WO2017202289A1 - Composition solide pour la purification du sucre - Google Patents

Composition solide pour la purification du sucre Download PDF

Info

Publication number
WO2017202289A1
WO2017202289A1 PCT/CN2017/085456 CN2017085456W WO2017202289A1 WO 2017202289 A1 WO2017202289 A1 WO 2017202289A1 CN 2017085456 W CN2017085456 W CN 2017085456W WO 2017202289 A1 WO2017202289 A1 WO 2017202289A1
Authority
WO
WIPO (PCT)
Prior art keywords
compound
ammonium compound
quaternary ammonium
solid composition
sugar
Prior art date
Application number
PCT/CN2017/085456
Other languages
English (en)
Inventor
Zhaofei Chen
Shujing Cheng
Original Assignee
Rhodia Operations
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Rhodia Operations filed Critical Rhodia Operations
Priority to BR112018074072A priority Critical patent/BR112018074072A2/pt
Priority to CN201780032571.5A priority patent/CN109154029A/zh
Publication of WO2017202289A1 publication Critical patent/WO2017202289A1/fr

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C13—SUGAR INDUSTRY
    • C13B—PRODUCTION OF SUCROSE; APPARATUS SPECIALLY ADAPTED THEREFOR
    • C13B20/00—Purification of sugar juices
    • C13B20/14—Purification of sugar juices using ion-exchange materials
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C211/00—Compounds containing amino groups bound to a carbon skeleton
    • C07C211/62—Quaternary ammonium compounds
    • C07C211/63—Quaternary ammonium compounds having quaternised nitrogen atoms bound to acyclic carbon atoms
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C211/00—Compounds containing amino groups bound to a carbon skeleton
    • C07C211/62—Quaternary ammonium compounds
    • C07C211/64—Quaternary ammonium compounds having quaternised nitrogen atoms bound to carbon atoms of six-membered aromatic rings
    • C—CHEMISTRY; METALLURGY
    • C13—SUGAR INDUSTRY
    • C13B—PRODUCTION OF SUCROSE; APPARATUS SPECIALLY ADAPTED THEREFOR
    • C13B20/00—Purification of sugar juices
    • C13B20/02—Purification of sugar juices using alkaline earth metal compounds

Definitions

  • the present invention relates to a solid composition for sugar purification.
  • the solid composition can remove colour impurities in a sugar liquor or syrup.
  • Said solid composition comprises a quaternary ammonium compound and a phosphoric compound.
  • Fine sugars are normally obtained by purification of raw sugars or sugar juices.
  • raw sugars can be obtained from sugar juices by the processes of clarification, evaporation to a thick sugar syrup, and crystallization. Then the crystallized product can be dissolved in water so as to obtain sugar liquors. Subsequently, the sugar liquors can be further purified and processed for obtaining fine sugars having an acceptable standard of purity.
  • sugar syrups which are obtained from sugar juices, can be subject to the purification process without the step of crystallization of the raw sugars.
  • the whiteness of fine sugars is one important sugar quality criteria.
  • One aim of purification of the sugar liquor or syrup is to reduce the colour impurities, such that the purified sugar product has desired whiteness.
  • Various methods for reducing the colour impurities during the sugar purification process are known in the art.
  • One known method is phosphatation process which is aimed to produce calcium phosphate floc using phosphoric compound and lime, followed by a flocculation step by adding a polymer as flocculant.
  • One important modification to the phosphatation process is the application of colour precipitants, such as certain quaternary ammonium compounds. Quaternary ammonium compounds, which are cationic in nature, can improve the precipitation of anionic high molecular weight colour impurities, which can be more readily removed as flotation scum.
  • the quaternary ammonium compound and the phosphoric compound are added to sugar containing mixtures in separate streams.
  • US Patent No. 3,698,951 there is disclosed a method for removing colour impurities in sugar liquors by adding a quaternary ammonium compound, followed by addition of phosphoric acid.
  • the separate addition of the reagents is laborious and such method requires high carpex costs, energy and maintenance costs as well.
  • the quaternary ammonium compound is usually diluted in water before its addition to the sugar liquor or syrup.
  • the quaternary ammonium compound solution tends to have relatively high viscosity, which affect the efficiency of the addition and may sometimes cause blockage of the equipment.
  • high dilution factors are required so as to bring the viscosity of the solution of the quaternary ammonium compound to a sufficiently low level. This will waste water and costs.
  • a solid composition notably a solid composition for removing colour impurities in a sugar liquor or syrup, comprising at least a quaternary ammonium compound and a phosphoric compound; wherein the weight ratio of the quaternary ammonium compound to the phosphoric compound is in the range of 1: 1 to 1: 5.
  • the weight ratio of the quaternary ammonium compound to the phosphate compound is in the range of 1: 1 to 1: 3.
  • the quaternary ammonium compound has the general formula of:
  • R 1 , R 2 , R 3 , and R 4 which may be same or different, represent a saturated or unsaturated, straight or branched aliphatic group having from 1 to 30 carbon atoms, or an aromatic group;
  • X is an anion
  • y is the valence of X.
  • the quaternary ammonium compound has the general formula:
  • R 5 is an alkyl or hydroxyalkyl group containing from 8 to 22 carbon atoms
  • R 6 is a alkyl or hydroxyalkyl group containing from 1 to 4 carbon atoms
  • R 7 is R 5 or R 6 ;
  • X is an anion
  • y is the valence of X.
  • the quaternary ammonium compound may have the general formula:
  • R 8 is independently selected from C 1 -C 24 alkyl or hydroxyalkyl group
  • R 9 is independently selected from C 1 -C 4 alkyl or hydroxylalkyl group
  • R 10 is hydrogen, a C 1 -C 6 alkyl or a C 1 -C 6 hydroxyalkyl group
  • n is an integer from 0 to 5;
  • n is selected from 1, 2 and 3;
  • X is an anion
  • y is the valence of X.
  • the quaternary ammonium compound may have the general formula of:
  • R 11 and R 12 which may be the same or different, represent a straight or branched alkyl or hydroxyalkyl group having from 1 to 24 carbon atoms;
  • R 13 is a straight or branched alkyl or hydroxyalkyl group having from 1 to 8 carbon atoms
  • z 0 or an integer of 1 to 3;
  • Ph represents phenyl group
  • X is an anion
  • y is the valence of X.
  • the quaternary ammonium compound is selected from the group consisting of C 14 -C 18 alkyl dimethyl ammonium compound, di stearyl dimethyl ammonium compound, di palmityl dimethyl compound, di hexadecyl dimethyl ammonium compound, di octadecyl dimethyl ammonium compound, di oleyl dimethyl ammonium compound, di hydrogenated rapeseed alkyl dimethyl ammonium compound, and a mixture thereof.
  • the phosphoric compound is phosphoric acid.
  • a method for reducing colour impurities in a sugar liquor or syrup by adding a quaternary ammonium compound and a phosphoric compound to the sugar liquor or syrup; wherein the weight ratio of the quaternary ammonium compound to the phosphoric compound is in the range of 1: 1 to 1: 5.
  • the method further comprises the steps of:
  • the flocculating agent is a polyacrylamide.
  • the quaternary ammonium compound is present in an amount of from 100 to 500 ppm based on the weight of solid sugar in the sugar liquor or syrup.
  • a method for preparing a solid composition comprising a quaternary ammonium compound and a phosphoric compound; wherein the method comprises a step of mixing the quaternary ammonium compound and the phosphoric compound, the weight ratio of the quaternary ammonium compound to the phosphoric compound is in the range of 1: 1 to 1: 5.
  • any particular upper concentration, weight ratio or amount can be associated with any particular lower concentration, weight ratio or amount.
  • alkyl means a saturated hydrocarbon radical, which may be straight, branched or cyclic, such as methyl, ethyl, n-propyl, iso-propyl, n-butyl, sec-butyl, t-butyl, pentyl, n-hexyl, cyclohexyl.
  • hydroxyalkyl means an alkyl radical, which is substituted with a hydroxyl groups, such as hydroxymethyl, hydroxyethyl, hydroxypropyl, and hydroxydecyl.
  • aryl means a monovalent unsaturated hydrocarbon radical containing one or more six-membered carbon rings in which the unsaturation may be represented by three conjugated double bonds, which may be substituted one or more of carbons of the ring with hydroxy, alkyl, alkenyl, halo, haloalkyl, or amino, such as, for example, phenoxy, phenyl, methylphenyl, dimethylphenyl, trimethylphenyl, chlorophenyl, trichloromethylphenyl, aminophenyl.
  • aralkyl means an alkyl group substituted with one or more aryl groups, such as, for example, phenylmethyl, phenylethyl, triphenylmethyl.
  • the present invention provides a solid composition, notably a solid composition for reducing colour impurities in a sugar liquor or syrup, comprising at least a quaternary ammonium compound and a phosphoric compound; wherein the weight ratio of the quaternary ammonium compound to the phosphoric compound is in the range of 1: 1 to 1: 5.
  • the colour impurities in the sugar liquor or syrup notably include plant pigments, melanoidins, caramels and alkaline degradation products of fructose.
  • the solid composition has good storage stability and can provide excellent colour removal efficiency.
  • solid composition refers a composition in the form of a solid such as a powder, a particle, an agglomerate, a flake, a granule, a pellet, a tablet, a brick, a paste, a block such as a molded block, a unit dose, or another solid form known to those of skill in the art.
  • solid refers to the state of the composition under the expected conditions of storage and use of the composition. In general, it is expected that the composition will remain in solid form at ambient temperature (approximately 25°C) .
  • the solid composition will not flow perceptibly and will substantially retain its shape under moderate stress or pressure or mere gravity, as for example, the shape of a mold when removed from the mold, the shape of an article as formed upon extrusion from an extruder, and the like.
  • quaternary ammonium compound (also referred to as “quat” ) , as used herein, means a compound containing at least one quaternized nitrogen wherein the nitrogen atom is attached to four organic groups.
  • the quat may comprise one or more quaternized nitrogen atoms.
  • the quat comprises only one quaternized nitrogen atom.
  • sugar liquor or syrup means any liquor or syrup containing a sugar or a melted raw sugar.
  • the sugar is derived from a plant source, such as, a sugar cane, a sugar beet and a corn.
  • “Raw sugar” means a sugar which has been minimally processed and which contains soluble and insoluble impurities.
  • the raw sugar can be obtained from sugarjuices by the processes of clarification, evaporation to a thick sugar syrup, and crystallization. Then the crystallized product can be dissolved in water so as to obtain the sugar liquors, which is also called “melter liquor” .
  • sugar syrups which are obtained from sugar juices, can be used as the feedstock for the sugar refining process.
  • the quat may have the general formula of:
  • R 1 , R 2 , R 3 , and R 4 which may be same or different, represents a saturated or unsaturated, straight or branched aliphatic group having from 1 to 30 carbon atoms, or an aromatic group, such as aryl or aralkyl group;
  • X is an anion, for example halide, such as Cl or Br, sulphate, alkyl sulphate, nitrate or acetate, preferably, X is chloride or methylsulfate;
  • y is the valence of X.
  • the aliphatic group as defined in general formula (I) may comprise hetero atoms such as oxygen, nitrogen, sulphur and halogens.
  • the aliphatic group comprises at least an ester or amide function.
  • the quat is an alkyl quat which has the general formula:
  • R 5 is an alkyl or hydroxyalkyl group containing from 8 to 22 carbon atoms, such as C 8 H 17 , C 10 H 21 , C 12 H 25 , C 14 H 29 , C 16 H 33 , C 18 H 37, preferably, R 5 contains from 12 to 20 carbon atoms;
  • R 6 is an alkyl or hydroxyalkyl group containing from 1 to 4 carbon atoms, such as methyl, ethyl and propyl group, preferably R 6 is methyl;
  • R 7 is R 5 or R 6 ;
  • X is an anion, for example halide, such as Cl or Br, sulphate, alkyl sulphate, nitrate or acetate, preferably, X is chloride or methylsulfate; y is the valence of X.
  • the quat according to general formula (II) is a dialkyl dimethyl quat.
  • the quat of general formula (II) include C 14 -C 18 alkyl dimethyl ammonium compound (such as DHT21 sold by the Solvay Company) , di tallow alkyl dimethyl ammonium compound, di stearyl dimethyl ammonium compound, di palmityl dimethyl compound, di hexadecyl dimethyl ammonium compound, di octadecyl dimethyl ammonium compound, di oleyl dimethyl ammonium compound, di hydrogenated rapeseed alkyl dimethyl ammonium compound.
  • C 14 -C 18 alkyl dimethyl ammonium compound such as DHT21 sold by the Solvay Company
  • di tallow alkyl dimethyl ammonium compound such as DHT21 sold by the Solvay Company
  • di tallow alkyl dimethyl ammonium compound such as DHT21 sold by the Solvay Company
  • the quat has the general formula:
  • R 8 is independently selected from C 1 -C 24 alkyl or hydroxyalkyl group
  • R 9 is independently selected from C 1 -C 4 alkyl or hydroxylalkyl group
  • R 10 is hydrogen, a C 1 -C 6 alkyl or a C 1 -C 6 hydroxyalkyl group
  • n is an integer from 0 to 5;
  • n is selected from 1, 2 and 3;
  • X is an anion, for example halide, such as Cl or Br, sulphate, alkyl sulphate, nitrate or acetate, preferably, X is chloride or methylsulfate;
  • y is the valence of X.
  • the quat may have the general formula:
  • R 8 , R 9 , T, n, X and y are as defined in general formula (III) .
  • TET Di (tallowcarboxyethyl) hydroxyethyl methyl ammonium methylsulfate
  • TEO Di (oleocarboxyethyl) hydroxyethyl methyl ammonium methylsulfate
  • TEHT Di (hydrogenated tallow-carboxyethyl) hydroxyethyl methyl ammonium methylsulfate
  • TEP Di (palmiticcarboxyethyl) hydroxyethyl methyl ammonium methylsulfate
  • DEEDMAC Dimethylbis [2- [ (1-oxooctadecyl) oxy] ethyl] ammonium chloride.
  • the quat has the general formula of:
  • R 11 and R 12 which may be the same or different, represents a straight or branched alkyl or hydroxyalkyl group having from 1 to 24 carbon atoms;
  • R 13 is a straight or branched alkyl or hydroxyalkyl group having from 1 to 8 carbon atoms, preferably from 1 to 3 carbon atoms;
  • Ph represents phenyl group, the phenyl group may have at least one substituent selected from the group consisting of halide, nitrite, and sulphate on any available position;
  • X is an anion, for example halide, such as Cl or Br, sulphate, alkyl sulphate, nitrate or acetate, preferably, X is chloride or methylsulfate;
  • y is the valence of X.
  • Examples of the quats of general formula (V) include di stearyl methyl benzyl ammonium compound, di tallow alky methyl benzyl ammonium compound, di palmityl methyl benzyl compound, di hexadecyl methyl benzyl ammonium compound, di octadecyl methyl benzyl ammonium compound.
  • the solid composition may comprise a single quat or a mixture of more than one quats.
  • the phosphoric compound may be phosphoric acid or a phosphate compound.
  • Suitable phosphate compounds include, but not limited to tripolyphosphates, prophosphates, hexametaphophates, trisodium phosphates, sodium phosphate monobasic, calcium phosphate monobasic, ammonium phosphate monobasic, sodium phosphate dibasic, ammonium phosphate dibasic or any water-soluble phosphate salt which will not substantially decrease the pH of the sugar syrup or sugar liquor is expected to be within the purview of this invention.
  • the phosphoric compound is phosphoric acid.
  • the solid composition may further comprise water and an organic solvent, such as ethanol and isopropanol.
  • the solid composition may further comprise a polycationic polymer.
  • Suitable polycationic polymers include copolymer of di-allyl dimethyl ammonium chloride (DADMAC) and acrylic amide, copolymer of DADMAC and sodium acrylate, copolymer of DADMAC, acrylic amide and sodium acrylate, copolymer of dimethylamine-epichlorohydrin.
  • the solid composition may also comprise oxidant which can be used in sugar purification.
  • oxidants include hydrogen peroxide and hypochloride.
  • the weight ratio of the quat to the phosphoric compound which are comprised in the solid composition is in the range of 1: 1 to 1: 5 (including: 1: 1, 1: 1.1, 1: 1.2, 1: 1.3, 1: 1.4, 1: 1.5, 1: 1.6, 1: 1.8, 1: 2, 1: 2.2, 1: 2.4, 1: 2.6, 1: 2.8, 1: 3, 1: 4, 1: 5 etc., and all values and subranges between stated values as if explicitly written out) .
  • said weight ratio is in the range of 1: 1 to 1: 3, more preferably in the range of 1: 1.2 to 1: 3.
  • the weight ratio is calculated based on the weight of the active ingredients.
  • the solid composition may be prepared by blending the quat component and the phosphoric compound component by any mixing means well known to a person skilled in the art. Accordingly, the present invention also provides a method for preparing a solid composition comprising a quaternary ammonium compound and a phosphoric compound; wherein the method comprises a step of mixing the quaternary ammonium compound and the phosphoric compound, the weight ratio of the quaternary ammonium compound to the phosphoric compound is in the range of 1: 1 to 1: 5.
  • the quat is melt by heating it to a temperature above its melting point, such as about 65°C, then the phosphoric compound can be added to the quat with agitation, preferably with heating. Subsequently, the mixture may be cooled to ambient temperature for solidifying the composition.
  • the present invention provides a method for reducing colour impurities in a sugar liquor or syrup by adding a quaternary ammonium compound and a phosphoric compound to the sugar liquor or syrup; wherein the weight ratio of the quaternary ammonium compound to the phosphoric compound is in the range of 1: 1 to 1: 5.
  • the quaternary ammonium compound and the phosphoric compound may be added to the sugar liquor or syrup at the same time or premixed and added as a blend.
  • the present invention also provides a method for reducing colour impurities in a sugar liquor or syrup by using the solid composition described herein. Notably, the method comprises the steps of:
  • the solid composition may be dissolved or dispersed in water, optionally with organic solvents.
  • concentration of the quat in such solution or dispersion is from 5 wt%to 30 wt%, more preferably from 10 wt%to 20 wt%.
  • the solution or dispersion that contains the quat and the phosphoric compound may be added in the sugar liquor or syrup in a reaction tank with metering pump and agitation apparatus, which brings the quat into contact with the colour impurities.
  • the reaction is conducted at a temperature of 70-90°C, preferably 80-85°C.
  • the precipitate formed in this reaction is initially very finely divided and can hardly be observed with the naked eye; but its presence can be revealed by measurement of the optical properties of the liquor, for example by measuring the optical density at 420 nm, using a spectrophotometer.
  • such fine precipitate can be removed by filtration, using a filter medium having sufficiently small porosity.
  • One advantage of the present invention is that it allows the quat and the phosphoric compound being conveniently added to the sugar liquor or syrup in a single stream, which can save time and costs. Also, the viscosity of a diluted aqueous solution of the solid composition is lower compared to a solution containing quat alone at the same quat concentration. This is particularly advantageous as lower viscosity of the dilution aqueous solution allows rapid and sufficient mixing of the quat with the sugar liquor or syrup, which can enhance the efficiency of the reaction between the quat and the colour impurities. In addition, the melting point of the solid composition is lower than that of a quat solid, energy can thus be saved by using the solid composition when melting the colour precipitate due to lowertemperature and shorter heating time required.
  • the effective dose amount of the solid composition can be readily determined by a person skilled in the art. Generally, the dose amount of the solid composition is from about 200 to about 2000 ppm based on the weight of the solid sugar in the sugar liquor or syrup. Preferably, the dose amount of the solid composition is from about 400 to about 1000 ppm based on the weight of the solid sugar in the sugar liquor or syrup.
  • the method may further comprise the steps of:
  • the flocculant precipitate is calcium phosphate.
  • lime-based compound used herein refers to calcium-containing compound which can be used to neutralize the solution acidity and form precipitating insoluble calcium phosphates in the sugar liquors or syrups with the phosphoric compounds.
  • Suitable lime-based compounds include, but not limited to, calcium hydroxide, either as slurry with water (milk of lime) and lime succrate.
  • the lime-based compound may be added to the sugar liquor or syrup in a sufficient amount to raise the pH of the sugar liquor or syrup to be between 6 and 8, preferably between 6.8 and 7.2.
  • a flocculating agent may be added to the sugar liquor or syrup to increase the size of precipitate scum comprising most of calcium phosphate coagulum and other colour impurities precipitated by incorporating with the quat.
  • the flocculating agent is an anionic polyeletrolyte, such as polyacrylate, polyacrylamide, preferably polyacrylamide.
  • the polyacrylamide may be comprised in an amount of about 5 to about 30 ppm based on the weight of the solid sugar in the sugar liquor or syrup.
  • the polyacrylamide is present in an amount of about 10 to about 25 ppm based on the weight of the solid sugar in the sugar liquor or syrup.
  • the polyacrylamide used in the present invention preferably has an average Molecular Weight of from 12,000,000 to 30,000,000 Daltons. More preferably, the polyacrylamide has an average Molecular Weight of 22,000,000 Daltons.
  • the flocculant precipitate containing the colour impurities can be removed from the sugar liquor or syrup by a physical separation method including flotation such as air-flotation, filtration and the like.
  • a preferred separation method for the present invention is the air-flotation method, for which there is an additional step of micro aeration before the step of adding the flocculating agent.
  • the micro aeration may take place to produce an aerated sugar liquor or syrup. This step can either perform in a reaction tank with a stirring device or using an air compressor.
  • the air trapped scums to float in the sugar liquor or syrup can be then removed from the liquor surface by a skimming device, such as a scrapper.
  • the colour value of the sugar product can be reduced to 15-100 ICUMSA units, more typically, 20-50 ICUMSA units.
  • Di-alkyl quat DHT21; C 14 -C 18 alkyldimethyl ammonium chloride (CAS No. 68002-59-5) ; from the Solvay Company
  • Mono-alkyl quat octadecyl trimethyl ammonium chloride (CAS No. 112- 03-8) ; from the Solvay Company
  • Benzyl quat di C 14 -C 18 alkyl methyl benzyl ammonium chloride (CAS No. 61789-73-9) ; from the Solvay Company
  • Solid blends were prepared by mixing DHT21 (from the Solvay Company) and phosphoric acid, wherein the weight ratios of the DHT21 to the phosphoric acid in such samples were shown in Table 1 below.
  • the solid blends were melt at 60°C and subsequently diluted in hot water to obtain solutions with a concentration of DHT21 being 10 wt% (active) .
  • Raw sugars, obtained from sugar cane juice by simple lime treatment, were dissolved in hot water to obtain a sugar liquor of 60-65 Brix.
  • the sugar liquor had a sugar value of 500-1500 ICUMSA units.
  • the sugar liquor was heated to 80-85°C, subsequently, the diluted solution of the blend was added in the sugar liquor and stirred for 15 mins.
  • the dose amount of quat was 300 ppm based on the weight of the solid sugar in the sugar liquor.
  • lime succrate was added in the mixture, with stirring, to bring the pH value of the mixture to 6.9-7.0.
  • the sugar liquor was transferred to a separatory funnel and a PAM solution (0.1 wt%) was added in the sugar liquor (the dose amount of PAM was 15-20 ppm based on the solid sugar content) .
  • the sugar liquor was shaken and the separatory funnel was immerged in boiling water bath for 10 mins. The precipitate containing the colour impurities floated up to the top of the sugar liquor. 40 ml of the clear sugar liquor were collected from the bottom of the funnel for colour value tests.
  • the collected sugar liquor was diluted in water (final concentration of the sugar was 35-40 Brix) .
  • the pH value of the solution was adjusted to 7.0 by using diluted HCl or NaOH solution.
  • the solution was filtered with a filter paper (porous size 0.45 ⁇ m) and the absorption of the solution was detected at 420 nm with UV/Vis spectrometer.
  • the colour value (COL) was calculated according to the formula :
  • A420 is expressed as absorbance of the sugar liquor at 420 nm wave length
  • B is the brix of the sugar liquor at 25°C (detection of brix of the sugar liquor is performed with Abbe-Refractometer, unit is °Bx) ;
  • L is the length of the cuvette
  • ⁇ is the density of the sugar liquor.
  • the colour removal efficiency of the solid composition was affected by the weight ratio of the quat to the phosphoric compound.
  • the solid compositions are more effective in reducing the colour impurities when the weight ratio is no less than 1: 1.
  • a solid blend containing DHT21 and phosphoric acid were prepared as described above.
  • the solid blend was incubated in an oven at 54°C for four weeks.
  • the contents of DHT21 and phosphoric acid were titrated before and after the incubation, respectively.
  • Titration of the phosphoric acid was conducted, using NaOH, and phenolphthalein as the colour indicator. The procedure of such titration method is well known by a person skilled in the art.
  • Titration of DHT21 was conducted according to the methods described in Chinese National Standard GB/T 5174-2004. Results were shown in Table 3 below:
  • results showed that the solid composition according to the present invention can maintain the stability of its components after incubation at 50°C for up to 4 weeks. There was a slight decrease in the content of DHT21, which should be due to evaporation of organic solvents.
  • Solid DHT21 or solid blends of DHT21 and phosphoric acid were dissolved in water with the various DHT21 concentrations as shown in Table 4 below. Then the viscosity of the solutions was measured by using a Brookfield LVT viscometer at 100 rpm shearing speed (spindle #S2) . The measurement was done at ambient temperature, 40°C and 60°C, respectively. The unit of the viscosity is cP. S. Results are shown in Table 4 below:
  • Solid blends were prepared according to the procedure as described above and according to the formulations in Table 6 below. Either di-alkyl quat (DHT21) or mono-alkyl quat was used. The weight ratio of the quat compound and the phosphoric acid in the solid blends was 1: 1 (w/w) .
  • the solid blends were melt at 60°C and subsequently diluted in hot water to obtain solutions with a concentration of quat being 10 wt% (active) .
  • Raw sugars obtained from sugar cane juice by simple lime treatment, were dissolved in hot water to obtain a sugar liquor of 60-65 Brix.
  • the sugar liquor had a sugar value of 500-1500 ICUMSA units.
  • the sugar liquor was subject to phosphatation treatment as described above. Subsequently, the sugar liquor was transferred to a separatory funnel and a PAM solution (0.1 wt%) was added in the sugar liquor (the dose amount of PAM was 15-20 ppm based on the solid sugar content) .
  • the sugar liquor was shaken and the separatory funnel was immerged in boiling water bath for 10 mins. The precipitate containing the colour impurities floated up to the top of the sugar liquor. Floatation rate was determined at different time points after the separatory funnel was immerged in the boiling water bath.
  • the results are estimated by naked eye examination and the floatation rate is expressed by dividing the amount of flocculent participates floated to the top surface of the sugar liquor by total amount of flocculent participates occurring in the sugar liquor. Results are shown in Table 6 below.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Biochemistry (AREA)
  • Separation Of Suspended Particles By Flocculating Agents (AREA)
  • Paper (AREA)
  • Alcoholic Beverages (AREA)
  • Distillation Of Fermentation Liquor, Processing Of Alcohols, Vinegar And Beer (AREA)
  • Treatment Of Liquids With Adsorbents In General (AREA)

Abstract

L'invention concerne une composition solide pour éliminer des impuretés de couleur dans une liqueur ou un sirop de sucre et un procédé d'utilisation de cette composition solide, ladite composition solide comprenant au moins un composé d'ammonium quaternaire et un composé phosphorique.
PCT/CN2017/085456 2016-05-26 2017-05-23 Composition solide pour la purification du sucre WO2017202289A1 (fr)

Priority Applications (2)

Application Number Priority Date Filing Date Title
BR112018074072A BR112018074072A2 (pt) 2016-05-26 2017-05-23 composição sólida para a purificação do açúcar
CN201780032571.5A CN109154029A (zh) 2016-05-26 2017-05-23 用于糖纯化的固体组合物

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
CN2016083428 2016-05-26
CNPCT/CN2016/083428 2016-05-26

Publications (1)

Publication Number Publication Date
WO2017202289A1 true WO2017202289A1 (fr) 2017-11-30

Family

ID=60411040

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/CN2017/085456 WO2017202289A1 (fr) 2016-05-26 2017-05-23 Composition solide pour la purification du sucre

Country Status (3)

Country Link
CN (1) CN109154029A (fr)
BR (1) BR112018074072A2 (fr)
WO (1) WO2017202289A1 (fr)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US11787967B2 (en) 2020-07-13 2023-10-17 Advansix Resins & Chemicals Llc Branched amino acid surfactants for inks, paints, and adhesives
US11857515B2 (en) 2020-07-13 2024-01-02 Advansix Resins & Chemicals Llc Branched amino acid surfactants for use in healthcare products
US11897834B2 (en) 2020-07-09 2024-02-13 Advansix Resins & Chemicals Llc Branched amino acid surfactants

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3698951A (en) * 1967-09-29 1972-10-17 Tate & Lyle Ltd Sugar refining
CN101812546A (zh) * 2010-04-23 2010-08-25 广西大学 磷酸复合物脱色剂的制备及其应用方法

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US8486473B2 (en) * 2009-11-11 2013-07-16 Carbo-UA Limited Compositions and processes for improving phosphatation clarification of sugar liquors and syrups

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3698951A (en) * 1967-09-29 1972-10-17 Tate & Lyle Ltd Sugar refining
CN101812546A (zh) * 2010-04-23 2010-08-25 广西大学 磷酸复合物脱色剂的制备及其应用方法

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US11897834B2 (en) 2020-07-09 2024-02-13 Advansix Resins & Chemicals Llc Branched amino acid surfactants
US11787967B2 (en) 2020-07-13 2023-10-17 Advansix Resins & Chemicals Llc Branched amino acid surfactants for inks, paints, and adhesives
US11857515B2 (en) 2020-07-13 2024-01-02 Advansix Resins & Chemicals Llc Branched amino acid surfactants for use in healthcare products

Also Published As

Publication number Publication date
CN109154029A (zh) 2019-01-04
BR112018074072A2 (pt) 2019-03-06

Similar Documents

Publication Publication Date Title
WO2017202289A1 (fr) Composition solide pour la purification du sucre
US3926662A (en) Production of cane sugar
US9163293B2 (en) Compositions and processes for improving phosphatation clarification of sugar liquors and syrups
US20070237701A1 (en) Silica Sol and Process for Producing Same
RU2362764C2 (ru) Фенольные антиоксиданты в кристаллической форме
US3698951A (en) Sugar refining
US8784509B2 (en) Composition for enhancing the production of crystal agglomerates from a precipitation liquor
EP0787212B1 (fr) Procede de decoloration de solutions
CN102906279A (zh) 用于糖汁和糖浆澄清的组合物和方法
US8394202B2 (en) Method for manufacturing sugar from sugarcane
DE10326630A1 (de) Verwendung wässriger Dispersionen, enthaltend Ethylencopolymerwachse
US3508965A (en) Sugar purification
EP0689555B1 (fr) Polycocondensats a base d'acide aspartique, procedes de preparation et utilisation
AU753253B2 (en) Production of alumina
CN109154028B (zh) 减少糖液或糖浆中有色杂质的方法
KR101134502B1 (ko) 피틴산의 제조방법
CN102392081B (zh) 一种制糖专用絮凝剂及其制备方法
CN111039884A (zh) 一种品质稳定的造纸用液体荧光增白剂的制备方法
DE102017215243A1 (de) Verfahren zur Herstellung von funktionsverbessertem Carbokalk
CN101913691B (zh) 一种用于净水的天然絮凝剂的制备方法
Steindl et al. Syrup clarification for plantation white sugar to meet new quality standards
SU1824377A1 (ru) Способ извлечения лития из литийсодержащего раствора
Abdel-Razig et al. Effect of addition of separan at different concentrations as a flocculants on quality of sugar cane juice
EP0123647B1 (fr) Procédé pour empêcher la gélatination de solutions aqueuses de photoactivateurs
CN113039291A (zh) 用于纯化木糖的方法

Legal Events

Date Code Title Description
NENP Non-entry into the national phase

Ref country code: DE

121 Ep: the epo has been informed by wipo that ep was designated in this application

Ref document number: 17802135

Country of ref document: EP

Kind code of ref document: A1

REG Reference to national code

Ref country code: BR

Ref legal event code: B01A

Ref document number: 112018074072

Country of ref document: BR

ENP Entry into the national phase

Ref document number: 112018074072

Country of ref document: BR

Kind code of ref document: A2

Effective date: 20181123

122 Ep: pct application non-entry in european phase

Ref document number: 17802135

Country of ref document: EP

Kind code of ref document: A1