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New Trends in the Clarification Process in the Sugar Industry

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 International Conference on: ‫א‬ ‫א‬:
The Arab Region and Africa in the World Sugar Context " ‫א‬ ‫א‬ ‫א‬ ‫"א‬
9-12 March 2003, Aswan, Egypt ‫א‬ ‫א‬ ٢٠٠٣ ١٢−٩

Assiut University STRI ISO

Technical Lecture No.: TL 2.1

New Trends in the Clarification Process in the Sugar Industry

Eng. A. A. Abara, Dr. Ali K. Abdel-Rahman, Prof. M. R. Bayoumi

Ph. D. Stud., Sugar Technology Research Institute, Assiut University, Assiut, Egypt
Assoc. Prof., Mech. Eng. Dep., Fac. of Eng., Assiut University, Assiut, Egypt
Prof., Mech. Eng. Dep., Fac. of Eng., and Dean of Sugar Technology Research
Institute, Assiut University, Assiut, Egypt

‫اﺗﺠﺎهﺎت ﺟﺪﻳﺪة ﻓﻲ ﻋﻤﻠﻴﺔ اﻟﺘﺮوﻳﻖ ﻓﻲ ﺻﻨﺎﻋﺔ اﻟﺴﻜﺮ‬

‫ ﻤﺤﻤﺩ ﺭﺠﺏ ﺒﻴﻭﻤﻲ‬/.‫ﺩ‬.‫ ﺃ‬، ‫ﻋﻠﻰ ﻜﺎﻤل ﻋﺒﺩ ﺍﻟﺭﺤﻤﻥ‬/.‫ ﺩ‬،‫ ﻋﺒﺩ ﺍﻟﻌﺯﻴﺯ ﻋﺒﺎﺭﺓ‬/.‫ﻡ‬
‫ﻤﻌﻬﺩ ﺩﺭﺍﺴﺎﺕ ﻭﺒﺤﻭﺙ ﺘﻜﻨﻭﻟﻭﺠﻴﺎ ﺼﻨﺎﻋﺔ ﺍﻟﺴﻜﺭ – ﺠﺎﻤﻌﺔ ﺃﺴﻴﻭﻁ – ﺃﺴﻴﻭﻁ – ﻤﺼﺭ‬
‫ ﺠﺎﻤﻌﺔ ﺃﺴﻴﻭﻁ – ﺃﺴﻴﻭﻁ – ﻤﺼﺭ‬-‫ﻜﻠﻴﺔ ﺍﻟﻬﻨﺩﺴﺔ‬-‫ ﻗﺴﻡ ﺍﻟﻬﻨﺩﺴﺔ ﺍﻟﻤﻴﻜﺎﻨﻴﻜﻴﺔ‬-‫ﺍﺴﺘﺎﺫ ﻤﺴﺎﻋﺩ‬
‫ﻜﻠﻴﺔ ﺍﻟﻬﻨﺩﺴﺔ ﻭﻋﻤﻴﺩ ﻤﻌﻬﺩ ﺩﺭﺍﺴﺎﺕ ﻭﺒﺤﻭﺙ ﺘﻜﻨﻭﻟﻭﺠﻴﺎ‬-‫ ﻗﺴﻡ ﺍﻟﻬﻨﺩﺴﺔ ﺍﻟﻤﻴﻜﺎﻨﻴﻜﻴﺔ‬-‫ﺍﺴﺘﺎﺫ‬
‫ﺼﻨﺎﻋﺔ ﺍﻟﺴﻜﺭ – ﺠﺎﻤﻌﺔ ﺃﺴﻴﻭﻁ – ﺃﺴﻴﻭﻁ – ﻤﺼﺭ‬
International Conference on: “ The Arab Region and Africa in the World Sugar Context “

New Trends in the Clarification Process

in the Sugar Industry

Eng. Abdul Aziz Abbara1, Dr. Ali K. Abdel-Rahman2,

Prof. Dr. Mohamed R. Bayoumi3
1
Ph.D. student (on leave) at Sugar Technology Research Institute, Instructor at
Department of Food Engineering, Al-Baath University, Homs, Syria.
2
Associate Professor at Mechanical Engineering Department, Assiut University.
3
Professor of Production Engineering and Mechanical Design, The Dean of Sugar
Technology Research Institute, Assiut University.

Abstract

One of the most factors that determine the sugar quality and
recovery in both cane and sugar manufacture is clarification process.
However, problems associated with clarification, the desire to upgrade
the quality of sugar, and production of new products like organic sugar
have always promoted the sugar technologists to explore new separation
process, which were commercially proven in other industries.
This paper reviews the current directions in clarification process
focusing on cross flow membrane filtration which seems the key process
for replacing the conventional carbonation process and to produce refined
sugar directly from raw cane juice.
Keywords: Clarification, Beet, Cane, Crossflow membrane, Fouling.

Introduction

Diffusion beet juice or raw cane juice contains beside sucrose more
than 50 nonsugar impurities, like reducing sugars organic acids and non-
organic acid, amino acids, proteins, starches, waxes, gums, minerals
(such as potassium, magnesium, calcium, silica), coloring matters, and
other suspended matters (Gil and Wright 1994), that cause dark color and
high turbidity to the juice (Gil and Wright 1994, Verma et al. 1996).
Table I shows a typical analysis of the Southern Idaho of Beet diffusion
juice (Kochergin 2002).

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Table I A typical analysis of the Southern

Idahoof beet diffusion juice
(Source Kochergin 2000).
Concentration Molecular
Component % on non-
% on DS weight
sugar
Sucrose 87.75 N/a 342
Invert sugars 1.03 8.59 180
Raffinose 0.42 3.50 595
Betaine 0.31 2.58 117
Citric acid 0.73 6.09 210
Malic acid 0.36 3.00 134
Lactic acid 0.12 1.00 91
Acetic acid 0.25 2.08 60
Oxalic acid 0.29 2.38 126
Other organic acids 0.20 1.67 -
Calcium, magnesium*** 0.35 2.92 24-41
Sodium, potassium 2.01 16.76 23-40
Inorganic anions (chloride,
2.97 24.76 <100
sulphate, nitrate, etc.)
Proteins ** - 15,000-100,000
Colorants ** - 10,000-1,000,000
Dextrans 0.3 2.50 50,000-2,000,000
Pectins ** - 20,000-400,000
Glutamine* 0.7 5.84 146
Other amino acids* 0.7 5.84 100-300
Un accounted non-sugars 1.26 10.50 -
Total non-sucrose 12.00 100.00 -
Total solids 100.00 -
*Concentration of glutamine and amino acids calculated based on
molasses content of about 9% on non-sugars.
**Information was not available
***Calcium and magnesium are calculated based on hardness level of
12meq/100 DS.

Separation of these impurities from the juice as early as possible

should be done by clarification to avoid the problems of increasing color,
sucrose inversion, high viscosity, and the generation of excess molasses
(Gil and Wright 1994). The quality of the product mainly depends on the
efficiency of clarification (Xian et al. 1998).

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Because conventional clarification methods need heavy equipment

and represent high operating costs, in addition create environmental
problems (Lancrenon et al. 1993), the sugar industry has contemplated
the possible use of advanced technologies which were proven in other
industries.
Membrane separation is one of such technologies that will compete
favorably for reducing energy usage, reducing, or elimination of chemical
clarification and improved final product quality. Another promising area
of application is in production of new products, such as organic sugars
(Godshall et al. 1999).
Today most membrane filtration systems use cross-flow (or
tangential flow) filtration, where the feed stream flows across the
membrane rather than through it. This helps to prevent clogging of the
membrane by retained particles (Steindl and Doyle 1999, Saska 2000).
The solution passing through the membrane, containing solvent and
solutes not retained by the membrane is called permeate while the
solution containing the retained (rejected) species called retentate reject
stream, or concentrate.
Based on the size (or molecular weight) of the targeted particles,
membranes used in filtration are usually classified as reverse osmosis
(RO), nanofiltration (NF), ultrafiltration (UF), or microfiltration (MF)
filters (Saska 2000). The properties of each type and the range of
impurities that can be separated are shown in table II.

Table II Characteristics of the different type of pressure -driven

membranes (Source: Steindl and Doyle 1999, Saska 2000)
MF UF NF RO
Pore size 0.05-10 µm 2,000 Ao 10-80 Ao <10 Ao
Larger Than 20,000- Smaller than
MWCO* 200-20,000
400,000 400,000 200
Operating
Pressure Up to 3 7 20 20-100
(bar)
Colloidal Divalent
Particulate Allow only
matter- ions- organic
Reject matter, water to pass
macromolec solutes(sugar
suspension through
ues s)
Molecular weight cut-off: the molecular mass of standard molecules (blue
dextran) with 90 to 95% retention by membrane (Decloux et al 2000).

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The favored configurations for sugar industry applications include

tubular for the ceramic, carbon and stainless steel membranes, spiral
wound and hollow fiber for the polymeric membranes (Saska 1997,
Steindl and Doyle 1999). (See Figure 1)
Spiral
Wound

Tubular

Hollow
Fiber

Figure 1 Different membrane configurations for sugar industry

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In spite, investigations to study the possibilities of application

membrane to the sugar industry were made by Danico a/s in the late
1960’s(Madsen 1990), A few industrial installations both in cane and beet
factories are now in service. Among of them the New Applexion Process
(NAP) at Puunene factory in Hawaii.
In the following paragraphs, the importance of new process to the
sugar industry will be presented as well as the factors affecting the
performance of membrane separation will be discussed.

New separation process (NSP), why?

Beet Sugar Industry
Figure 2 represents a simplifies scheme of sugar production, with
indicated black points of possible application of membrane filtration
(Hinkova et al. 2002).

Figure 2 Simplified scheme of sugar production with indicated Spots of potential

applications of membrane separation process
( Source: Hinkova 2002)

Raw juice purification

Clarification of the raw beet juice using carbonation process is used
by all sugar factories worldwide with many modifications (Kochergin
2002).
The following steps are usually used for clarification the diffusion juice:
• Preliming the diffusion juice with milk of lime and calcium
carbonate so that a "prelimed juice " is prepared;

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• Subjecting the prelimed juice to main liming in which substantial

amounts of milk of lime are used to generate a "treated juice ";
• Carbonating the treated juice in a first carbonation stage with CO2
gas;
• Allowing the treated juice to settle (in most cases); and
• Carbonating the treated juice product in a second carbonation stage
with CO2 gas to create a thin juice product which (after additional
filtering and SO2 (treatment if needed) is ready for evaporation
(Ekern et al. 1998).
Notwithstanding the foregoing process is efficient to manufacture a
final sugar from raw beets, it nonetheless creates significant problems in
respect of energy, raw material consumption (Ekern et al. 1998,
Mantovani and Vaccari 2001) and water consumption, as well as
handling and disposal of carbonatation sludge. (Mantovani and Vaccari
2001).
Specifically, the CaO consumption of lime varies between 1 and
3% on beet (Schiweck 1998) and there is not much scope to reduce usage
below about 1% CaO (Tebble 2000). This means that a sugar factory
processing 10,000 tonnes beet/day discharges, on average, about 1,000
tonnes waste lime per day (Mantovani and Vaccari 2001). Moreover,
Lime is initially produced using a high-temperature calcination process,
which takes place in a lime kiln. To produce lime within the kiln,
limestone (calcium carbonate) is heated to a temperature of about 980-
1200 oC for about 30-120 minutes. In this regard, the calcination process
is energy intensive (Ekern et al. 1998).
Consequently, several processes using crossflow microfiltration or
ultrafiltration have been proposed by different researchers as potential
routes to reduce or eliminate the use of lime in the beet sugar factory
(Vaccari et al. 1997, Gilles 2002, Hinkova et al. 2002, Tebble 2002) (See
item 2 Figure 2).
In parallel with membrane investigation Amalgamates Sugar has
developed and patented a process for purification of diffusion juice based
upon softening and chromatographic separation technology (Kearny and
Rearick 1996).
The benefits of using membrane filtration which could eliminate
the traditional carbonation process, are summarized as follows:
• Elimination of the carbonatation sludges
• Reduction of the waste waters
• Decrease in energy consumption

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• Reduction of carbon dioxide emission

• Plants simplification
• Problems arising from beet technological quality (Vaccari et al.
1997)
• Retentate after sweetening-off, could be incorporated directly in
the pulp or sold separately on the market as a nitrogen-rich
compound (Lancrenon 1993).
• Reduction of sugar end handling (Kearny and Rearick 1996).

Clarification of press water

Another encouraging route to improve the quality of diffusion
juice, which will be reflected on clarification, is to apply membrane
filtration for clarification of press water (see point 3 in Figure 4).
Press water is a very dilute stream containing about 3-4% of total
sugar entering he factory. It is recycled back to a diffusion stage after
pulp presses. Membrane filtration can be applied for both press water
sterilization and suspended solids removal (Kochergin 1998,2002).
Figure 3 represents a flow diagram of press water treatment with
RO or NF (Hinkova et al. 2002).

Extracted pulps
Pressing Pressed Pulp
Press water Retenate to Low Grade
Sugar Crystallization
Purification RO RO
Permeate to Diffuser

RNF RNF to Low Grade

Sugar Crystallization
RRO
RRO to Waste
NF RO
Permeate to Diffuser

Figure 3. Schematic of press water treatment with

RO/NF ( Source: Hinkova et al. 2002).

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Thin juice concentration

It was reported that approximately 50% of the energy utilized to
produce beet and cane sugar is consumed during the evaporation of water.
That is why the highest potential for energy reduction is concentration of
clarified thin juice from 12 to 14% of refractometric dry substance (RDS)
to a maximum of 30% RDS while osmotic pressure is already about 3.5
MPa (See item 1 in the figure 4).
However, many problems associated with thermal creep within the
membrane modules must be further solved. Moreover, higher osmotic
pressure of concentrated thin juice needs higher energy inputs, what
impedes an easy industrial application (Hinkova et al. 2002).
Madsen (1990) has carried out pilot tests on nanofiltration of thin
juice. The tests showed that it is possible to concentrate thin juice from
approximately 14% sucrose content to 17-19% sucrose content with an
average approximately 30 l/(m2.h) at a filtration pressure of 40 bar. The
permeate has a sugar content of less than 0.5 %, and the purity of the
permeate is approximately 60%. The best operating temperature is in the
region of 70 oC. During one campaign, the plant was operated at a
temperature just above 80 oC. The membrane life under these conditions
was only about 50 days. The juice before membrane filtration has to be
softened by ion- exchange because otherwise rapid membrane fouling
occurs. Operating at 70 oC gave bacteriological problems if a disinfectant
was not added regularly.

Cane Sugar Industry

In recent years the market requirements demand production of
higher quality raw sugar for export and good quality refined or semi-
refined for direct consumption that the traditional mill white or plantation
white could not attain. Consequently, production processes have
developed to meet these requirements using two main routes. One method
is to attach a refinery to a group of existing raw sugar factories and make
use of the supply of cheap energy during the crop season by burning
bagasse. The second route has been the adoption of direct white processes
by cane sugar factories, such as the TALO system developed and
marketed by Tate & Lyle. The current interest in membrane processes
indicates their considerable potential for the future production of white
sugar (Editorial staff 1997).
Figure 4 represents the possible application of membrane as an
innovative technology in white sugar manufacture.

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Cane

Milling

Raw Juice
1
Mixed Juice
Lime RVF
Clarification
SO 2 Scum
3
2 Clear Juice

Evaporation

Syrup
4
SO 2

Crystallization
Molasses

White Sugar

Figure 4. Flow-sheet of membrane applications

in white sugar manufacture

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Clarification of raw juice

Simple defecation of raw cane juice is generally sufficient for
producing raw sugar. No additional decolorization is normally necessary,
the remaining purification needed for raw sugar production being taken
care of by the final crystallization process (Trott 1988). However, The
production of mill white sugar for direct consumption requires
sulphitation clarification process using milk of lime and SO2 gas (Trott
1988, Chen 1993, Doherty and Edye 1999).
Investigation over the past three decades have demonstrated that
ultrafiltration is a promising option for the clarification of raw cane sugar
juice (Balakrishnan et al. 2000).
Replacing sulphitation process with microfiltration or ultrafiltration
would lead to reduce substantially or even eliminate the use of lime and
SO2 gas which cause heavy corrosion and hard scaling in the heat
exchangers (Shrivastva 1998). What’s more, the reduction of SO2
consumption at this stage could significantly lower the sulphur content in
the white sugar (20-100 ppm), so that it meets the FDA requirement of
less than 10 ppm (Chou et al. 2000).
Rotary Vacuum filtrate (RVF)
In conventional clarification process in cane mills, the mud result
from clarifier is sent to rotary vacuum filters for sugar recovery. Filtrates
from the filtration station are very dirty with an apparent purity some 1-5
percent lower than clarified juice and under some circumstances this
purity drop can increase to much higher values so that it is difficult to
sent these filtrates straight to the evaporator station (Trott 1988).
Therefore, filtrates are returned to the mixed juice tank and recirculated
through the mainstream clarification system.
Recycling the filtrates from rotary vacuum filters has many
disadvantages like:
It makes the operation of the filters directly affects the performance
of the clarifier i.e. the mud solids output at the filters must match the mud
solids rate entering the factory in mixed juice. If this basic requirement is
not satisfied then mud will accumulate in the clarifier. During periods of
high mud loadings, the buffer capacity available in the clarifier for
variations in mud volume is usually very limited.
The other problem of filter operations that affects significantly on
the clarifier is the retention of mud solids in the filter cake and the
amount of mud being recycled with filtrate. The returned mud will exceed
the mud loading problems at the clarifier, particularly during periods of
high incoming mud solids loadings (Steindl 1998).

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Another disadvantage of recycling filtrates appears from the fact

that these filtrates contain the microbiological degradation products of
sugar decomposition, and all of these extremely harmful impurities are
normally returned to the mixed juice tank, where they are recycled
through juice liming, juice heating, and juice clarification and this results
in additional color generation and sucrose inversion. (Bennett, Trott
1988)
To overcome these problems, and for production of white sugar a
separate flotation clarification system is used (Trott 1988, Chen 1993).
As an alternative to flotation process, Balakrishnan et al. (2000)
used ultrafiltration to clarify the RVF (See point 3 at figure 4). The
average purity rise was over 3 units with sugar rejection below 5% and
permeate could directly send to the evaporators.
The benefit of clarification filtrate may be summarized as follows:
eliminating the recycling of impurities through juice clarification station
have a dramatic effect on clarified juice and hence thick syrup quality.
Besides this highly beneficial effect on purity, the process would save
energy and chemicals at the clarification station as well as increases the
capacity of the juice clarifier station by the proportion of RVF filtrate.

Clarification of clear juice

The clarified juice obtained from clarification process still contains
bacterial remnants as well as macromolecular impurities like starch,
dextran, fat, waxes and coloring compound in colloidal form (Cartiier et
al 1996, Balakrishnan 2000).
Cartier et al (1996) indicated that the successive combination of
both classical clarification and ultrafiltration (Point 2 at figure 4) results
in a very high quality cane juice as illustrated in table III.

Table III. Typical analytical results from ultrafiltration of clarified

juice on Techsep mineral membranes
Brix Purity Color Turbidity
(% dry (%) (ICUMSA) (ICUMSA)
matter)
Clarified juice 16.7 83.3 11350 2470
Ultrafiltered juice 16.9 84.0 9650 170
Balakrishnan (2000) summarize the benefit of using ultrafiltration
at different stage of the conventional sulphitation clarification process in
table IV.

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Table IV. Impact of ultrafiltration at different stages in clarification

using sulphitation (Balakrishnan 2000)
Mixed/raw Clarified
Parameter RVF
juice juice
Sugar Recovery Substantial Marginal Intermediate
Sugar quality Substantial Marginal Substantial
Lime consumption Substantial Intermediate None
SO2 Consumption
Substantial Intermediate None
(Clarification stage)
Chemicals for
Substantial Marginal Substantial
evaporator cleaning

Clarification of syrup
During the evaporation of the clarified juice to the syrup, a
considerable quantity of non-sugars that were soluble in the clarified juice
became insoluble in the syrup due to the loss of 80 percent juice original
water content. For this reason, evaporator syrup is usually almost opaque.
These impurities have an adverse effect on the crystallization and curing
of the massecuite for the following reasons:
• During pan boiling a large part of these insoluble impurities are
inevitably occluded within the various layers of the forming
crystals and carried with them the high colored mother liquor of
decreasing purity (Suzor 1979, Rein et al. 1986, Bennett).
• The relatively high density of these impurities has an adverse effect
on the viscosity of massecuite during pan boiling and separation of
mother liquor from the crystal wall in the centrifugal is impeded
(Bennett). During purging, the portion of these insoluble non-
sugars that were not included in the crystal causes blockages of the
channels existing between the crystals through which the mother
liquor is supposed to be forced out. This results in more high
colored molasses being retained with the sugar further yielding a
poor quality sugar (Suzor 1979).
Phhosflotation is used for clarifying syrup as in blanco directo
process (trott 1988, Chou 1993). However, the large calcium phosphate
precipitates are friable and cannot be subjected to intensive aeration
which can only be obtained by violent mechanical means, if subject to
intensive aeration, a large portion of these precipitates are eroded and
again somehow defeat the initial intent of their optimum utilization
(Suzor 1979). Moreso indicated that, it is impossible to ensure a complete
interreaction between the various reagents in the sugar solution, therefore

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a portion of these reagents remains in solution in the syrup, increasing the

non-sugar concentration of the latter which result in lesser sugar recovery
by crystallization due to the increase in sucrose solubility by the presence
of these added non-sugars.
Saska (2000) discovered that nanofiltration of syrup through a
membrane with pore size on the order of 20 to 50 .ANG. not only
decolorizes the solution, but also produces a permeate having enhanced
crystallization properties. The feed can have a color as high as about
25,000 IU. The decolorized permeate can have a color as high as about
3,000, and even at this high level of color may be used for the direct
crystallization of white sugar without further processing. No intermediate
crystallization of a raw sugar is needed. syrup should be clarified to
remove polysaccharides and colloids to give a solution with a turbidity
below 1 NTU/Brix. A preferred method of clarification is to initially
clarify juice through conventional means (e.g., liming and settling),
followed by ultrafiltration of the clarified juice through a ceramic or
polymeric filter having a pore size between about 0.01 and about 0.2
micron, i.e., having an approximate molecular weight cut-off in the range
from about 20,000 to about 500,000 (Saska 2000).
Chromatographic separation using coupled loop process were
applied to clarify syrup (Kochergin et al. 2000). Sugar recovery in the
chromatographic process exceeds 99%. The low color, ash and reducing
sugar content of the extract leads to direct production of white sugar.
However, the following conditions should be taken into
consideration when applying chromatographic separation (Paillat and
Cotillon 2000):
• The products coming into the separator must be free of any
suspended solids.
• The separation medium must remain in the initial ionic form,
which has been selected for optimum separation
• It is necessary to remove the divalent cations before separation.

Raw Sugar Refining

Clarifying of sugar melt
Raw sugar is coated with a film of molasses from which the sugar
was crystallized. It contains a number of undesirable nonsugar
constituents such as cane fiber, numerous forms of insect life,
accumulation of many kinds and frequently microorganisms, some of
which are harmful, and cause it to be unacceptable as a foodstuff for
human consumption (Hugill 1979). Raw sugar has a color in the range of

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1,000 to 5,000 IU. The conversion of raw sugar into refined sugar as
required by the food-processing industry and the domestic consumer,
either in crystalline form or as in an aqueous solution (liquid sugar) is
accomplished in a series of complementary unit processes as follows:
The raw sugar is washed or affined; "melted" (i.e., dissolved in hot
water); and then clarified to remove polysaccharides and colloids.
Conventional clarification is usually performed by liming, carbonatation,
or phosphatation. The clarified syrup is decolorized, typically by
adsorption of impurities onto activated carbon, charcoal, or ion exchange
resins. A conventionally decolorized syrup should have no more than 800
IU color for successful refining to white sugar having a color below 25
IU; for some uses, a color as high as 50 IU can be acceptable (Saska
2000). The fine liquor is then crystallized to yield refined sugar. The
degree of refinement depends on the number, and effectiveness, of the
flocculation and decolorization steps (Gudnason and Stell, 1981).
Researches were performed to replace both the affination and
clarification process by a single crossflow ultrafiltration (Lancrenon
1993) or microfiltration (Dornier et al. 1995). This would simplify the
process, as shown in figure 5, eliminate the pollution problem and
produce of a retentate, which can be easily blended with final molasses of
the refinery (Lancrenon et al 1998).

Decolorization using ion exchange with brine recovery

The ion exchange resin process is considered as on of the most
efficient method for decolorization sugar liquor. However, effluents
resulting from alkaline brine regeneration create some disposal problems.
This is due to the regeneration effluent contains a high concentration of
sodium chloride and colored organics (Carteir 1996).
To overcome these problems, Applexion developed a method for
brine recovery using low cost spiral membrane. The color is concentrated
in small volume of retentate, while in the permeate the main part of the
salt is recovered, re-usable for a further resin regeneration (Theoleyre
1999).

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Figure 5. Comparison between the conventional and the suggested process of

raw cane sugar refining (Dornier et al. 1995)

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Factors affecting membrane separation process

Permeability and selectivity

Efficiency of membrane can be described by membrane
permeability and selectivity. These characteristics are typically measured
by permeate flux and rejection respectively. Permeate flux is the mass or
volume flow of solution through the membrane per membrane area (Net
site (a)). It can be expressed by the following equation given by (Hagen
Poiseuille equation) (Casani and Jørgensen 2000)
TMP
Jm = (1)
µ ∗ Rtot
Where:
TMP transmembrane hydrostatic pressure difference (Pa)
µ the Viscosity (kg/m s)
Rtot the total resistance of the membrane (m)
The selectivity of a membrane is described by rejection. Rejection
of totally selective membrane is 1 or 100%. Typically, rejection is
between 0.7-0.99. The rejection of the membrane is expressed by (Net
site (b)):
Cp
R = 1− (2)
Cr
Where: Cp Solute concentration in permeate (kg/m3)
Cr Solute concentration in retentate (kg/m3)
To make the raw sugar clarification by microfiltration or
ultrafiltration viable, the rejection of sugar should be as less as possible
while the rejection of other solids should be high enough so that the
permeate stream is rich in sugars only (Bhattacharya et al 2001).
Permeate flux and rejections are dependent on the following
variables: pressure, concentration of solute, temperature and flow velocity
of membrane (Niemi and Palosaari 1993).
Osmotic pressure
The specific flux can be calculated according to the equation (3)
J = L p ( TMP − ∆Π ) (3)
where: Lp Pure water permeability (m/(Pa s))
∆∏ Osmotic pressure difference (Pa)
This model regards the specific flux as a consequence of the
increased osmotic pressure produced by the high concentration of the

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rejected solute near the membrane surface, taking into account that the
concentration of rejected solute increases with applied pressure [Paris et
al. 2002).
Osmotic pressure of sucrose with concentration can be related by
the following expression:
Π = 3.77 × 10 3 C + 38.79 C 2 − 0.04 C 3 (4)
3
Where ∏ is in Pa and C in Kg/m . (Bhattacharya et al. 2001)
It is appear From Eq (4) that the concentration of sugar solutions
increases the osmotic pressure increases. In addition, sugar solutions at
high concentration exhibit high viscosity. Therefore, It seems that
membrane filtration are limited more or less by dilute streams.
Concentration polarization
In microfiltration crossflow membrane filtration, suspended
particles are transported to the membrane surface by the permeate flow
and form a concentration polarization (CP) layer. As particle
accumulation continues, particle concentration near the membrane
surface reaches its maximum value and a particle cake layer forms
between the membrane surface and the CP layer. Further transport of
particles to the membrane surface results in the growth of the cake layer
until a steady state is attained. At steady state, as shown in figure 6, the
convective flux of particles carried toward the membrane with permeate
is balanced by back-diffusion away from the membrane (Hong et al.
1997)

Figure 6. Schematic representation of a crossflow membrane filtration

channel of length L depicting a steady state concentration
polarization (CP) layer on the membrane surface
( Source: Bhattacharjee et al. 1999)

Once the working pressure and the feed flow have been fixed,
according to the gel- polarization model, the specific flow of filtrate (J) is
a function of the solids concentration in the feed stream (Cb). Both

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variables are related through the mass transfer constant of the system (k),
according to the following equation (Palacios et al. 2002):
Cg
J = KLn (5)
Cb
Where: J Specific flow (m/s)
K Mass transfer coefficient (m/s)
Cg Concentration in the gel layer (kg/m3)
As shown in Eq. (5), if the solids concentration in the feed stream is
higher than the Cg value, there is a certain filtrate flow, but if solids in the
feed streams are more concentrated than this value, there will be no
effective filtration.
Fortunately, the action of the bulk layer of suspension tangent to
the membrane surface limits the accumulation of the immobile cake layer
(Davis and Sherwood 1990).
Nevertheless, The external cake of rejected particles may also act
as a secondary or dynamic membrane, which screens the primary
membrane from the more strongly fouling species of smaller size. The
large particles form an external cake on the surface of the primary
membrane, which then acts as a deep-bed filter and captures some of the
small particles and prevents them from fouling the primary membrane.
[Vinod T. Kuberkar et al]. Kochergin (1997) conducted experiments with
MF and UF membranes with pore size ranging from 200,000 MWCO to
0.2 µm and results showed insignificant differences in dextran and color
rejection. These confirm the idea that a secondary dynamic membrane is
responsible for the observed separation characteristics.

Fouling
Membrane fouling is a very complicated phenomenon caused by
many chemical and physical factors. According to Huang and Morrissey
(1998) the membrane fouling is a dynamic process starting with pore
blocking at the initial stage of filtration, and followed by a continuous
cake layer formation.
Balakrishnan et al. (2000) considered that fine bagacillo particles
found in all the feed, except for clear juice, have a tendency to settle
down on the membrane surface during UF thus creating a secondary
filtration layer that results in a drop of flux.
According to Vercellotti et al. (1998) the component of sugarcane
syrup that foul ultrafiltration membrane are dextrans, starch, cell wall

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polysaccharides (soluble hemicellulose), high molecular weight colorant,

and possible complexes of polysaccharide and colorant.
Successful operation of membrane plant requires careful
management of fouling of the membrane; its avoidance is probably not
possible, but its impact can be limited by a variety of techniques
(Wakeman and Williams 2002). The choice of membrane, module,
process configuration and pre- treatment are all important to varying
extents if a high degree of separation is to be achieved without
productivity being lessened unacceptably by fouling [Net site (a),
Balakrishnan et al 2000, Wakeman and Williams 2002).
Table V explains the methods of reducing fouling for an installed plant.
Table V Methods for reduction of flux degradation
( Source:Wakeman and Williams 2002).

Physical Chemical
Pretreatme Prefiltration, Precipitation, Coagulation/
nt flocculation, Use of
disinfectants, Use of
antiscalants, Adsorption

Design Use of turbulence promoters, Choice of membrane

Pulsed/ reversed flow, material, Membrane surface
Rotating/vibrating modification
membranes, Additional (e. g.
electrical) fields
Operation Limit transmembrane Choice of cleaning
pressure (i. e. production chemicals, Frequency of
rate), Maintain a high cleaning
crossflow, Periodic hydraulic
cleaning, Periodic
mechanical cleaning

Physical Pretreatment
Different physical separation processes were proposed to treat the
sugar solutions before subsequent membrane filtration.
Donovan et al. 2002 pointed out that removing at least 90% by
weight of all fibers and silt ,having a largest dimension of about 50 µm,
from the diffusion beet juice is necessary for minimizing the fouling of
membrane. This can be done by screening and/or filtration through filter
or screen has a mesh size of about 30-100 microns. Nevertheless,

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Prefiltration of the raw juice with sieve up to 150 mesh was not
successful in eliminating the bagacillo [Balakrishnan et al 2000].
Vercellotti et al. (1998) used Alfa Laval lab disk-stack centrifuge
with maximum flow rate 6 gallons per minute at 8000 x g and 200 oC for
clarifying the clear juice before membrane filtration through a ceramic
type filter of 0.2 µm average pore size. Tests should, (Table VI), that
centrifugation of clarified cane juice improved flux rate by 80% to 100%
above that of untreated clarified juice. Hence, cycle times for membranes,
between cleaning, should be approximately doubled.

Table VI. Test of UF membrane with disk-stack treated clarified

juice (Source: Vercellotti et al 1998)

Sample Normalized flow rate

Untreated clarified juice 1.00
Juice treated at 0.5 gallon/min 2.32
Juice treated at 1.0 gallon/min 1.66

Chemical pretreatment.
Vaccari et al. (1997) proposed pre- filteration of raw beet juice,
after being heated at 75-90° C and after pH-stabilisation , in order to
eliminate the organic and mineral particles whose size is above 50-100
micron that cause fouling. It may also, be settled, with or without using
coalescents.
Another method, which includes thermal and acidic treatment of
raw beet juice followed by electrochemical treatment before ultrafiltration
was developed by Shimanskaya et al. (2000) to overcome the problem
associated with direct ultrafiltration of beet raw juice represented by the
low flux of ultrafiltration conditioned by diffusion juice that is rich in
high- molecular components.
Donovan et al. (2002) suggested introducing air into the feed juice
before the first ultrafiltration, in order to oxidize color-forming materials.
This oxidation, while increasing the color of the juice, (e.g., resulting in a
color increase from 8,000 to 16,000) causes the color-forming materials
to polymerize, which facilitates their removal in the subsequent
ultrafiltration. Another option is to introduce hydrogen peroxide, ozone,
or both, into the feed juice prior to the first ultrafiltration. These materials
also facilitate oxidation. It is preferred to adjust the pH of the feed juice

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to about 6-8, for example by the addition of a base, prior to ultrafiltration

more preferably 6.5-7.5. This can help minimize formation of invert.

Operation
Hanssens et al. (1984) considered that the greatest problem in
ultrafiltration was fouling of membranes and using tubular membranes at
high Reynolds numbers could reduce this problem. He ultrafiltered the
raw beet juice with tubular membranes and found that raw juice treated
by ultrafiltration gave a thin juice similar in quality to that by the
conventional method but that further treatment with 0.05% lime on beet,
electrodialysis or ion exchange might be necessary to remove some of the
remaining impurities. At a linear velocity of 4m/sec there was no fouling
problem and no need for pretreatment. Electricity consumption accounts
for 40% of the treatment costs. Fouling membrane were cleaned
effectively with 1500 mg/l hypochlorite solution containing 1500 mg/l
active chlorine while in some cases proteinase-containing detergent in
combination with the chlorine solution were used for cleaning heavily
fouled membranes.
Almost all pressure driven membrane modules operate in cross
flow mode, in which the feed is pumped across (tangentially) the
membrane surface. This mode of operation is advantageous because it
limits the build up of solids or solutes at the membrane surface. A higher
flow rate tends to remove the deposited material and, consequently,
reduces the hydraulic resistance through the membrane and the obtained
permeate flux will be higher (Casani and Jørgensen 2000). These
advantageous obtained at an energy cost. The pumping energy is required
in order to remove the slurry tangentially to the filter medium must be
supplied in addition to the energy required to supply the transmembrane
pressure for filtration (Perry and Green 1984).

Process conditions
Many studies have demonstrated that the operating conditions
modify the selectivity of membrane [Decloux et al 2000]
The permeate flux increases with the TMP (Eq (1)) but the relation
between them is only linear when the feed is pure water. If the feed is
another product, the flux becomes independent of the pressure and mass
transfer controlled when the pressure increases above the level, where the
concentration polarization layer reaches a limiting concentration (see
Figure 7) (Casani and Jørgensen 2000)

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Figure 7. Generalised correlation between operating parameters and flux,

indicating the areas of pressure control and mass transfer control (Source:
Casani and Jørgensen 2000)

Regarding of the rejection of solute (both total dissolved solids and

sugars), it increases with pressure for a fixed feed Brix. At higher
pressure, the polarization layer becomes more compact. This reduces the
permeability of this layer and consequently, the solutes are retained more
and therefore, the retention of total solids and sugars increase with the
operating pressure (Bhattacharya et al. 2001).

MWCO M1=10000
MWCO M2=15000
MWCO M3=20000

Figure 8. Variation of percent recovery of sugars vs. pressure for

different membranes at 10 Brix of clear limed cane juice
( Source: Bhattacharya et al. 2001).

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Increasing temperature should result in higher flux but could also

result in a decrease in flux for certain feeds. However, the beneficial
effects (lower viscosity, higher diffusivity) will outweigh the harmful
effects like loss of solubility of salts or denaturation of proteins or
gelatinisation of starch and may result in a net increase in flux (Casani
and Jørgensen 2000). However, to prevent the bacterial infection the
temperature should be at least 80 oC.

Membrane Operation
A membrane system may either be operated in batch mode, where
some or all of the retentate is returned to the feed tank, and the processing
is stopped when the feed tank level or the filtration flow rate reaches a
preset limit; or the system may be operated in a multi-stage design, where
within each stage a portion of the retentate is recirculated to provide the
required cross-flow velocity on the retentate side of the membrane. A
multi-stage mode with three or four stages would be preferred for
industrial operations (Monclin 1995).
Diafiltration, which is a special case of a batch mode, refers to
dilution of the concentrate by solvent (water) and continuation of
ultrafiltration until satisfactory removal of the permeable species is
reached. The dilute may be added continuously to make up the volume
lost through permeation or discontinuously by diluting back the
concentration obtained after a batch ultrafiltration operation (Net site (a)).

Notices on Performance of Membrane Filtration of Sugar Juices

It is clear from table 1 that the distribution of the component by

molecular weight of a typical beet diffusion juice is bimodal. . A group of
components with molecular weight exceeding 500,000 Da includes
suspended solids and colloidal materials as well as high molecular weight
dextrans, starch, etc. Over 90% of dissolved solids have molecular weight
ranging between 100 and 600 Da (Kochergin et al. 2002). Therefore, it
may be concluded that microfiltration or ultrafiltration may be feasible
for the removal of suspended solids, colloidal material and other high
molecular weight compounds, but they perform poorly for separation of
most of the dissolved non-sugar components.
The expected purity change across MF or UF membrane should not
exceed more than one purity point, corresponding to 10% elimination of
non-sugars at juice purity of 88 (Kochergin 2002). This observation will
be valid for raw cane juice also.

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Nevertheless, It is necessary to clarify permeate, resulted from MF

or UF of raw juice, in order to de-ash the clarified juice before
evaporation. This would aid in controlling the evaporator fouling. Thus, it
would mean less frequent shut downs for cleaning and reduced
consumption of cleaning chemicals (Balakrishnan and Ghosh 2000).
Different separation methods were proposed such as
electrodialysis, ion exchange (cartier et al. 1998, Donovan et al 2002),
nanofiltration, reverse osmosis (Balakrishnan and Ghosh 2000, Saska
2000, Donovan et al 2002), chromatographic separation (Donovan et al
2002), and cooling crystallization (vaccari et al. 1997). While, Duffaut
and Godshall (2002) describes combining ultrafiltration and hydrogen
peroxide treatment of clarified cane juice to produce a high quality, low
color juice suitable for producing direct consumption sugar or very high
purity raw sugar requiring a minimum of refining. The process exploits
the strengths of two existing systems: ultra filtration to remove turbidity
and macromolecules and hydrogen peroxide to reduce color.
It is also important to analyze the influence of membrane filtration
on the sugar end operation and properties of product sugar.
Cartier et al. (1996) indicated that the color and the turbidity of
sugar resulted from UF of clear cane juice decrease on average by 53%
and 87% respectively, as compared to standard sugar (no membrane
treatment). This was attributed to that the UF removes colorant precursors
that generate color in boiling, and high molecular weight colorants, which
are preferentially occluded within the crystal. to In addition, the crystal
yield is also increased from 42 to 49%, because the partial removal of
polysaccharides by UF which induces a viscosity decrease in the
massecuite.
Kishihara and Fujii (2000) studied the effect of clarification of raw
sugar melt by ultrafilter with molecular weight cut-off of 100,000 on
crystallization. Results showed that “In crystallization from the permeate,
it can be supposed that the massecuite in a boiling pan is more thoroughly
stirred and crystallization of sucrose is accelerated. Surface tension of
Raw sugar solution became larger after UF, which demonstrated that
surface active substances were eliminated. From this fact it can be
supposed that foaming during pan boiling is depressed. Through the
improvement of the physical properties (viscoelasticity and surface
tension) of sugar solutions, it is expected that the handling of pan boiling
may become easier, and the boiling time may be shortened.”

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Examples of Using New Separation Process as an Alternative for

Conventional Production of Sugar
Vaccari et al. (1997) proposed a method for direct production of
commercial white sugar without using the traditional clarification
process. The process, as illustrated in Figure 9, includes adding sodium
hydroxide to the raw juice to adjusting the pH to 7 in order to limit the
sucrose inversion by subsequent steps. Then the raw juice is subjected to
microfiltration using an organic membrane having a pore size of 0.2 µm.
After that, the microfiltered juice is passed through a cationic resin in the
sodium form to eliminate the magnesium ion. Finally, the thin juice is
concentrated at low temperatures and three stages cooling crystallization.
Results showed that commercial white sugar could be obtained
directly without the need of refining in the first crystallization step. The
energy balance is largely in favor of the new process in comparison with
the traditional method (Vaccari et al. 1997)

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Figure 9. Scheme for a complete crystallization cycle of

microfiltered and softened raw juice
(Source: Vaccari et al. 1997)

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A new process recently reported by Chou et al. (2000) called

Simplified Advanced Technology (SAT) uses proprietary processing aids
in conjunction with a tight filtration media such as the cross membrane
process. The process can produce plantation white sugar without
excessive use of SO2. Using the SAT process will improve yield by
avoiding sucrose destruction due to low pH and improve product quality.
The SAT process can also be integrated into a raw sugar mill (“the New
Raw Sugar Mill”) as shown in figure 10. The new raw sugar mill will
thereby have the capability to produce food grade sugar for direct sale, as
well as a very low color (VLC) sugar of 500 I.C.U. or an ultra low color
(ULC) sugar of 200 I.C.U. Either of which can act as input to a sugar
refinery, allowing the refinery to bypass the entire conventional unit.
processes of refining, except for secondary decolorization and
crystallization, in the case of the VLC sugar, or retain only crystallization
in the case of ULC sugar.
New Raw Sugar Mill

Clarified SAT Sugar Additional Refined

Crystallization
Juice Process Products Crystallization Products
Color Color
VLC ULC
8500/12000 20/45
500 200

Food
Sugar Refinery Products

Raw Primary Secondary

Affination Crystallization Products
Sugar Decolorization Decolorization
Color 1000/1500 500/700 200/300 Color
1500/3000 20/45

Figure 10. Flow diagram of new sugar mill and sugar

refinery based on the SAT process.
(Source: Chou et al. 2000)
Although the idea to use ultrafiltration for clarified juice was
studied since early 80’s, a large-scale system was installed in Puunene,
Hawaii, plant only several years ago. According to this method, called the
new Applexion process (Figure 11), the clarification of raw juice is
achieved by membrane filtration followed by softening. The UF system
comprises 940 m2 of Kerasesep membrane having a membrane porosity
of 0.02 µm. The juice softening system comprises two columns of strong
cationic resin and is designed to remove at least 80% of the hardness in
filtered clarified juice. The benefits derived from these two additional
unit operations are mainly: producing higher quality sugar, increasing
sugar recovery, reducing chemical usage in evaporator cleaning and
reducing steam consumption (Kwok 1996).

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Cane

Milling

Mixed Juice

Clarification Mud Filters

Clarified Juice

Ultrafiltration

Filtered Juice

Soft B Molasses Juice Softening Hard Molasses

Soft Juice

Evaporation

Soft Syrup

A Crystallization

A Massecuite

A Centrifugals Super VLC

A Molasses

B Crystallization

B Massecuite

B Magma B Centrifugals

C Crystallization

C Massecuite

Low Grade
Crystallizers

Low Grade
C Melt
Centrifugals

Final Molasses

Figure 11. A Flow diagram of New Applexion Process

(Source Kwok 1996).
An industrial plant has been processing 1000 gpm of clarified juice
since 1994. As expected, it has been running 800 days, then due to partial
erosion, the membrane performances declined and part of them has to be
changed (Kwok 1996).
Honiron (a division of Cameco industries) developed the A.B.C.
process to produce refined sugar from cane mixed juice. The process,

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which has been trialed in Louisiana and Guatemala consists of three

steps:
• Continuous screening to remove all insoluble particles down to
about 50 µm.
• Ultraclarification using hollow fibre polymeric membranes of 0.1-
0.2 µm pore size to remove high molecular weight impurities.
There is no conventional clarification step and the pH is adjusted to
6.6-6.8 using caustic soda.
• Adsorption to remove phenolic and caramel colorants and viscosity
precursor compounds from juice or syrup (Willet 1997)
However, it was discovered after a short period of operation that
clarification through the polymeric membranes is not sustainable and the
process may not be viable. It is understood that the feed to the filtration
membranes has been switched to clarified juice rather than raw mixed
juice. This was an obvious problem in the original process design (Steindl
and Doyle 1999).

Costs of Using Membrane

The critical factors that are needed for an economic assessment of a

membrane installation are the achievable flux levels, the required
frequency, and duration of the cleaning cycle, and the membrane life or
replacement frequency. As well, the increase in pan stage throughput and
the economic benefit of improved sugar quality must be included. The
buffer tanks, pumps and control equipment associated with a membrane
filtration plant remain essentially the same irrespective of the membrane
type (Steindl and Doyle 1999).
Approximate costs for three membrane types are given in Table VI.

Table VI Approximate costs of some type of membrane

( Source: Steindl and Doyle 1999).

Spiral Stainless
Membrane type Ceramic
Polymeric steel
Membrane cost, US 140 1100 750
2
$/m 2 4 5
Warranty Period
(seasons)*
* Specified in terms of 150 days per crushing season.

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Honiron estimates that operating costs for their A.B.C. Process

labor, chemicals, energy, maintenance, and replacement of membranes,
and adsorbent — is less than US $5 per tonne of sugar (based on U.S.
sugar production). However, These costs were estimates based on small-
scale pilot trials. There were insufficient factory data on costs to validate
these claims. Some estimate that membranes may have to be replaced
once a year, at a cost of around $4/ton (Willet 1997).
It is estimated that the capital cost, including membrane membranes
for installing the system in a 10,000 tonnes/day in the U.S. is $ 8 million
to $ 10 million. Another estimate was about $3 million to $ 4 million to
install a mill having a capacity of 3,000 tonnes/day (Krapf 1996).
However, membrane technology has improved dramatically in
recent years and continues to move forward. This should reduce future
installing and replacement costs.

Conclusions
• Review of data indicated that micro- and ultrafiltration of raw beet,
raw cane juices can provide high quality permeate and therefore,
improve sugar quality.
• Applying membrane filtration to purify raw juices leads to
eliminate or minimize the consumption of the lime.
• Direct production of refined sugar from raw cane juice could be
achieved by applying membrane filtration along with softening and
chromatographic separation.
• The membrane filtration need to optimize and long term testing
should be run to evaluate the performance of the membrane and the
required period to replace it.
• A cleaning program should be developed and losses of sugar in
concentrate should be carefully studied.

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