Classifications

• • C—CHEMISTRY; METALLURGY
  • C13—SUGAR INDUSTRY
  • C13B—PRODUCTION OF SUCROSE; APPARATUS SPECIALLY ADAPTED THEREFOR
  • C13B20/00—Purification of sugar juices
  • C13B20/12—Purification of sugar juices using adsorption agents, e.g. active carbon
  • C13B20/126—Organic agents, e.g. polyelectrolytes
• • C—CHEMISTRY; METALLURGY
  • C13—SUGAR INDUSTRY
  • C13B—PRODUCTION OF SUCROSE; APPARATUS SPECIALLY ADAPTED THEREFOR
  • C13B20/00—Purification of sugar juices
  • C13B20/005—Purification of sugar juices using chemicals not provided for in groups C13B20/02 - C13B20/14

Definitions

• the present invention generally relates to the use of a quaternary ammonium salt and a cationic (co)polymer to clarify sugar cane juice during the production of crystal or raw sugar.
• the invention also refers to a new process for producing crystal or raw sugar from sugar cane juice. More specifically, the present invention describes a process for improving the phosphatation clarification of crystal or raw sugar by adding a quaternary ammonium salt and a cationic (co)polymer before, during or just after the clarification step.
• a kit comprising a quaternary ammonium salt and a cationic (co)polymer is also provided.
• Sugar cane is the main sugar producing crop, with a world sugar production approximately six times bigger than from sugar beet, the other major source of sugar.
• Sugar cane is one of the several species of tall perennial true grasses, with an established agricultural field crop, in all tropical and subtropical countries of the world, and being put into progressively improved sugar production processes.
• the conventional process for producing crystal and raw sugar from sugar cane involves the extraction of sugar cane juice from the harvested sugar cane.
• the sugar cane juice is submitted to purification, also commonly known as clarification, resulting in crystal sugar or raw sugar.
• the raw sugar can be remelted to give sugar syrups or sugar liquors, which are the raw material used to produce the refined sugar.
• the sugar cane juice clarification is the most important step to supply sugar of optimum quality to the market.
• a sugar cane juice clarification technology called sulfitation
• This usual process of clarification involves the addition of sulfur dioxide (S0 2 ) to the juice in order to separate non-sugar constituents, including colored materials.
• S0 2 sulfur dioxide
• the sugar produced by this process may contain about 20 ppm or more of sulfur and this contaminant causes health and environmental problems and became difficult to be accepted in food and beverages markets.
• another process to clarify beet juice called carbonatation. This process consists in adding a slurry of calcium hydroxide and to bubble carbon dioxide gas in order to precipitate calcium carbonate.
• this kind of process suffers from several issues, in particular an over-consumption of lime, which renders the process economically not sustainable.
• the two sugar sources have different compositions, in particular the nature of non-sugars is different and beet does not have any reducing sugars.
• this process can be applied to refined sugar clarification but not in raw/crystal sugar production from cane.
• WO2014/011496 and FR 2578238 are disclosing such carbonatation processes using polymer color precipitants.
• the common clarification process is the phosphatation clarification. This process principle is based on the precipitation of calcium phosphates by adding phosphoric acid and lime.
• DHT Dimethyl-dioctadecylammonium chloride
• sugar syrups or liquors are melted raw sugars, they are more concentrated and with less impurities, which were removed in the previews steps of the sugar refining process, on the other hand, sugar cane juice is the juice extracted directly from crushing whole or peeled sugar cane in a mill.
• Dimethylamine-epichlorohydrin copolymer (DMA-Epi) is known from the Food and Drug Administration, HHS, 21 CFR Ch.l (4-1-12 Edition), paragraph 173.60 to be a "food additive used as a decolorizing agent and/or flocculant in the clarification of refinery sugar liquors and juices. It is added only at the defecation/clarification stage of sugar liquor refining at a concentration not to exceed ISO parts per million of copolymer by weight of sugar solids.” However, a good performance in sugar cane juice clarification in the process to produce crystal or raw sugar is achieved for quantities which exceed the regulation limitations. In view of the above, up to now there is no solution for improving clarification process of sugar cane juice to obtain crystal or raw sugar.
• the present invention aims to an optimized solution for clarifying sugar cane juice when producing crystal or raw sugar, using preferably the phosphatation principle.
• a further object of the invention is to propose an improved process to produce crystal or raw sugar with a low degree of coloration and thus, acceptable by the food, pharmaceutical and beverage industries.
• Another objective of the present invention is to propose a more efficient process, with fewer chemicals consumed, less corrosion and easier to control.
• the invention thus proposes the use of a quaternary ammonium salt and a cationic (co)polymer to clarify sugar cane juice during the production of crystal or raw sugar.
• the invention aims at the use of a quaternary ammonium salt and a cationic (co)polymer to clarify sugar cane juice by phosphatation during the production of crystal or raw sugar.
• the present invention also provides a process for producing crystal or raw sugar comprising the following steps:
• sugar cane juice or “mixed juice” in the sense of the present invention is any juice containing sugar and extracted by shredding and crushing whole or peeled sugar cane in a mill.
• Usual degree of coloration of sugar cane juice is between 5000-50000 IU (ICUMSA unit), more frequently between 10000 and 25000 IU, even more frequently between 12000 and 20000 IU.
• the method of measure of the degree of coloration in IU of a juice is described in the experimental part below.
• “Decanted juice” is the juice obtained from the sugar cane juice after performing a clarification step using a quaternary ammonium salt and a cationic (co)polymer according to the invention. Decanted juice with a degree of coloration below 10000 IU is preferred.
• the percentage of discoloration obtained from the mixed juice using a quaternary ammonium salt and a cationic (co)polymer according to the invention to clarify sugar cane juice during the production of crystal or raw sugar is generally the following:
• crystal sugar also known as plantation white sugar
• crystal sugar is a sugar produced directly from sugar cane juice obtained from sugar cane, basically by the processes of extraction, clarification, evaporation and crystallization.
• Examples of crystal sugar may include those with sucrose crystals with an average size of 0.4 to 0.8 mm, preferably 0.5 to 0.7mm, with a degree of coloration between 50 to 400 ICUMSA units, preferably 90 to 150 ICUMSA units and notably used for domestic and industrial purposes.
• raw sugar also known as a VHP (Very High Polarization) sugar
• VHP Very High Polarization
• raw sugar may include those with a degree of coloration between 400 to 1200 ICUMSA units, preferably 700 to 900 ICUMSA units and generally used as feedstock for the refining process to obtain refined sugar.
• phosphatation means that at least a portion of impurities responsible for the color of the sugar cane juice is removed by precipitation of phosphates using a phosphorous source.
• a quaternary ammonium salt or "a cationic (co)polymer” is a generic plural. It means that it has to be interpreted as “one or more” or “at least one”.
• the quaternary ammonium salt is advantageously a compound having the formula (I):
• Ri and R 2 independently from one another, are selected in the group consisting of C 8 to C 36 linear or branched, saturated or unsaturated aliphatic groups, optionally containing a heteroatom or an ester or amide group;
• R 3 and R 4 independently from one another, are selected in the group consisting of Ci to Ci 8 linear or branched, saturated or unsaturated aliphatic groups, optionally containing a heteroatom or an ester or amide group;
• X is an anion, for example selected from halide, nitrate, phosphate or acetate; preferably X is a halide; more preferably X is chloride.
• Ri and R 2 are selected in the group consisting of C i2 to C 20 linear or branched, saturated or unsaturated aliphatic groups, optionally containing a heteroatom or an ester or amide group, preferably Ci 6 to Ci 8 linear alkyl groups.
• R 3 and R 4 are selected in the group consisting of Ci to Ci 2 linear or branched, saturated or unsaturated aliphatic groups, optionally containing a heteroatom or an ester or amide group, preferably Ci to C 4 linear alkyl groups.
• the quaternary ammonium salt is dimethyl- dioctadecylammonium chloride.
• the quaternary ammonium salt according to the present invention can be derived from plants or animals or can be synthesized by a reaction between trialkylamines and haloalkanes, under well-known classical conditions.
• the dimethyldioctadecylammonium chloride is a reaction between methyldioctadecylamine and methyl chloride.
• the quaternary ammonium salt can be present in an amount of from 10 ppm to 700 ppm, preferably from 10 ppm to 160 ppm, more preferably from 20 ppm to 100 ppm, even more preferably from 20 to 60 ppm, notably 40 to 60 ppm or 20 to 40 ppm by weight based on the solid amount weight in the sugar cane juice.
• the amount is the "active content" weight based on the solid amount weight in the sugar cane juice.
• the quaternary ammonium salt can be added in the form of an aqueous solution or an alcoholic solution or a hydro-alcoholic solution.
• a preferred embodiment is the use of a solution containing ethanol and/or isopropanol as solvents for the quaternary ammonium salt, and also water.
• the cationic (co)polymer can either be a cationic homopolymer or copolymer.
• the cationic (co)polymer is a cationic copolymer of dialkylamine and epichlorohydrin, wherein the alkyl part is a linear or branched alkyl comprising from 1 to 6 carbon atoms, preferably 1 to 4 carbon atoms.
• the preferred cationic copolymer is a cationic copolymer of dimethylamine and epichlorohydrin (DMA-Epi).
• the preferred copolymer of dimethylamine and epichlorohydrin of CAS Reg. No. 25988-97-0, can have not more than 5 mole% of dimethylamine that may be replaced by an equimolar amount of ethylenediamine, and its mole ratio of total amine to epichlorohydrin is preferably about 1:1.
• the nitrogen content of the copolymer of dimethylamine and epichlorohydrin is 9.4 to 10.8 weight percent on a dry basis.
• DMA-Epi suitable molar mass can vary from 6,500 to 30,000 g/mol, preferably from 7,000 to 25,000.
• Cationic copolymer of dimethylamine and epichlorohydrin can be prepared by the step- reaction synthesis of 2-hydroxy-3-dimethylaminopropyl, a monomer formed by the reaction of epichlorhydrin and dimethylamine, as disclosed in Water Science and Technology: Water Supply Vol 1 Nol pp 43-50, IWA Publishing 2001. It is also available under the commercial names: Glokill PQ60 from Solvay S.A., and Barquat PQfrom Lonza Group AG.
• the cationic (co)polymer is polydiallyl dimethyl ammonium chloride (PolyDADMAC).
• the molecular weight of the polydiallyl dimethyl ammonium chloride (PolyDADMAC) can vary from 100000 to 200000 g/mol, preferably from 140000 to 180000 g/mol and more preferably around 160000 g/mol.
• PolyDADMAC can be prepared by radical polymerization of diallyldimethylammonium chloride (DADMAC), more precisely by free radical addition polymerisation of diallyldimethylammonium chloride (DADMAC) using persulfate or an organic peroxide as initiator. It is also available under the commercial names: Mirapol 100 from Solvay S.A., Percol 1697 from Allied Colloids Ltd, and Merquat 100 from Lubrizol Corporation.
• the cationic (co)polymer is advantageously present in an amount of from 10 ppm to 150 ppm, preferably from 10 ppm to 70 ppm, more preferably from 15 ppm to 40 ppm by weight based on the solid amount weight in the sugar cane juice.
• the amount is the "active content" weight based on the solid amount weight in the sugar cane juice.
• the cationic (co)polymer can be added in the form of an aqueous solution. - Additional components
• a phosphorus source is preferably also added during the production of crystal or raw sugar, preferably before, during or just after the clarification step.
• it is preferably selected from the group consisting of any salt containing a phosphate anion, selected preferably from hydrogen phosphites (HP0 3 ⁇ ), dihydrogen phosphates (H 2 P0 4 ⁇ ), orthophosphates (P0 4 3 ⁇ , HP0 4 2" , H 2 P0 4 ⁇ ), hypophosphates (H 2 P 2 0 6 2 ), metaphosphates (P0 3 ⁇ ) or pyrophosphates (P 2 0 7 4 ⁇ ), and a cation, preferably selected from ammonium, such as R 4 N + , R 3 NH + , R 2 NH 2 + , RNH 3 + , NH 4 + , wherein R is generally a linear or branched Ci to C 6 alkyl group, sodium (Na + ) or calcium (Ca 2+ ).
• the phosphorus source is phosphoric acid.
• the phosphoric acid is used as an aqueous solution, usually at a concentration by weight of between 50 and 95%, preferably at 70 to 85% by weight.
• the phosphorus source can be added together with the quaternary ammonium salt and/or together with the cationic copolymer and/or separately from the quaternary ammonium salt and the cationic copolymer.
• the total amount of phosphorus source is advantageously from 50 % to 400 %, preferably from 50 % to 200%, more preferably from 100 % to 200% by weight of the total weight of the quaternary ammonium salt and cationic copolymer.
• the relative quantities of DMA-Epi and Phosphorus source is about 20 to 30% by weight of DMA-Epi and 35 to 60% preferably 35 to 50% by weight of phosphorus source, the rest being water.
• the relative quantities of DHT and Phosphorus source is about 30 to 60% by weight of DHT and 5 to 30%, preferably 10 to 30% and more preferably 15 to 25% by weight of phosphorus source, the rest being water and/or alcohols like ethanol or isopropanol.
• phosphorus source in particular phosphoric acid is added separately from the quaternary ammonium salt and the cationic copolymer, it is in the form of an aqueous solution of phosphoric acid at 50 and 95%, preferably at 70 to 85% by weight.
• a particularly preferred embodiment consists in the use of 2 or 3 solutions:
• a hydro-alcoholic solution of quaternary ammonium salt with a phosphorus source preferably a hydro-alcoholic solution of DHT with phosphoric acid,
• An aqueous solution of cationic (co)polymer with a phosphorus source preferably an aqueous solution of DMA-Epi with phosphoric acid,
• an aqueous solution of phosphorus source, preferably phosphoric acid, to clarify sugar cane juice during the production of crystal or raw sugar.
• the quantities of each of the 2 or 3 solutions are the following:
• a hydro-alcoholic solution of quaternary ammonium salt with a phosphorus source preferably a hydro-alcoholic solution of DHT with phosphoric acid
• concentrations of each of the 2 or 3 solutions are the following:
• an hydro-alcoholic solution comprising from 30 to 60% of quaternary ammonium salt with 5 to 30% preferably 10 to 30% of a phosphorus source, preferably a hydro- alcoholic solution of 40 to 60% of DHT with 5-30% preferably 10 to 30% of an aqueous solution of phosphoric acid at a concentration by weight of between 50 and 95% by weight, - an aqueous solution comprising from 40 to 60% of an aqueous solution of cationic (co)polymer at a concentration by weight of between 50 and 70%, with 35 to 60%, preferably 40 to 60% of a phosphorus source, preferably an aqueous solution of 40 to 60% of DMA-Epi at a concentration of 50 to 70% with 40 to 60% of an aqueous solution of phosphoric acid at a concentration by weight of between 50 and 95%,
• an aqueous solution of phosphorus source preferably an aqueous solution of phosphoric acid at a concentration by weight of between 50 and 95%, preferably at 70 to 85% by weight.
• a hydro-alcoholic solution comprising from 30 to 60% of quaternary ammonium salt with 5 to 30%, preferably 10 to 30% of a phosphorus source, preferably a hydro-alcoholic solution of 30 to 60%, preferably 40 to 60% of DHT with 5 to 30% preferably 10 to 30% of an aqueous solution of phosphoric acid at a concentration by weight of between 50 and 95% by weight,
• aqueous solution comprising from 40 to 60% of an aqueous solution of cationic (co)polymer at a concentration by weight of between 50 and 70%, with 35 to 60% preferably 40 to 60% of a phosphorus source, preferably an aqueous solution of 40 to 60% of DMA-Epi at a concentration of 50 to 70% with 40 to 60% of an aqueous solution of phosphoric acid at a concentration by weight of between 50 and 95%,
• aqueous solution of phosphorus source preferably an aqueous solution of phosphoric acid at a concentration by weight of between 50 and 95%, preferably at 70 to 85% by weight.
• the invention provides a process for producing crystal or raw sugar from sugar cane juice comprising the following steps:
• sugar cane is selected either by hand or mechanized cutting, both with positive aspects. Mechanical harvesting equipment is capable of either cutting the intact cane stalk or chopping the cane.
• the manually cutting avoids the introduction of foreign matter commonly carried into the processing mill along with the sugar cane.
• the foreign matter often comprising ten percent or more of the sugar cane weight, primarily consists of soil, sludge, ash, leaves, minerals and cane tops.
• the introduction of the foreign matter has the undesirable effect of altering the natural flavor of subsequently extracted sugar cane juice.
• step (a) the cut sugar cane stalks can be subjected to a standard washing step to remove the foreign matter mentioned above and to reduce impurities on the surface of the stalks. Subsequently, the sugar cane stalks are generally reduced into smaller individual pieces either with the use of rotating knives or hammer mill shredders and leaves and nodes are advantageously removed.
• the sugar cane juice extraction includes any conventional extraction means suitable for breaking sugar cane cells, these means being well known by a person skilled in the art, such as crushing by tandem mills and extraction by diffusion.
• a tandem mill is a special type of modern rolling mill where rolling is done in one pass and there are several stands (sets of rolls).
• the sugar cane stalks are conveyed through a standard rolling mill to extract the sugar cane juice, as is well known to those skilled in the art, at a temperature from 30°C to 90°C, more preferably from 60°C to 85°C.
• the sugar cane juice obtained by the extraction step (a) described above has a pH level between 4 and 6, 10 to 30 % by weight of sucrose, 60 to 80 % by weight of water and 5 to 20 % by of insoluble materials and 10 to 30 % by weight of soluble solids.
• the sugar cane juice obtained by the extraction step (a) described above has a pH level between 4.5 and 5.5, 13 to 22 % by weight of sucrose, 68 to 76 % by weight of water and 8 to 16% by of insoluble materials and 18 to 25 % by weight of soluble solids.
• the process for producing crystal or raw sugar from sugar cane juice comprises a clarification of sugar cane juice wherein a quaternary ammonium salt and a cationic (co)polymer are added before, during or just after the clarification step (b).
• the quaternary ammonium salt is advantageously as described above according to the various embodiments.
• the quaternary ammonium salt is advantageously solubilized or dispersed in water or in an organic solvent, preferably ethanol or isopropanol, before its addition in the clarification step (b).
• the quaternary ammonium salt can be added in the amount described above.
• the cationic (co)polymer is as described above according to the various embodiments.
• the cationic (co)polymer can be added in the amounts described above.
• the clarification step is advantageously a phosphatation step.
• a phosphorus source is thus also added before, during or just after the clarification step.
• the phosphorus source is as described above according to the various embodiments.
• the phosphorus source can be added in the amounts described above.
• the quaternary ammonium salt, the cationic (co)polymer and optionally the phosphorus source are added either as a homogeneous blend, or separately but simultaneously, or separately and at different stages before, during or just after the clarification step (b).
• from 3 to 25 % of the total amount of phosphorous source is added with the quaternary ammonium salt, from 10 to 70 % of the total amount of phosphorous source is added with the cationic (co)polymer and from 0 to 80 % of the total amount of phosphorous source is added separately but simultaneously before, during or just after the clarification step (b).
• the clarification step (b) comprises pre-heating (bl), pH correction (b2) and heating (b3) steps.
• step (bl) the sugar cane juice is pre-heated preferably at a temperature from 40 °C to 75 °C, more preferably from 60 °C to 70 °C. While pre-heating is conducted, in order to facilitate the following chemical reactions and to improve the precipitation of colloids and finely dispersed matter from the clarified sugar cane juice, the juice is advantageously subjected to the pH correction step (b2).
• the standard procedure in sugar mills is to add any source of lime, but calcium oxide, also referred to as lime milk, is preferred.
• the addition of lime raises the pH and has the purpose of forming calcium phosphate precipitate, which upon sedimentation carries with it the impurities present in the juice.
• step (b2) calcium oxide or lime milk is advantageously added to the sugar cane juice in a sufficient amount to bring the pH level of the juice to 6.0 to 8.0, preferably 6.8 to 7.4, more preferably 6.8 to 7.2.
• the amount of calcium oxide used in the present invention is reduced when compared with existing processes. Minimizing the quantity of additives, such as calcium oxide, during the clarification, is essential for maintaining the natural flavor of the sugar cane juice and consequently in the final product.
• step (b3) the sugar cane juice is heated, in a second heating stage, preferably at a temperature from 90 °C to 120 °C, more preferably from 98 °C to 110 °C.
• Steps (bl) and (b3) are performed using standard heating equipment, as it is well known in the sugar mill industry.
• the quaternary ammonium salt, the cationic (co)polymer and optionally the phosphorus source are added during the steps bl, b2 and/or b3.
• the quaternary ammonium salt, the cationic (co)polymer and optionally the phosphorus source are added between steps b2 and b3 and even more preferably during step b3.
• the juice is subjected to evaporation step (c) to concentrate the juice.
• the clarified juice is generally transferred to standard evaporators and preferably heated at a temperature from 60 °C to 95 °C, more preferably from 80 °C to 85 °C.
• the juice is subsequently extracted from the evaporators at a soluble solid content of 50 to 70 °Brix, preferably at 55 to 65 "Brix. Crystallization
• the clarified sugar cane juice is directed to the subsequent crystallization step (d), which is generally carried out in a vacuum pan to form solid crystals.
• the juice is boiled preferably at a temperature from 50 °C to 90 °C , more preferably from 60 °C to 75 °C and under vacuum which causes the development and growth of solid crystals and the outcome called "massecuite" (mixture of crystals and mother liquor, also called molasses, resulting from the crystallization).
• step (e) the crystal or raw sugar and molasses obtained from the crystallization are then separated after a centrifugation and dried preferably at a temperature from 65 °C to 95 °C, more preferably from 70 °C to 80 °C.
• the process for producing crystal or raw sugar consists in the following steps:
• quaternary ammonium salt, a cationic copolymer and optionally a phosphorous source are added before, during or just after the clarification step.
• the process according to the invention is sulfur free, which means that no sulfur compound or derivative is added during the process.
• the process according to the invention does not contain carbon dioxide addition step.
• carbon dioxide addition step very few C02 amounts can be dissolved in water but we mean that no C02 volunteer addition is performed during the process according to the invention.
• the resulting crystal sugar obtained according to the invention has a degree of coloration between 50 and 400 ICUMSA units, preferably 90 to 150 ICUMSA units.
• the resulting raw sugar obtained according to the invention has a degree of coloration between 400 and 1200 ICUMSA units, preferably 700 to 900 ICUMSA units.
• the present invention provides advantages over existing processes to obtain crystal or raw sugar.
• the invention proposes an improved sugar cane juice clarification process by adding a quaternary ammonium salt and a cationic (co)polymer at the beginning of the process. This process presents an increased decolorizing performance, reducing the sugar color leaving no trace of chemicals in the final product. Crystal and raw sugars produced using the process according to the invention has a low degree of coloration and it is acceptable in food, pharmaceutical and beverage industries.
• the invention also provides a kit comprising:
• a phosphorous source optionally a phosphorous source.
• the quaternary ammonium salt is advantageously corresponding to formula I and preferred embodiments above described, it is preferably dimethyl-dioctadecylammonium chloride.
• the cationic (co)polymer is advantageously corresponding to the preferred embodiments above described; it is preferably a cationic copolymer of dimethylamine and epichlorohydrin (DMA-Epi).
• DMA-Epi dimethylamine and epichlorohydrin
• the optional phosphorous source of the kit it is possible to use one of the phosphorous sources described above in the description of the invention. It is preferably phosphoric acid.
• the kit advantageously comprises the 2 or 3 following solutions:
• an hydro-alcoholic solution comprising from 30 to 60% of quaternary ammonium salt with 5 to 30% preferably 10 to 30% of a phosphorus source, preferably a hydro- alcoholic solution of 40 to 60% of DHT with 5 to 30% preferably 10 to 30% of ah aqueous solution of phosphoric acid at a concentration by weight of between 50 and 95% by weight,
• an aqueous solution comprising from 40 to 60% of an aqueous solution of cationic (co)polymer at a concentration by weight of between 50 and 70%, with 35 to 60% preferably 40 to 60% of a phosphorus source, preferably an aqueous solution of 40 to 60% of DMA-Epi at a concentration of 50 to 70% with 40 to 60% of an aqueous solution of phosphoric acid at a concentration by weight of between 50 and 95%, - optionally an aqueous solution of phosphorus source, preferably an aqueous solution of phosphoric acid at a concentration by weight of between 50 and 95%, preferably at 70 to 85% by weight.
• the kit preferably comprises the 3 solutions above.
• the kit is usable in the process according to the present invention.
• DMA-Epi copolymer 150 ppm by weight of sugar solids
• the food additive is used as a decolorizing agent and/or flocculant in the clarification of refinery sugar liquors and juices. It is added only at the defecation/clarification stage of sugar liquor refining at a concentration not to exceed 150 parts per million of copolymer by weight of sugar solids.
• DHT 700 ppm by weight of sugar solids
• the ICUMSA color for the mixed and decanted juices was determined by measuring absorbance of the juices solutions at 420 nm, and calculated by the equation below:
• A is the absorbance measured at 420 nm
• b is the cell length
• C represents the concentration (g/100 mL) of the solution.
• the juice turbidity was expressed as the difference between the measurements at 720 nm before and after the sample filtration through the 0.45 ⁇ membrane. Turbidity before and after filtration was calculated by the equation below:
• Turbidity -—— — x 1000
• T is the transmittance measured at 720 nm
• b is the cell length
• the clarification performance was verified by clarification tests in order to evaluate the efficiency of the sugar cane juice treatment.
• DHT Blend 1 is a solution comprising 53.3 % by weight of dimethyldioctadecylammonium chloride ("DHT"), solubilized in ethanol (75/25), 25.9 % by weight of an aqueous solution of phosphoric acid at a concentration of 85 % by weight, 7.2 % by weight of isopropanol and 13.6 % by weight of anhydrous ethanol.
• DHT dimethyldioctadecylammonium chloride
• phosphoric acid a concentration of 85 % by weight
• the ratio between the dimethyldioctadecylammonium chloride and the phosphoric acid should be around 1.5 to 2.
• composition named herein "DMA-Epi Mix 1" is a solution comprising 50 % by weight of a 50 % by weight aqueous solution of dimethylamine-epichlorohydrin copolymer, and 50 % by weight of an aqueous solution of phosphoric acid at a concentration of 85 % by weight.
• the ratio between the dimethylamine-epichlorohydrin copolymer and the phosphoric acid should be around 0.3 to 1.
• Lime was added to the mixed juice in a sufficient amount to bring the pH to 6.8 - 7.2 and the mixture was heated at a temperature from 98 °C to 105 °C for 30 seconds.
• Anionic polyacrylamides of high molecular weight (“Polymer”) were also added to the mixture and then the treated juice was stored for 10 minutes. After that a sample of the supernatant was withdrawn for analysis.
• Turbidity values for clarified juices treated with DHT Blend and/or DMA-Epi Mix were better than the one obtained with sulfitation.
• compositions were dosed in a fresh mixed juice after the pre-heating step. Subsequently, phosphoric acid was added, in a way that the maximum authorized amount of each clarifying agent according to FDA was reached.
• DHT Blend 2 is a solution comprising 53 % by weight of dimethyldioctadecylammonium chloride ("DHT"), solubilized in ethanol (75/25), 40% by weight of anhydrous ethanol, 7 % by weight of an aqueous solution of phosphoric acid at a concentration of 85 % by weight.
• DHT dimethyldioctadecylammonium chloride
• the ratio between the dimethyldioctadecylammonium chloride and the phosphoric acid should be around 5-8.
• composition named herein "DMA-Epi Mix 2" is a solution comprising 40 % by weight of a 60 % by weight aqueous solution of dimethylamine-epichlorohydrin copolymer, and 60 % by weight of an aqueous solution of phosphoric acid at a concentration of 85 % by weight.
• the ratio between the dimethylamine-epichlorohydrin copolymer and the phosphoric acid should be around 0.3-1.
• Lime was added to the mixed juice in a sufficient amount to bring the pH to 6.8 - 7.2 and the mixture was heated at a temperature from 98 °C to 105 °C for 30 seconds.
• Anionic polyacrylamides of high molecular weight (“Polymer”) were also added to the mixture and then the treated juice was stored for 10 minutes. After that a sample of the supernatant was withdrawn for analysis.
• the ICUMSA color was measured according to the method described above.
• EXAMPLE 3 Crystal sugar production To evaluate the performance of the compositions as clarifying agents an industrial trial was performed and the results were compared to sulfitation. Color of juice, syrup and sugar were measured to control the clarification efficiency during the process.
• the ICUMSA color of the juices was determined by measuring absorbance of the solutions at 420 nm, as explained above.
• the industrial trial consisted in 12 days of test. It was performed with dosages of 61 ppm of active content of "DHT Blend 2", 30 ppm of active content of "DMA-Epi Mix 2", and 150 ppm of H3P04. During the trial the proposed solution performed better than sulfitation, with color reduction of 46 % on average on the decanted juice. In the period prior to the trial, sulfitation provided color reduction of 30 % on average on the decanted juice.

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