Title of Invention

"SUGAR CANE JUICE CLARIFICATION PROCESS"

Abstract A process to clarify raw sugar cane juice, which comprises adding a source of lime, adding an anionic inorganic colloid or polyacyrlamide, and carbonating.
Full Text TITLE OF INVENTION
SUGAR CANE JUICE CLARIFICATION PROCESS
FIELD OF THE INVENTION
The invention refers to an enhanced process to clarify raw sugar
cane juice by means of the use of an anionic inorganic colloid or
polyacrylamide polymer, particularly together with a carbonating process.
BACKGROUND OF THE INVENTION
Sugar cane juice is an extremely complex liquid medium, containing
many organic and inorganic constituents in soluble, suspended/decantable
and suspended/colloidal form. Cane sugar for human consumption is
produced by means of clarification of sugar cane juice using an extraction
process, which is then processed and concentrated to obtain sugar.
Clarification is therefore an essential step to obtain high yields and
high quality of the sugar. The clarification process needs to remove
components other than sucrose and, at the same time, minimize loss of
sucrose and color formation.
Sulfitation is currently the most widely used process to clarify cane
juice. It consists of SO2 (sulphurous anhydride) absorption by the juice,
reducing its original pH to levels between 3.7 and 4.2. The use of the
sulfitation process involves: (a) inhibition reactions causing color
formation; (b) coagulation of suspended colloids; and (c) formation of a
precipitate of CaSO3 (calcium sulfite). Furthermore, it also reduces the
viscosity of the juice and consequently of the syrup, massecuites, and
molasses, facilitating evaporation and baking operations.
Nevertheless, the sulfitation process has problems which the
sugar/alcohol industry would like to be solved, including (a) sucrose
inversion due to low pH during the process; (b) potential environmental
and external corrosion problems in the area, caused by any emission of
SO2/SO3; (c) incrustation and corrosion of the evaporation equipment; and
(d) presence of sulfite in the final sugar.
Another method to clarify sugar cane juice is carbonation, which
generally employs treatment with lime and controlled addition of carbon
dioxide (CO2). However, this process results in (a) increase in the loss of
inverted sugar in the juice (fructose and glucose) due to the high alkaline
pH (generally pH of about 10) and the high temperatures used for the
process, adversely affecting yield of alcohol production from the final
molasses, and (b) difficulty in filtering the precipitates from clarifiers,
requiring a higher investment in equipment, higher operational costs and a
more complex operation.
Therefore, there is a desire to have a clarification process which is
superior to the sulfitation process, but which avoids the problems with
carbonation. The present invention provides such a process.
Silicate microgels are used in water purification and water flow
processes. WO 99/61377 discloses a process to clarify water streams
containing biosolids resulting from processing food and organic residues,
which comprises contact of the stream with an anionic colloid, which may
be a silicate microgel, and an organic polymer to flocculate the biosolids.
For sugar cane juice clarification it is desired to minimize the
accumulation of silica in the juice and in production heating equipment.
The process of the present invention resolves this problem while avoiding
the problems with the prior art sulfitation and carbonation processes.
SUMMARY OF THE INVENTION
The invention comprises a sugar cane juice clarification process
comprising at least the steps of addition of lime; addition of anionic
inorganic colloid, a polyacryamide polymer, or both said colloid and said
polymer; and carbonation.
More specifically, the invention comprises an improved process to
clarify sugar cane juice by carbonating, comprising the addition of an
anionic inorganic colloid or polyacrylamide polymer, according to the
following steps:
a) heating of the raw sugar cane juice to be clarified;
b) adding a source of lime;
c) adding an anionic inorganic colloid, a polyacrylamide
polymer, both the said colloid and polymer sequentially,
or a mixture thereof;
d) carbonating by adding carbon dioxide; and
e) decanting precipitates formed to yield a supernatant
containing sugar cane juice.
Optionally, the addition in step c) can be after, instead before, the
step d) carbonation; i.e., downstream of the carbonating step.
The process optionally further comprises:
a) heating of the supernatant from step e) above;
b) carbonating by adding carbon dioxide; and
c) decanting any precipitates formed to yield a further
supernatant containing sugar cane juice.
DETAILED DESCRIPTION OF THE INVENTION
According to a specific embodiment of the invention, the clarification
process of the present invention comprises the steps of:
a) heating of the raw sugar cane juice to be clarified;
b) adding a source of lime;
c) adding an anionic inorganic colloid, or a polyacrylamide
polymer, or both the said colloid and polymer
sequentially, or a mixture of said colloid and said
polymer;
d) carbonating by adding carbon dioxide; and
e) decanting precipitates formed to yield a supernatant
containing sugar cane juice.
In particular, the present invention provides an improved process for
clarifying raw sugar cane juice using carbonation wherein • the
improvement comprises addition of an anionic inorganic colloid, a
polyacrylamide polymer, both said colloid and polymer sequentially, or a
mixture of said colloid and said polymer. The preferred anionic inorganic
colloid is silicate microgel.
During step a), raw sugar cane juice is heated to a temperature
between about 45 °C and about 90 °C, preferably between about 50 °C
and about 85 °C, and still more preferably between about 55 °C and about
80 °C. Juice heating has the purpose of facilitating downstream
processes by speeding up chemical reactions and improving the
coagulation and sedimentation of colloids and others non-sugars.
The liming step b) is the addition of a source of lime (CaO) to the
raw cane juice. Any suitable source of lime can be employed, but lime
milk (Ca(OH)2) or calcium saccharate are preferred. The addition of the
source of lime raises the pH of the sugar cane juice. Lime is added up to
a maximum concentration of about 2 % by weight of the solids content of
the juice. This addition has the purpose of eliminating juice colorants,
neutralizing organic acids, and forming calcium phosphate precipitate,
which upon sedimentation carries with it the impurities present in the
liquid.
Between steps b) and c), it is particularly advantageous that a time
interval of between about 0.5 and about 10 minutes is optionally observed.
In step c) of the process of the present invention an anionic
inorganic colloid is added. Such colloids useful in the process of this
invention include silica-based anionic inorganic colloids and mixtures
thereof. Silica-based anionic inorganic colloids include, but are not limited
to, colloidal silica, aluminum-modified colloidal silica, polysilicate
microgels, polyaluminosilicate microgels, polysilicic acid, and polysilicic
acid microgels, and mixtures thereof. For those colloids containing
aluminum, the aluminum can be on the surface and/or in the interior of the
particles.
The anionic inorganic colloids used in this invention can be in the
form of a colloidal silica having an S value >70%, generally >75%, and
containing about 2 to 60% by weight of SiO2, preferably about 4 to 30% by
weight of SiO2. The colloid can have particles with at least a surface layer
of aluminum silicate or it can be an aluminum modified silica sol. The
alumina content of the surface-modified silica sol can be in the range of 2
to 25%. The colloidal silica particles in the sols commonly have a specific
surface area of 50-1200 m2/g, more preferably about 200-1000 m2/g. The
silica sol can be stabilized with alkali in a molar ratio of SiO2:M2O of from
10:1 to 300:1, preferably 15:1 to 100:1, and most preferably 6:1 to 12:1 (M
is Na, K, Li, or NH4).
Preferred for use in the process of the present invention are silicate
microgels. Microgels are distinct from colloidal silica in that the microgel
particles usually have surface areas of 1000 m2/g or higher and the
microgels are comprised of small 1-2 nm diameter silica particles linked
together into chains and three-dimensional networks. Polysilicate
microgels, also known as active silicas, have SiO2:Na2O ratios of 4:1 to
about 25:1, and are discussed on pages 174-176 and 225-234 of "The
Chemistry of Silica" by Ralph K. Her, published by John Wiley and Sons,
N. Y., 1979. Polysilicic acid generally refers to those silicic acids that have
been formed and partially polymerized in the pH range 1-4 and comprise
silica particles generally smaller than 4 nrn diameter, which thereafter
polymerize into chains and three-dimensional networks. Polysilicic acid
can be prepared in accordance with the methods disclosed in U. S.
Patents 5,127,994 and 5,626,721. Polyaluminosilicates are polysilicate or
polysilicic acid microgels in which aluminum has been incorporated within
the particles, on the surface of the particles, or both. Polysilicate
microgels, polyaluminosilicate microgels and polysilicic acid can be
prepared and stabilized at acidic pH: Microgel size can be increased by
any of the known methods such as of aging of the microgel, changing pH,
changing concentrations, or other methods, known to those skilled in the
art. The use of silicate microgels provides the advantage in the process of
the present invention of reducing scaling in equipment, and therefore
equipment and maintenance cleaning problems.
The polysilicate microgels and polyaluminosilicate microgels useful
in this invention are commonly formed by the activation of an alkali metal
silicate under conditions described in U. S. Patents 4,954,220 and
4,927,498. However, other methods can also be employed. For example,
polyaluminosilicates can be formed by the acidification of silicate with
mineral acids containing dissolved aluminum salts as described in U. S.
Patent 5,482,693. Alumina/silica microgels can be formed by the
acidification of silicate with an excess of alum, as described in U. S. Patent
2,234,285.
In addition to conventional silica sols and silica microgels, silica sols
such as those described in European patents EP 491879 and EP 502089
can also be used for the anionic inorganic colloid in this invention. These
are commonly referred to as low "S value" sols. EP 491879 discloses a
silica sol having an S value in the range of 8 to 45% wherein the silica
particles have a specific surface area of 750 to 1000 m2/g, which have
been surface-modified with 2 to 25% alumina. EP 502089 discloses a
silica sol having a molar ratio of SiO2 to M2O, wherein M is an alkali metal
ion and/or an ammonium ion of 6:1 to 12:1 and containing silica particles
having a specific surface area of 700 to 1200 m2/g.
Included within the scope of colloidal silica sols useful in the
present invention are colloidal silica sols having a low "S value". S value
is defined by ller and Dalton in J. Phys. Chem., 1956, vol. 60, pp. 955-957.
S value is a measure of the degree of aggregate or microgel formation and
a lower S value indicates a higher microgel content and is determined by
the measure of the amount of silica, in weight percent, in the disperse
phase. The disperse phase consists of particles of anhydrous silica
together with any water that is immobilized at the surface or in the interior
of the particles.
In the process of the present invention the preferred silicate
microgel is added to the mixture of sugar cane juice and lime source in
step c), preferably at a quantity of between about 50 ppm and about 500
ppm, more preferably from about 50 ppm to about 200 ppm. Silicate
microgels are commercially available, such as Particlear® manufactured
by E. I. du Pont de Nemours and Company of Wilmington DE, and are
produced by any method known in the art. US Patent 6,060,523 and US
Patent 6,274,112 disclose enhanced processes allowing reliable
preparation of the microgels. Silicate microgel typically is obtained from
sodium silicate. It is also designated as silicon dioxide microgel or active
silica, comprising between about 0.5% and 2% SiO2, particularly about 1%
SiOz solution.
Alternatively, a polyacrylamide polymer is employed in step c) of the
process of the present invention. A quantity of from about 1 ppm to about
10 ppm is employed, preferably from about 2 ppm to about 5 ppm.
Suitable polyacrylamide polymers for use herein include mainly anionic
polymers, which carry the same charge as the particles of the suspension
in raw juice. Preferred are partially hydrolyzed polyacrylamides having a
moderate degree of hydrolysis (between about 15% and about 40%
hydrolyzed). The polymer molecular weights usually are above 1,000,000.
Suitable polyacrylamides are available commercially, for example from
Kemwater Brasil S.A., Sao Paulo, Brazil.
The silicate microgel and polyacrylamide can both be used in the
process of the present invention by adding them sequentially in any order
or as a mixture. Use of the silicate microgel is preferred due to faster
dewatering during filtration resulting in better filtration.
Applicant has developed an enhanced carbonati ng process for
cane juices, comprising the addition of an anionic inorganic colloid,
preferably silicate microgel, and adjusting it to the operating conditions of
a modified and improved carbonating process, thus solving the problems
for its industrial implementation and permitting higher yields of purer
sugar. The process of the present invention recovers the waste CO2 from
fermenters and replaces SO2 currently used in the sulfitalion process for
juice clarification with the recovered CO2. It also lowers scale formation in
evaporators and heat-exchangers by removal of scale forming compounds
from the juice through the improved clarification process. Furthermore,
the process of the present invention solves the problem of filtering the
precipitates/sedimentation generated by the traditional carbonation
processes, and does not increase the loss of inverted sugars.
Furthermore, the process of the present invention reduces the
consumption of CaO in comparison with the traditional carbonation
processes.
The process of the present invention reduces sucrose losses by
inversion, obtains better purification of the cane juice by removal of more
organic and inorganic impurities, reduces corrosion of equipment due to
the absence of SO2, lowers scaling in evaporators, and provides improved
sugar production.
According to a preferred embodiment of the invention, the microgel
is activated by an acid, particularly from CO2, because CO2 is abundant at
sugar cane processing facilities that produce ethanol by fermentation of
juice and/or molasses.
A time interval between step c) and the subsequent one is
advantageous and this time interval is typically between 0.5 and about 10
minutes.
In step d), CO2 is added, preferably in sufficient quantity to form
calcium carbonate precipitates. The flow of CO2 is regulated to control
foaming and reaction time. In a preferred embodiment of the present
invention, the CO2 is added through a carbonation column, in counter flow
with the limed raw sugar juice source fed into the top of the column.
Optionally the anionic inorganic colloid, or the polyacrylamide, or
each of the former, or a mixture thereof, can be added after the
carbonating step instead of prior to the carbonating step in the amounts
previously disclosed.
After the carbonation step, the decanting step e) is undertaken. In
step e), the sugar cane juice is purified by removing precipitated impurities
as solids. The decanted juice is removed from the upper part of the
decanter and delivered to an evaporator, where it is concentrated. The
precipitated and sedimented materials have a solid concentration of about
10°Be and are usually taken from the bottom of the decanter and sent to a
filtering sector where the materials are subsequently filtered to recover
sugar. According to the invention, the required decanting time is less than
one hour, usually about 30 minutes. The pH of the supernatant, after this
first carbonation, is usually between about 8 and 10, preferably about 9.
The carbonation process of the present invention is particularly
advantageous when conducted using the final supernatant as the starting
material in a second carbonation. Thus, the present invention further
comprises a carbonation process which, in addition to the above-disclosed
steps, additionally comprises the following steps:
a) heating of supernatant resulting from the abovedescribed
process;
b) carbonating by adding carbon dioxide; and
c) decanting any solids precipitated to yield a further
supernatant containing sugar cane juice.
During step a), the supernatant is heated at temperatures between
about 60 °C and 90 °C, preferably about 70 °C. Heating is followed by a
carbonation step. Operating conditions are employed which avoid
excessive foam formation and generate the expected neutral pH for the
juice. In a preferred embodiment, CO2 is added through a second
carbonation column, in counter flow with the clarified juice fed into the top
of such column. This column adjusts the final pH of the treated juice. The
final pH is typically from about 6.5 to about 8, preferably about7. Any
solids precipitated are decanted to yield a further supernatant containing
sugar cane juice. Often there are no precipitants formed during the second
carbonation.
The process of the present invention as disclosed herein makes
use of carbonation to clarify sugar cane juice, presenting advantages over
the sulfitation process in higher yields with better quality product.
The elimination of use of sulfur in the process of the present
invention represents a noticeable advantage, not only in cost, but also
resulting in higher process safety, lower corrosion and/or scaling of
heating equipment, and less environmental degradation.
Sucrose inversion in the process of the invention is reduced by
between about 1.5% and 2.5%, which represents a yield increase. As a
direct consequence of this aspect a higher yield in crystal sugar production
is obtained using the same equipment, since sucrose forms sugar crystals
and not reducing sugars. This single standard demonstrates that the
process of the present invention is significantly better than those in the
prior art.
The process of the present invention results not only in a lower loss
of sucrose, but also in higher removal of non sugars such as starches,
proteins, solids in suspension and dissolved solids. The protein and
starch are surprisingly reduced, typically to less than 3 ppm in the clarified
juice.
The process of the present invention yields purer product with
better physical features such as color. The purity (Purity = POL/Brix) may
increase for two different reasons: (i) higher content of sucrose (higher
numerator) or (ii) lower content of non-sugars (lower denominator). Higher
reduction in sucrose inversion favors further crystallization since the
process will suffer less interference from impurities.
The lower quantity of impurities is very desirable and benefits the
whole operation, since it reduces the overall volume to be processed
throughout the system. Therefore, there is less incrustation/scaling in the
heating equipment, especially the evaporator, which then does not need to
be cleaned so frequently. This reduces maintenance and steam energy
costs and increases safety for employees who conduct such cleaning
operations at the industrial facility.
Furthermore, the impurity reduction provided by the process of the
present invention, results in much higher sugar quality. Impurities and
color (standard Icumsa (420 nm)) are reduced improving its market value.
A color measure of the clarified sugar juice having a maximum of 7100,
preferably a maximum of 6000, and more preferably a maximum of 5000,
is attainable.
Besides being a safer process with superior product, the process of
the present invention provides a reduction in impurities in the juice
between about 1.5% and 2.0%. For all of the above reasons, the process
provides increased efficiency overall. Fewer impurities are processed
under the same installed capacity, thus increasing sugar production.
This increase in sugar production does not affect alcohol production
from the molasses. Reducing sugars remain in the final molasses and can
be converted to ethanol. Therefore, due to the reduction in sucrose
inversion, there will be less final molasses for alcohol production. But, to
keep the same desired levels, it is only required to deviate more raw juice
to the distillery, skipping the clarification, evaporation and vacuum steps of
the process.
In addition to the above advantages, the process of the present
invention improves the reduction of juice turbidity, reduction of organic
colloids (e. g. starch), and improved coagulation and flocculation. In
particular, the time to form flakes is reduced and the size of the flakes is
reduced. Thus sedimentation time is reduced overall. A further
advantage is the optional elimination of the addition of flocculating agents.
The carbonation process of the present invention is especially
advantageous for use at temperatures between about 70 °C and about
80 °C, thus avoiding a negative effect on yield of alcohol production from
the final molasses. Simultaneously, energy cost and decanting time are
reduced. Keeping the juice at an elevated temperature leads to inversion
and reducing sugar degradation to form organic acids, resulting in a
decrease in purity and pH. The reduction in decanting time of the process
of the invention reduces the loss of sugar by inversion.
The fact that the new process generates precipitates/sediment with
easier filtering characteristics than traditional carbonation is exceptionally
advantageous to the sugar/alcohol industry. The sediment resulting from
traditional carbonation is difficult to filter, requiring the installation of
pressing filters, representing a large financial investment and a more
complicated process. This is one of the main reasons why the prior art
carbonation process is not more widely used. The process of the present
invention generates precipitates/sediment which does not require the
installation of press filters, since vacuum rotating filters can be used.
Besides better filtering, the precipitates/sediment resulting from the
process of the invention comprises a lower quantity of sucrose. The loss
of sucrose represents less than 0.4% of the total sugar entering the plant,
thus representing approximately half of the current losses. Furthermore,
as opposed to traditional carbonation processes, lime consumption is
much lower. It is less than 2 % by weight of solids present in the juice. In
the traditional carbonation processes, the lime consumption is between 6
to 10 % by weight of solids present in the juice.
Thus, the process of the invention is a faster and safer process,
results in a significant increase in yield, generates superior quality, and
avoids the problems in the conventional carbonation process. It is useful
to clarify sugar cane juice more efficiently.
As the experts in the art will realize, numerous modifications and
variations of the scope of the invention are possible in the light of the
above teachings. It should therefore be understood that the invention can
be embodied in other ways besides those specifically described herein.
EXAMPLES
Raw sugar cane juice from the past crop season typically had the
following properties: pH of 5.2-5.8, turbidity of 5000, color of 10,000 to
12,000 using the ICUMSA Method #4, Brix of 14 to 16, and total reducing
sugars of 13 to 15.
Example 1
Raw sugar cane juice (I liter) was heated slowly to 80 ° C in a 2 liter
beaker, followed by gradual addition of 33 ml of liming milk (calcium
hydroxide, Ca(OH)2) to raise the pH to 8.5. The solution was maintained
for about one (1) minute, following which was added 160ppm silica
microgel available as Particlear® from E. I. du Pont de Nemours and
Company, Wilmington, DE. The solution was then held for about 2
minutes. The pH of the solution was kept at 8.4 via simultaneous addition
of liming milk and carbon dioxide gas. Liming milk (105mL) was added to
reach a total of 2% CaO by weight on solids content. The carbon dioxide
was introduced at a steady rate of 260 cc/minute. Finally, the pH of the
solution is lowered to 7.0 by bubbling additional carbon dioxide into the
solution. Total carbonation time was 15 minutes. During carbonation,
foam formation was controlled by regulating the CO2 flow rate and due to
the presence of microgel. The precipitate volume (in the original
carbonation beaker) was 160mL after 45 minutes of sedimentation.
This was followed by a filtration step, whereby 10OmL of the
concentrated precipitate was filtered in a vacuum of 58 mm Hg (7733 Pa).
Filtration time for a 75 ml sample was 6 minutes, with a time to cake
dryness of 8 minutes. The final pH of both the filtrate and the supernatant
liquid sugar juice was 7.9. The supernatant juice and vacuum filtered
juice were analyzed for pH, color, turbidity, Brix, and total reducing sugars.
Excellent clarity and transparency of the juice was evident during the
process. The turbidity of the final sugar juice was 16 NTU, and its color
was 6436 measured using the ICUMSA method #4. The Brix was 17.8.
Total reducing sugars was 16.7.
Comparative Example A
Sugar cane juice was processed in the mill using the sulfitation
process. The juice was contacted with SO2 and liming milk (calcium
hydroxide, Ca(OH)2) to form a precipitate of calcium sulfite (CaSO3). The
coagulated precipitate was then separated from the supernatant. The
product had a pH of 6.5, color of 9030 using ICUMSA Method #4, Brix of
15.8, Total reducing sugars of 14.6, and sulfites of 150.
Example 2
Raw sugar cane juice was processed as in Example 1. The final
product had a pH of 8, turbidity of 54 NTU, color of 7096 using the
ICUMSA Method #4, Brix of 17.0 and Total reducing sugars of 16.2.
Example 3
Raw sugar cane juice was processed continuously in a pilot plant
using 2 to 3 liters of juice per hour and running 3 to 4 hours per day using
the process of the present the invention. Raw sugar cane juice was
heated to 55 °C, followed by addition of liming milk (calcium hydroxide,
Ca(OH)2) to raise the pH to 10.5. Liming milk consumption was about 1.2
% CaO by weight on solids content. The solution was maintained for about
five (5) minutes. The solution was then carbonated in a counter flow
column. The carbon dioxide was introduced from the bottom, at a steady
flow rate, in order to get a final carbonated juice pH of 9.5, downstream of
the column. In the column, the carbonation time was 10 minutes.
Following which was added 150 ppm silica microgel available as
Particiear® from E. I. du Pont de Nemours and Company, Wilmington, DE.
The solution was then held for about 5 minutes. The microgel-carbonated
juice was then sent to a decanter in order to separate the precipitate from
the clarified juice (supernatant). Finally, the supernatant was heated up to
70 °C, and the pH of this heated solution was lowered to 7.0 by bubbling
additional carbon dioxide into the solution, in a second counter flow
carbonation column. The precipitate from the decanter was sent for
characterization and the results are given in Table 1 and 2 below.
Table 1 compares the properties of the sugar juice made using the
process of the present invention according to Example 3 to average
results reported in the literature for carbonation processes not employing
silica microgel.
(Table Removed)
Examples 4-12 and Comparative Examples A-F
Carbonated materials from the process of Example 3 were filtered
using 200 ml suspension volume at three different pressures as indicated
in table 3 using a Bokela filter device, available from Bokela, Karlsruhe,
Germany. Materials from a traditional sulfitation process were filtered
under the same conditions. The material using the process of the present
invention showed solids which were fiber like and formed a filter cake of
16-27% solids, which was easier and faster to dewater. In contrast,
material from the comparative sulfitation process formed a gel-like filter
cake of about 23% solids, which was more difficult to dewater. Turbidity of
the resulting sugar juice (filtrate) was about 11,000-12,000 NTU for the
comparative sulfitation process and about 4,000-5,000 NTU for the
process of the present invention. Specific results are listed in Table 3
beiow.
(Table Removed)
Also in this case, according to above results, the material using the
process of the present invention showed percent solids in the cake similar
to Examples 4-6 above. However, as in the comparison with sulfitation
process, the filtrate turbidity from the process of the present invention
using silicate microge! or polyacrylamide was better and the filtration of the
cake was easier. The process of the present invention using silicate
microgel was faster to dewater. In addition, in terms of filter operation, the
cake from the carbonation process of the present invention using the
silicate microgel released better from the filter screen, in comparison with
the other processes.




We Claim:
1. A process to clarify raw sugar cane juice characterized by the steps of:
a) addition of a source of lime;
b) addition of a silicate microgel having a surface area of 1000 m2/g or higher; and
c) carbonation.
2. The process of claim 1, wherein the process consists of the following steps:
a) heating of the raw sugar cane juice to be clarified;
b) adding a source of lime;
c) adding a silicate microgel having a surface area of 1000 m /g or higher;
d) carbonating by adding carbon dioxide; and
e) decanting precipitates formed to yield a supernatant containing sugar cane juice.
3. The process of claim 2, wherein the process consists of the following optional
steps:
a) heating of supernatant;
b) carbonating by adding carbon dioxide; and
c) decanting any precipitates formed to yield a further supernatant containing sugar cane juice.

4. The process of claim 2, wherein the silicate microgel is added after the step d) instead of before step d).
5. The process of claim 2, wherein the raw sugar cane juice is heated at a temperature between about 45°C and about 90°C.
6. The process of claim 2, wherein the lime is added to the raw cane juice to achieve a maximum concentration of 2% by weight of solids of the raw cane juice, and the lime is in the form of lime milk (Ca(OH)2) or calcium saccharate.
7. The process of claim 2, wherein the silicate microgel is added in an amount
from about 50 ppm to about 500 ppm, and the addition of silicate microgel is conducted after
a period of from about 0.5 to about 10 minutes after adding lime.
8. The process of claim 2, wherein the carbon dioxide is added after a time
interval of from about 0.5 to about 10 minutes has elapsed after the addition of silicate
microgel.
9. The process of claim 2, wherein the precipitates have a solid concentration of
about 10°Baume, said precipitates are subsequently decanted to separate the purified sugar
cane juice from the precipitates, and the final pH of the supernatant is from about 6.5 to about
8.
10. The process of claim 3, wherein the supernatant is heated at temperatures
between about 60°C and about 90°C, and the carbon dioxide is added in an amount sufficient
to lower the pH of the sugar cane juice supernatant to about 7.0.
11. The process of claim 3, wherein the supernatant has a maximum color of 6000.

Documents:

4736-delnp-2006-abstract.pdf

4736-delnp-2006-assignment.pdf

4736-DELNP-2006-Claims-(10-05-2012).pdf

4736-delnp-2006-claims.pdf

4736-DELNP-2006-Correspondence Others-(10-05-2012).pdf

4736-DELNP-2006-Correspondence Others-(10-10-2011).pdf

4736-DELNP-2006-Correspondence-Others-(18-05-2010).pdf

4736-delnp-2006-correspondence-others.pdf

4736-delnp-2006-description (complete).pdf

4736-delnp-2006-form-1.pdf

4736-delnp-2006-form-18 (18-02-2008).pdf

4736-delnp-2006-form-2.pdf

4736-DELNP-2006-Form-3-(10-05-2012).pdf

4736-DELNP-2006-Form-3-(10-10-2011).pdf

4736-delnp-2006-form-3.pdf

4736-delnp-2006-form-5.pdf

4736-DELNP-2006-GPA-(10-05-2012).pdf

4736-DELNP-2006-GPA-(18-05-2010).pdf

4736-delnp-2006-gpa.pdf

4736-delnp-2006-pct-210.pdf

4736-delnp-2006-pct-401.pdf

4736-delnp-2006-pct-409.pdf

4736-delnp-2006-pct-416.pdf


Patent Number 254837
Indian Patent Application Number 4736/DELNP/2006
PG Journal Number 52/2012
Publication Date 28-Dec-2012
Grant Date 26-Dec-2012
Date of Filing 18-Aug-2006
Name of Patentee E.I. DU PONT DE NEMOURS AND COMPANY.
Applicant Address 1007 MARKET STREET, WILMINGTON, DELAWARE 19898, U.S.A.
Inventors:
# Inventor's Name Inventor's Address
1 FABIO ALESSIO ROMANO DIONISI RUA PORANGABA, 217 BOSQUE DA SAUDE, 04136-020 SAO PAULO, BRAZIL
2 IDALINA VIEIRA AOKI RUA DAVID BEN GURION, 1064 APARTMENT 121 (VILA SUSANA), 05634-001 SAO PAULO, BRAZIL
3 RAFAEL JANUARIO CALABRESE ALAMEDA ARAPANES, 628 APARTMENT 61 (MOEMA), 02338-050 SAO PAULO, BRAZIL
PCT International Classification Number C13D 3/02
PCT International Application Number PCT/US2005/008596
PCT International Filing date 2005-03-15
PCT Conventions:
# PCT Application Number Date of Convention Priority Country
1 60/553,442 2004-03-16 U.S.A.
2 11/072,909 2005-03-04 U.S.A.