively as shown in Table
Coded levels
-α -1 0 +1 +α
Factors Fixed Temp 85⁰C
P2O5 ≤ 117.8 117.8 400 682.8 ≥ 682.8

At fixed ( PH )
Talodura 7.0 7.2 8.5 9.5 10.5 12.8
Table 3.1 Coded and corresponding actual value of the factors used in the central composite
design.
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Condition phosp floc Condition phosp floc Condition phosph floccul
5. +α 0 9 0 0
1. -1 -1
6. -α 0 10 0 0
2. -1 +1
7. 0 +α 11 0 0
3. +1 -1
8. 0 -α 12 0 0
4. +1 +1
13. 0 0
14. 0 0
15. 0 0
16. 0 0
22 =full factorial design Trials at axial points Trials at centeral points

Nf=4 Na=4 No =8
Table 3.2 Central composite design (CCD) for coded levels of the two factors
(phosphatation and flocculation)
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3.6 Statistical analysis
The data was analyzed and modeled using the statistical software JMP13 (by SAS Institute
Inc., Cary, NC, USA). Second degree polynomial models were generated. The significant
terms in the models were identified by analysis of variance (ANOVA) for each response.
Significance was judged if the probability level of the F-statistic calculated from the data
was less than 0.05. The model adequacy was checked by R2, R2adj and, Lack of Fit test.
The Tables of summary of fit, ANOVA, lack of fit and parameter estimates which were
generated by the software were presented in the Appendix part. Super imposed contour
plots were developed to search the optimum conditions for the three main responses,
namely, turbidity, color, and viscosity reduction.
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CHAPTER 4 RESULTS AND DISCUSSION
4.1 Results of the Syrup analysis from Wonji Sugar Factory
The raw syrup taken from the factory done by double sulfitation without any treatment has
the following values for color, turbidity, viscosity, phosphate, viscosity and purity.
Sample Sample Parameters
source Pol Brix Purity Turbidity Color Viscosity SO2 P2O5

code
(0Z) (%) (%) IU (IU) (mpa.s) ppm ppm
A 49.79 60.63 82.12 13731 17451 60 30 117.2

Wonji
Table 4.1 Analytical results of syrup from Wonji Sugar Factory.
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4.2 Results of syrup clarified at different level of combinations of phosphate

and flocculation.
The results of experimental work from the laboratory and analytical data for response
variables (Table) obtained are as follows. The results of each color, turbidity and viscosity
reduction were filled as CCD order and the data analyzed using the JMP software are
presented and discussed here under accordingly.
Table 4.2 Average results obtained from syrup at different level combinations of phosphate
and flocculation.
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4.3 Color of clarified syrup
It was observed that the minimum and the maximum color values were 9772 and 14669 IU,
respectively were gained after treatment with different dosages of the phosphate and
talodura flocculant. This wide range of responses indicated that the color value was
significantly affected by the dosage of phosphate and flocculants. For example, the
combination 668 ppm phosphate with 12 ppm flocculants gave a color value of 9772 where
as that of 117 ppm phosphate and 7.2 ppm flocculants gave a color of 14669 IU.
A quadratic model of color was developed as shown below: Final equation in terms of
actual factors:
Where C=Predicted color, t=talod, p=phosphate values.
The actual by predicted plot shows how well it was fitted. The actual values form a scatter
of points around each mean curve. It shows the actual color values on the y-axis and the
predicted values on the x-axis. The points were randomly distributed along the diagonal
line with in 95% confidence limit region.
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As Appendix table 1.1 indicates that summary of fit for syrup was given by R2 and Adj R2
0.69460 and 0.52290 respectively. The R2 reports that 80% of the variation in the response
can be absorbed by fitting the model. One measure of goodness-of-fit is how well the points
lie along the 45 degree diagonal line.
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Design-Expert® Softw are Normal Plot of Residuals

Color
Color points by value of

Color: 99
14658
95
9772
90
Normal % Probability
80
70
50
30
20
10
5
-1860.32 -897.421 65.4747 1028.37 1991.27
Residual
Figure 4.2 The actual by predicted plot for color points
MSc Thesis Page 75

Figure 4.3 Response grid slider shows variation in color.
4.4 Turbidity of clarified syrup
It was observed that the minimum and the maximum turbidity values were 4669 IU and
11534 IU respectively. This wide range of responses indicated that the turbidity value was
significantly affected by the dosage of phosphate and flocculant. For example, the
combination 668 ppm phosphate with 12 ppm flocculant gave a turbidity value of 4669
where as that of 120 ppm phosphate and 12 ppm flocculant gave a turbidity of 11534 IU.
A quadratic model of turbidity was developed as shown below: Final equation in terms of
actual Factors.
Where T=Predicted turbidity, t=talod, p=phosphate values.
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As Appendix table 1.2 indicates that summary of fit for syrup turbidity was given by R2 and
Adj R2 0.57460 and 0.392290 respectively. The R2 reports that 70% of the variation in the
response can be absorbed by fitting the model. One measure of goodness-of-fit is how well
the points lie along the 45 degree diagonal line.
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Turbidity

Turbidity: 99
11534
95
4668
90
80
70
50
30
20
10
5
-3088.55 -1413.65 261.241 1936.14 3611.03
Residual
Figure 4.5 The actual by predicted plot for turbidity points.
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Figure 4.6 Response grid slider shows turbidity variation
4.5 Viscosity of clarified syrup
The minimum and the maximum viscosity values were 45 and 54 mpa.s respectively. This
wide range of responses indicated that the viscosity value was significantly affected by the
dosage of phosphate and flocculant. For example, the combination 668 ppm phosphate with
12 ppm flocculant gave a viscosity value of 45 where as that of 300 ppm phosphate and 8.5
ppm flocculant gave a viscosity result 54 mpa.s
The combined effect of phosphate and flocculant on the syrup viscosity was statistically
significant with p - value 0.0029 (Appendix). The Prob > F = 0.2567 in the Lack of Fit
(Appendix Table 1.3) suggested that the fitted model was adequate. On the other hand,
higher levels of both phosphate and flocculant led to a low viscosity value.
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A quadratic model of turbidity was developed as shown below: Final equation in terms of
actual Factors.
Where v=Predicted viscosity, t=talod, p=phosphate values.
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Visc. reduction

Visc. reduction: 99
55
95
45
90
80
70
50
30
20
10
5
-2.85355 -1.38572 0.0821068 1.54994 3.01777
Residual
Figure 4.8 The actual by predicted plot for viscosity points
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Figure 4.9 Response grid slider shows viscosity variation
4.6 Optimum point for combined color, turbidity and viscosity reduction
Optimization of Phosphate and the Talodura flocculant conditions is one of the most
important stages in the development of clarified syrup leads clarified of sugar. Response
surface methodology (RSM) is an effective optimization tool wherein many factors and
their interactions affecting the response can be identified with fewer experimental trials
than one factor at a time experiment.
Individual optimum region for each of the responses, turbidity, color, and reducing
viscosity was located earlier. This is because; turbidity, color, and viscosity are more
influential in indicating the syrup clarification efficiency than the rest. Turbidity removal is
considered as primary objective and turbidity measurement can be used with a high degree
of confidence to measure the efficiency of clarification (Mkhize, 2003). The location of the
best regions and the model developed for the individual parameters can be used to improve
problems faced with regard to each parameter.
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Design-Expert® Softw are
Desirability
1
0
0.940
X1 = A: A
X2 = B: B
0.705
Desirability
0.470
0.235
0.000
-1.00
-1.00 -0.50
-0.50 0.00
0.00
0.50 0.50 A: A
B: B 1.00 1.00
Figure 4.10 The desired point for optimum clarification
There is a need to superimpose the contour maps of the three responses in a single contour
plot. The process of finding a region in which the responses are superimposed to provide
the highest or lowest possible yield is known as optimization. The intersection point of two
or more optimal contour lines defines the coordinates of the optimum level for each factor
(Maximo, and Gacula, 1993). The following desirable ranges of responses need to be
fulfilled in order to locate the common optimum point in Figure 4.10.
Turbidity: low values of turbidity are desirable; hence, one should use contour lines with
predicted responses in the neighborhood of 4668 to obtain low turbidity value. The region
bounded by 4668 contour lines was selected as the optimum region for turbidity.
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Color: The low value of color was bounded by contour lines 9772. This region selected as
an optimum region for low color.
Viscosity reduction: The high value of Viscosity reduction was 45 and selected as an
optimum region for Viscosity reduction.
Figure 4.11 Superimposed contour plots for optimum point.
Therefore, using JMP optimization software, the optimum range for the three response
combination was determined by choosing the intersection range that satisfied the three
responses accordingly in the contour plotting graph. The mentioned three scenarios help to
generate a common optimum region. The region obtained by superimposing the above
response boundaries was depicted in the arrowed region of the superimposed contour map
(Figure 4.10).
Table 4.3 The optimum phosphate and talodura for syrup clarification.
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CHAPTER 5 CONCLUSIONS AND RECOMMENDATIONS
5.1 Conclusion
All Ethiopian sugar factories are practicing production of plantation white sugar (PWS) by
double sulphitation system. Sulfur dioxide (SO2) is toxic gas. When it is used during the
manufacture of any food product residual traces of sulfur remaining in such food product is
hazardous to human health. The other technology of clarification is Syrup clarification using
flotation process. The basis of this process is based on the Phosphoflotation and froth flotation,
conveniently termed as 'phosphoflotation' process applied in sugar refineries. Since the syrup
liquor is very viscous, at about 65ºBrix, clarification is done by flotation. The flotation system
uses chemicals like cationic flocculant (talodura) and phosphates to bring up impurities to
surface of the syrup clarifier. For this operation proportionating the dosages of these chemicals
is mandatory. By this research experiments; dosages of phosphate of 668ppm and 12ppm of
talodura was approved. It is excellent to operate this flotation system with these chemical
dosages for excellent clarity of sugar at Wonji Sugar Factory.
5.2 Recommendation
By the time this research was done Wonji Sugar Factory is using syrup sulfitation by
missing juice sulfitation because of the failures of the system. This makes high ICUMSA
values of color, turbidity and viscosity reduction on sample analyzed. Because of these high
values of sample analyzed; the high change done, up to 70% is still not low color syrup.
Secondly these experiments were done at the laboratory scale with laboratory materials and
it is recommended that these experiments should be repeated with syrup clarification set up
made for syrup clarification.
MSc Thesis Page 85

REFERENCES
Peter, R. (2007). Manufacturing and refining of raw cane sugar Miami, Florida, Elsevier
Scientific publishing company.
Broadhurst, S. (2002). Modeling adsorption of cane-sugar solution colorant in packed-bed

ion exchangers. Journal 49, 2519-2532
Bennet, M. (1977). Sugar Industry Technology. Journal 34, 22-32 in the Brich, G.G and
K.J
Biotech, K. (2010). Modified single sulfitation process for producing better quality
plantation white sugar. pp. 1717- 1725
Hugot E, (1986). Hand Book of Cane Sugar Engineering. Elsevier Scientific Publishing
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MSc Thesis Page 88

APPENDICES
Appendix A. Table of Least Squares fit to results of color, turbidity and

viscosity for clarified syrup
Appendix table 1. Model fitting to results of color for clarified syrup
Appendix Table 1.1 Summary fit for results of color for clarified syrup
RSquare 0.6900054
RSquare Adj 0.700081
Root Mean Square Error 155.1574
Mean of Response 794.6875
Observations (or Sum Wgts) 16
Appendix Table 1.2 ANOVA for results of color for clarified syrup
MSc Thesis Page 89

Appendix Table 1.3 Lack of fit for results of turbidity for clarified syrup
Residual 1.000E+006 5 0.0030 0.3367
Lack of Fit 1.111E+007 3 3.703E+006 99.66 < 0.0001 significant
Pure Error 2.601E+005 7 37153.14
Cor Total 3.604E+007 15
The Model F-value of implies the model is significant. There is only a 3.367% chance that
a "Model F-Value" this large could occur due to noise.
Appendix table 2. Model fitting to results of turbidity for clarified syrup
Appendix Table 2.1 Summary fit for results of turbidity for clarified syrup
RSquare 0.791305
MSc Thesis Page 90

Appendix Table 2.2 ANOVA for results of turbidity for clarified syrup
Sum of Mean F p
Source Squares df Square Value value Prob > F
Model 2.468E+007 5 4.935E+006 4.34 0.0232 significant
A-A 2.054E+00 1 2.054E+006 1.81 0.2086
B-B 3.985E+006 1 3.985E+006 3.51 0.0907
AB 30450.25 1 30450.25 0.027 0.8733
A2 9.629E+006 1 9.629E+006 8.47 0.0156
B2 8.978E+00 1 8.978E+006 7.90 0.0185
The Model F-value of 4.34 implies the model is significant. There is only a 2.32% chance
that a "Model F-Value" this large could occur due to noise.
Appendix Table 2.3 Lack of fit for results of turbidity for clarified syrup.
Residual 35.78 103.58 0.0022 0.5567
Lack of Fit 34.49 3 11.50 62.14 < 0.0001 significant
Pure Error 1.29 7 0.19
Cor Total 70.80 15
MSc Thesis Page 91

Appendix table 3. Model fitting to results of viscosity for clarified syrup
Appendix Table 3.1 Summary fit for results of viscosity for clarified syrup
RSquare 0.722075
Appendix Table 3.2 ANOVA results of viscosity for clarified syrup
MSc Thesis Page 92

Appendix Table 3.3 Lack of fit for results of viscosity for clarified syrup.
Residual 3.873E+007 10 3.873E+006 0.0029 0.2567
Lack of Fit 3.868E+007 3 1.289E+007 1859.65< 0.0001 significant
Pure Error 48537.50 7 6933.93
Cor Total 6.405E+007 15
Appendix B. figures
MSc Thesis Page 93

Appendix Figure 1. Prediction profile
MSc Thesis Page 94

Appendix Figure 2. Interaction profiles
MSc Thesis Page 95

Appendix C. photos
Appendix Photo 1. Cane loading in the field
Appendix Photo 2. Flotation system syrup clarification plant
MSc Thesis Page 96

Appendix Photo 3. Flotation system syrup clarification plant
Appendix Photo 4. Sample of the syrup taken from wonji factory
MSc Thesis Page 97

Appendix Photo 5. The talodura flocculant
Appendix Photo 6. The CaCO3 used to precipitate the phosphate
MSc Thesis Page 98

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ADDIS ABABA UNIVERSITY

SYRUP CLARIFICATION USING FLOTATION SYSTEM WITH

By: Kuma Nacho

hereby certify that it is worthy of acceptance.

Mr. Adamu Z. (Ass. prof)

Advisor Signature Date

Internal Examiner Signature Date

External Examiner Signature Date

Chair person Signature Date

MSc Thesis Page 1

MSc Thesis Page 2

TABLE OF CONTENTS ................................................................................................... 3

LIST OF TABLES .............................................................................................................. 7

LIST OF FIGURES ............................................................................................................ 8

LIST OF ACRONYMS……………………………………………………………... ..... 10

CHAPTER 1 INTRODUCTION ............................................................................... 14

1.1 Background of the study ...................................................................................... 14

1.3.2 Specific objectives ........................................................................................ 20

1.4 Significance of the Study ..................................................................................... 20

2.1 The Sugar Industry general overview .................................................................. 21

2.3.2 Chemical reactions of clarification ............................................................... 26

2.4 Syrup clarification using the floatation method ................................................... 27

2.4.2 Benefits of syrup clarification ....................................................................... 32

2.5 Principals involved in syrup clarification............................................................. 33

2.5.2 Effect of added chemicals ............................................................................. 36

2.5.3 Effect of aeration of syrup ............................................................................ 39

MSc Thesis Page 3

2.6 Harmful effects of SO2 consumption with sugar ................................................. 41

2.7.2 Carbonatation Process ................................................................................... 47

2.7.3 Coagulation and Flocculation ....................................................................... 49

2.8 Froth flotation fundamental principles ................................................................. 53

2.8.2 Hydrophobicity/hydrophilicity ..................................................................... 54

2.8.3 Particle/Bubble Contact ................................................................................ 56

2.8.4 Collection in the Froth Layer ........................................................................ 57

2.8.5 Reagents ........................................................................................................ 57

CHAPTER 3 MATERIALS AND METHODS ........................................................ 60

3.1 Site of the experiment .......................................................................................... 60

3.4.2 Turbidity ....................................................................................................... 63

3.4.3 The pH .......................................................................................................... 64

3.4.4 Sulphur Dioxide (SO2). ................................................................................. 64

3.4.5 Determination of Brix in syrup (dilution 1:3 m/m) ...................................... 65

3.4.6 Determination of Pol in Syrup Clarification ................................................. 65

3.4.7 Determination of Soluble Phosphate content ................................................ 66

3.5 Experimental Design ............................................................................................ 68

MSc Thesis Page 4

4.3 Color of clarified syrup ........................................................................................ 73

MSc Thesis Page 5

MSc Thesis Page 6

Table 3.3 Calibration of phosphate concentration against its optical density

MSc Thesis Page 7

Figure 1.2 Wonji syrup clarification plants.

Figure 2.1 Satellite image of wonji sugar factory.

Figure 2.2 Wonji shoa sugar factories.

Figure 2.3 Turbidity removals in syrup as a function of flocculent dosage.

Figure 2.4 Effect of temperature on turbidity removal.

Figure 2.6 DAF Process Schematic.

Figure 2.7 Mode of interaction of Talofloc with colorant.

Figure 2.8 Typical flotation vessels.

Figure 2.9 Diagram of flocculation

Figure 2.11 Selective attachment of air bubbles to hydrophobic particles.