CN113150047A - Method for separating and extracting sucralose-6-acetate - Google Patents
Method for separating and extracting sucralose-6-acetate Download PDFInfo
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- CN113150047A CN113150047A CN202110452414.8A CN202110452414A CN113150047A CN 113150047 A CN113150047 A CN 113150047A CN 202110452414 A CN202110452414 A CN 202110452414A CN 113150047 A CN113150047 A CN 113150047A
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- FACOTAQCKSDLDE-YKEUTPDRSA-N [(2R,3R,4R,5R,6R)-6-[(2R,3S,4S,5S)-2,5-bis(chloromethyl)-3,4-dihydroxyoxolan-2-yl]oxy-3-chloro-4,5-dihydroxyoxan-2-yl]methyl acetate Chemical compound O[C@@H]1[C@@H](O)[C@@H](Cl)[C@@H](COC(=O)C)O[C@@H]1O[C@@]1(CCl)[C@@H](O)[C@H](O)[C@@H](CCl)O1 FACOTAQCKSDLDE-YKEUTPDRSA-N 0.000 title claims abstract description 37
- 238000000034 method Methods 0.000 title claims abstract description 20
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000007788 liquid Substances 0.000 claims abstract description 27
- 238000003756 stirring Methods 0.000 claims abstract description 27
- DKPFZGUDAPQIHT-UHFFFAOYSA-N Butyl acetate Natural products CCCCOC(C)=O DKPFZGUDAPQIHT-UHFFFAOYSA-N 0.000 claims abstract description 22
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000000967 suction filtration Methods 0.000 claims abstract description 22
- 238000010438 heat treatment Methods 0.000 claims abstract description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000005660 chlorination reaction Methods 0.000 claims abstract description 14
- 238000001816 cooling Methods 0.000 claims abstract description 14
- 238000004821 distillation Methods 0.000 claims abstract description 14
- 239000000706 filtrate Substances 0.000 claims abstract description 14
- 239000003960 organic solvent Substances 0.000 claims abstract description 14
- 238000004090 dissolution Methods 0.000 claims abstract description 11
- 238000000605 extraction Methods 0.000 claims abstract description 11
- 239000013078 crystal Substances 0.000 claims abstract description 9
- 239000007787 solid Substances 0.000 claims abstract description 8
- 239000012043 crude product Substances 0.000 claims abstract description 6
- 238000001035 drying Methods 0.000 claims abstract description 6
- 230000003472 neutralizing effect Effects 0.000 claims abstract description 3
- 239000000126 substance Substances 0.000 claims abstract description 3
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 27
- 239000000463 material Substances 0.000 claims description 15
- 239000002002 slurry Substances 0.000 claims description 9
- UOCLXMDMGBRAIB-UHFFFAOYSA-N 1,1,1-trichloroethane Chemical compound CC(Cl)(Cl)Cl UOCLXMDMGBRAIB-UHFFFAOYSA-N 0.000 claims description 7
- 239000000284 extract Substances 0.000 claims description 5
- 238000004321 preservation Methods 0.000 claims description 4
- FYSNRJHAOHDILO-UHFFFAOYSA-N thionyl chloride Chemical compound ClS(Cl)=O FYSNRJHAOHDILO-UHFFFAOYSA-N 0.000 claims description 4
- 102000004190 Enzymes Human genes 0.000 claims description 2
- 108090000790 Enzymes Proteins 0.000 claims description 2
- 239000002253 acid Substances 0.000 claims description 2
- 239000003513 alkali Substances 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 238000006386 neutralization reaction Methods 0.000 claims description 2
- 238000002360 preparation method Methods 0.000 claims description 2
- 239000006188 syrup Substances 0.000 claims description 2
- 235000020357 syrup Nutrition 0.000 claims description 2
- 238000002425 crystallisation Methods 0.000 abstract description 4
- 230000008025 crystallization Effects 0.000 abstract description 4
- 239000000047 product Substances 0.000 abstract description 4
- 239000003153 chemical reaction reagent Substances 0.000 abstract description 3
- 235000003599 food sweetener Nutrition 0.000 abstract description 2
- 238000011084 recovery Methods 0.000 abstract description 2
- 238000001953 recrystallisation Methods 0.000 abstract description 2
- 239000003765 sweetening agent Substances 0.000 abstract description 2
- 238000004042 decolorization Methods 0.000 abstract 2
- 229910052799 carbon Inorganic materials 0.000 abstract 1
- 238000001914 filtration Methods 0.000 abstract 1
- 239000004376 Sucralose Substances 0.000 description 12
- 235000019408 sucralose Nutrition 0.000 description 12
- BAQAVOSOZGMPRM-QBMZZYIRSA-N sucralose Chemical compound O[C@@H]1[C@@H](O)[C@@H](Cl)[C@@H](CO)O[C@@H]1O[C@@]1(CCl)[C@@H](O)[C@H](O)[C@@H](CCl)O1 BAQAVOSOZGMPRM-QBMZZYIRSA-N 0.000 description 12
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 3
- 238000005947 deacylation reaction Methods 0.000 description 3
- 239000012065 filter cake Substances 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 235000011837 pasties Nutrition 0.000 description 3
- 229920000642 polymer Polymers 0.000 description 3
- 239000006227 byproduct Substances 0.000 description 2
- 230000006196 deacetylation Effects 0.000 description 2
- 238000003381 deacetylation reaction Methods 0.000 description 2
- 230000020176 deacylation Effects 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 description 1
- 229930006000 Sucrose Natural products 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000032050 esterification Effects 0.000 description 1
- 238000005886 esterification reaction Methods 0.000 description 1
- 238000004128 high performance liquid chromatography Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000008267 milk Substances 0.000 description 1
- 235000013615 non-nutritive sweetener Nutrition 0.000 description 1
- CVHZOJJKTDOEJC-UHFFFAOYSA-N saccharin Chemical compound C1=CC=C2C(=O)NS(=O)(=O)C2=C1 CVHZOJJKTDOEJC-UHFFFAOYSA-N 0.000 description 1
- 235000019204 saccharin Nutrition 0.000 description 1
- 229940081974 saccharin Drugs 0.000 description 1
- 239000000901 saccharin and its Na,K and Ca salt Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000005720 sucrose Substances 0.000 description 1
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Classifications
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H13/00—Compounds containing saccharide radicals esterified by carbonic acid or derivatives thereof, or by organic acids, e.g. phosphonic acids
- C07H13/02—Compounds containing saccharide radicals esterified by carbonic acid or derivatives thereof, or by organic acids, e.g. phosphonic acids by carboxylic acids
- C07H13/04—Compounds containing saccharide radicals esterified by carbonic acid or derivatives thereof, or by organic acids, e.g. phosphonic acids by carboxylic acids having the esterifying carboxyl radicals attached to acyclic carbon atoms
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H1/00—Processes for the preparation of sugar derivatives
- C07H1/06—Separation; Purification
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Biochemistry (AREA)
- Biotechnology (AREA)
- General Health & Medical Sciences (AREA)
- Genetics & Genomics (AREA)
- Molecular Biology (AREA)
- Saccharide Compounds (AREA)
Abstract
The invention relates to the technical field of sweeteners, in particular to a method for separating and extracting sucralose-6-acetate, which comprises the following steps: neutralizing feed liquid obtained by chlorination reaction of sucrose-6-acetate to obtain chlorinated feed liquid, and distilling the chlorinated feed liquid under reduced pressure; adding pure water after distillation, stirring, and removing insoluble substances by suction filtration; adding active carbon into the filtrate for decolorization; after decolorization, the filtrate is extracted for multiple times by using butyl acetate and the extraction liquid is combined; distilling under reduced pressure to remove the organic solvent, adding butyl acetate, heating for dissolving, cooling to 0-10 ℃ for crystallization after complete dissolution, and performing suction filtration to obtain a crude product; dissolving the crude product in water, distilling under reduced pressure to remove residual organic solvent until solid is separated out, cooling, stirring, crystallizing, filtering, and drying to obtain refined crystal of sucralose-6-acetate. The method provided by the invention adopts recrystallization of the organic solvent and water, obviously improves the purity of the sucralose-6-acetate, effectively reduces the dosage of the organic reagent, and improves the recovery rate of the product to a certain extent.
Description
Technical Field
The invention relates to the technical field of sweeteners, and relates to a method for separating and extracting sucralose-6-acetate.
Background
Sucralose, also known as sucralose, saccharin or 4,1 ', 6' -trichloro-4, 1 ', 6' -trideoxy semi-milk sucrose, is a white powdery product with high sweetness, pure taste, long storage period and no calorie, and is a non-nutritive sweetener.
The industrial production of sucralose mainly comprises three steps, wherein the first step is esterification to obtain an intermediate sucrose-6-acetate, the second step is chlorination to produce the intermediate sucralose-6-acetate, and the last step is deacetylation to obtain sucralose. The sucrose-6-acetate is chloridized by Vilsmeier to generate sucralose-6-acetate, and side reactions occur in the chlorination reaction process to generate byproducts, such as non-6-position sucralose acetate and sucralose diacetate; if the subsequent deacetylation is directly carried out without purification, the byproduct of non-6-bit sucralose acetate and sucralose diacetate can also undergo deacylation reaction to generate sucralose with other structures, which is difficult to separate from sucralose, thereby affecting the product quality and increasing the subsequent production cost. The difficulty of separating the non-6-position sucralose acetate and the sucralose diacetate before deacylation is greatly reduced, so the separation and purification of the chlorinated material before deacylation are very important.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: provides a method for separating and extracting sucralose-6-acetate.
The technical scheme for solving the technical problems is as follows:
a method for separating and extracting sucralose-6-acetate is characterized by comprising the following steps:
(1) neutralizing a feed liquid obtained by chlorination reaction of sucrose-6-acetate to obtain a chlorinated feed liquid, and distilling the chlorinated feed liquid under reduced pressure to remove trichloroethane and N, N-dimethylformamide in the feed liquid;
(2) adding pure water after distillation, stirring, and removing insoluble substances by suction filtration; adding activated carbon into the filtrate, heating and stirring to decolor the feed liquid, and performing suction filtration to remove the activated carbon to obtain decolored filtrate;
(3) extracting the decolorized filtrate for multiple times by using butyl acetate, and combining the extract liquor after the extraction is finished; distilling under reduced pressure to remove organic solvent to obtain slurry material;
(4) adding butyl acetate into the slurry material, heating to dissolve the butyl acetate, cooling to 0-10 ℃ after complete dissolution, crystallizing, and performing suction filtration to obtain a sucralose-6-acetate crude product;
(5) adding water into the crude product of the sucralose-6-acetate for dissolving, carrying out reduced pressure distillation after complete dissolution to remove the residual organic solvent until white solid is separated out, cooling and stirring to ensure that the sucralose-6-ethyl ester is recrystallized and separated out, and carrying out suction filtration and drying to obtain the refined crystal of the sucralose-6-acetate.
Preferably, the preparation method of the chlorination solution in the step (1) is as follows: adding 4-5 times of N, N-dimethylformamide in mass ratio into sucrose-6-acetate solid or dry syrup synthesized by an enzyme method, fully dissolving, and then putting into a dropper; mixing trichloroethane and thionyl chloride, cooling to-10-0 ℃, slowly dropwise adding a sucrose-6-acetate solution dissolved in N, N-dimethylformamide in advance, controlling the temperature to be 0-10 ℃, preserving heat for 10-60 min after dropwise adding is finished, slowly heating to 60-80 ℃, preserving heat for 1-3 h, heating to 90-100 ℃ after heat preservation is finished, preserving heat for 1-4 h, and continuously heating to 105-120 ℃ after heat preservation is finished, and preserving heat for 1-3 h; and after the reaction is finished, adding alkali until the pH value is 8-9, and adding acid for neutralization to obtain a chlorination feed liquid.
Preferably, the mass of the pure water added in the step (2) is 5-10 times of that of the chlorination liquid, the stirring temperature is 50-65 ℃, and the stirring time is 10-100 min.
Preferably, the mass of the activated carbon added in the step (2) is 5-10% of that of the chlorination liquid, the stirring temperature is 40-60 ℃, and the stirring time is 10-100 min.
Preferably, the mass ratio of the total addition amount of butyl acetate for extraction to the chlorination feed liquid in the step (3) is 5-20: 1.
further, the mass ratio of the total addition amount of butyl acetate for extraction to the chloridized feed liquid in the step (3) is 10-15: 1.
preferably, the adding amount of the butyl acetate in the step (4) is 1-3 times of the mass of the slurry material, and the heating temperature is 50-80 ℃.
Further, the adding amount of the butyl acetate in the step (4) is 1.5-2 times of the mass of the slurry material, and the heating temperature is 60-80 ℃.
Preferably, the mass of the water added in the step (5) is 2.5-4 times of the mass of the crude crystal of the sucralose-6-acetate, and the heating temperature is 40-65 ℃.
The Chinese naming of the compound of the invention conflicts with the structural formula, and the structural formula is taken as the standard; except for obvious errors in the formula.
The method for separating and extracting the sucralose-6-acetate provided by the invention adopts recrystallization of the organic solvent and water, so that the purity of the sucralose-6-acetate is obviously improved to be more than 99.4%, the using amount of the organic reagent is effectively reduced, the extraction reagent can be recovered by reduced pressure distillation, and the cost is reduced; the recovery rate of the product is also improved to a certain extent.
Drawings
FIG. 1 is a hydrogen spectrum of sucralose-6-acetate obtained in the embodiment of the present application.
Detailed Description
The invention is illustrated but not limited by the following examples. The technical solutions protected by the present invention are all the simple replacements or modifications made by the skilled person in the art.
Example 1
Distilling 60g of sucrose-6-acetate chloride solution (containing 37.6g of sucralose-6-acetate) under reduced pressure to remove trichloroethane and N, N-dimethylformamide in the solution; adding 300g of pure water after distillation, stirring at 60 ℃ for 30 min; after stirring, removing insoluble carbon residue and part of high molecular polymer by suction filtration, adding 4g of activated carbon into the filtrate, stirring at 50 ℃ for 30min, decolorizing the feed liquid, and removing the activated carbon by suction filtration; and (3) extracting the filtrate for multiple times by using 750g of butyl acetate, combining the extract liquor after the extraction is finished, and distilling under reduced pressure to remove the organic solvent to obtain a pasty material. Adding 4 times of butyl acetate in mass into the slurry material, heating at 60 ℃ for dissolving, cooling to 0 ℃ for crystallization after complete dissolution, and performing suction filtration to obtain a crude crystal of sucralose-6-acetate; adding 3 times of water by mass into the crude sucralose-6-ethyl ester filter cake, dissolving at 50 ℃, carrying out reduced pressure distillation at 75 ℃ after complete dissolution to remove the residual organic solvent until white solid is separated out, cooling to 0 ℃, stirring to ensure that sucralose-6-ethyl ester is recrystallized and separated out, carrying out suction filtration and drying to obtain 20.3g of sucralose-6-acetate refined crystals, wherein the purity is 99.7% by high performance liquid chromatography detection.
Example 2
Distilling 60g of sucrose-6-acetate chloride solution (containing 36.8g of sucralose-6-acetate) under reduced pressure to remove trichloroethane and N, N-dimethylformamide in the solution; after distillation, 550g of pure water is added and stirred for 30min at 65 ℃; after stirring, removing insoluble carbon residue and part of high molecular polymer by suction filtration, adding 3g of activated carbon into the filtrate, stirring at 50 ℃ for 30min, decolorizing the feed liquid, and removing the activated carbon by suction filtration; the filtrate was extracted several times with 600g of butyl acetate, after the extraction was completed the extracts were combined and the organic solvent was removed by distillation under reduced pressure to obtain a paste material. Adding 2 times of butyl acetate by mass into the pasty material, heating at 60 ℃ for dissolving, cooling to 0 ℃ for crystallization after complete dissolution, and performing suction filtration; adding 3 times of water by mass into the crude sucralose-6-ethyl ester filter cake, dissolving at 50 ℃, carrying out reduced pressure distillation at 75 ℃ after complete dissolution to remove the residual organic solvent until white solid is separated out, cooling to 5 ℃, stirring to ensure that sucralose-6-ethyl ester is recrystallized and separated out, and carrying out suction filtration and drying to obtain 21.1g of sucralose-6-acetate refined crystals with the purity of 99.5 percent.
Example 3
Distilling 60g of sucrose-6-acetate chloride solution (containing 37.3g of sucralose-6-acetate) under reduced pressure to remove trichloroethane and N, N-dimethylformamide in the solution; adding 400g of pure water after distillation, stirring at 70 ℃ for 30 min; after stirring, removing insoluble carbon residue and part of high molecular polymer by suction filtration, adding 6g of activated carbon into the filtrate, stirring at 50 ℃ for 30min, decolorizing the feed liquid, and removing the activated carbon by suction filtration; the filtrate was extracted several times with 900g of butyl acetate, after the extraction was completed the extracts were combined and the organic solvent was removed by distillation under reduced pressure to obtain a paste material. Adding 1.5 times of butyl acetate into the pasty material, heating at 60 ℃ for dissolving, cooling to 0 ℃ for crystallization after complete dissolution, and performing suction filtration; adding 2.5 times of water by mass into the crude sucralose-6-ethyl ester filter cake, dissolving at 50 ℃, carrying out reduced pressure distillation at 75 ℃ after complete dissolution to remove the residual organic solvent until white solid is separated out, cooling to 0 ℃, stirring to ensure that sucralose-6-ethyl ester is recrystallized and separated out, and carrying out suction filtration and drying to obtain 20.4g of sucralose-6-acetate refined crystals with the purity of 99.4%.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various changes and modifications can be made without departing from the inventive concept of the present invention, and these changes and modifications are all within the scope of the present invention.
Claims (9)
1. A method for separating and extracting sucralose-6-acetate is characterized by comprising the following steps:
(1) neutralizing a feed liquid obtained by chlorination reaction of sucrose-6-acetate to obtain a chlorinated feed liquid, and distilling the chlorinated feed liquid under reduced pressure to remove trichloroethane and N, N-dimethylformamide in the feed liquid;
(2) adding pure water after distillation, stirring, and removing insoluble substances by suction filtration; adding activated carbon into the filtrate, heating and stirring to decolor the feed liquid, and performing suction filtration to remove the activated carbon to obtain decolored filtrate;
(3) extracting the decolorized filtrate for multiple times by using butyl acetate, and combining the extract liquor after the extraction is finished; distilling under reduced pressure to remove organic solvent to obtain slurry material;
(4) adding butyl acetate into the slurry material, heating to dissolve the butyl acetate, cooling to 0-10 ℃ after complete dissolution, crystallizing, and performing suction filtration to obtain a sucralose-6-acetate crude product;
(5) adding water into the crude product of the sucralose-6-acetate for dissolving, carrying out reduced pressure distillation after complete dissolution to remove the residual organic solvent until white solid is separated out, cooling and stirring to ensure that the sucralose-6-ethyl ester is recrystallized and separated out, and carrying out suction filtration and drying to obtain the refined crystal of the sucralose-6-acetate.
2. The method for separating and extracting sucralose-6-acetate according to claim 1, wherein the preparation method of the chlorination feed liquid in the step (1) is as follows: adding 4-5 times of N, N-dimethylformamide in mass ratio into sucrose-6-acetate solid or dry syrup synthesized by an enzyme method, fully dissolving, and then putting into a dropper; mixing trichloroethane and thionyl chloride, cooling to-10-0 ℃, slowly dropwise adding a sucrose-6-acetate solution dissolved in N, N-dimethylformamide in advance, controlling the temperature to be 0-10 ℃, preserving heat for 10-60 min after dropwise adding is finished, slowly heating to 60-80 ℃, preserving heat for 1-3 h, heating to 90-100 ℃ after heat preservation is finished, preserving heat for 1-4 h, and continuously heating to 105-120 ℃ after heat preservation is finished, and preserving heat for 1-3 h; and after the reaction is finished, adding alkali until the pH value is 8-9, and adding acid for neutralization to obtain a chlorination feed liquid.
3. The method for separating and extracting sucralose-6-acetate according to claim 1, wherein the mass of the pure water added in the step (2) is 5 to 10 times of the mass of the chlorination liquid, the stirring temperature is 50 to 65 ℃, and the stirring time is 10 to 100 min.
4. The method for separating and extracting sucralose-6-acetate according to claim 1, wherein the mass of the activated carbon added in the step (2) is 5 to 10 percent of the mass of the chlorination solution, the stirring temperature is 40 to 60 ℃, and the stirring time is 10 to 100 min.
5. The method for separating and extracting sucralose-6-acetate according to claim 1, wherein the mass ratio of the total addition of butyl acetate for extraction to the chlorinated feed liquid in the step (3) is 5-20: 1.
6. the method for separating and extracting sucralose-6-acetate according to claim 5, wherein the mass ratio of the total addition of butyl acetate for extraction to the chlorinated feed liquid in the step (3) is 10-15: 1.
7. the method for separating and extracting sucralose-6-acetate according to claim 1, wherein the amount of butyl acetate added in the step (4) is 1 to 3 times of the mass of the slurry material, and the heating temperature is 50 to 80 ℃.
8. The method for separating and extracting sucralose-6-acetate according to claim 7, wherein the amount of butyl acetate added in the step (4) is 1.5 to 2 times of the mass of the slurry material, and the heating temperature is 60 to 80 ℃.
9. The method for separating and extracting sucralose-6-acetate according to claim 1, wherein the mass of the water added in the step (5) is 2.5 to 4 times of the mass of the crude sucralose-6-acetate crystals, and the heating temperature is 40 to 65 ℃.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113717237A (en) * | 2021-08-17 | 2021-11-30 | 安徽金禾实业股份有限公司 | Method for preparing sucralose from sucralose-6-acetate neutralization solution |
| WO2024119464A1 (en) * | 2022-12-09 | 2024-06-13 | 安徽金禾实业股份有限公司 | Preparation method for sucralose |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113717237A (en) * | 2021-08-17 | 2021-11-30 | 安徽金禾实业股份有限公司 | Method for preparing sucralose from sucralose-6-acetate neutralization solution |
| CN113717237B (en) * | 2021-08-17 | 2024-03-29 | 安徽金禾实业股份有限公司 | Method for preparing sucralose from sucralose-6-acetate neutralization solution |
| WO2024119464A1 (en) * | 2022-12-09 | 2024-06-13 | 安徽金禾实业股份有限公司 | Preparation method for sucralose |
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