CN108659061B - A kind of purification treatment method of sucralose crystal mother liquor - Google Patents
A kind of purification treatment method of sucralose crystal mother liquor Download PDFInfo
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- CN108659061B CN108659061B CN201810776930.4A CN201810776930A CN108659061B CN 108659061 B CN108659061 B CN 108659061B CN 201810776930 A CN201810776930 A CN 201810776930A CN 108659061 B CN108659061 B CN 108659061B
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- 235000019408 sucralose Nutrition 0.000 title claims abstract description 76
- 239000004376 Sucralose Substances 0.000 title claims abstract description 74
- 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 title claims abstract description 74
- 239000012452 mother liquor Substances 0.000 title claims abstract description 63
- 238000000034 method Methods 0.000 title claims abstract description 31
- 238000000746 purification Methods 0.000 title claims description 16
- 239000013078 crystal Substances 0.000 title claims 4
- DKPFZGUDAPQIHT-UHFFFAOYSA-N Butyl acetate Natural products CCCCOC(C)=O DKPFZGUDAPQIHT-UHFFFAOYSA-N 0.000 claims abstract description 44
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 claims abstract description 44
- 238000000605 extraction Methods 0.000 claims abstract description 34
- 238000002425 crystallisation Methods 0.000 claims abstract description 26
- 230000008025 crystallization Effects 0.000 claims abstract description 25
- 239000002351 wastewater Substances 0.000 claims abstract description 13
- 238000003810 ethyl acetate extraction Methods 0.000 claims abstract description 3
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 108
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 69
- 238000003756 stirring Methods 0.000 claims description 19
- 238000004821 distillation Methods 0.000 claims description 14
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 9
- 239000010865 sewage Substances 0.000 claims description 9
- 239000003960 organic solvent Substances 0.000 claims description 8
- 238000003860 storage Methods 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 7
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- DCKVNWZUADLDEH-UHFFFAOYSA-N sec-butyl acetate Chemical compound CCC(C)OC(C)=O DCKVNWZUADLDEH-UHFFFAOYSA-N 0.000 claims description 5
- 229930006000 Sucrose Natural products 0.000 claims description 4
- 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 claims description 4
- 238000005070 sampling Methods 0.000 claims description 4
- 239000005720 sucrose Substances 0.000 claims description 4
- 125000000113 cyclohexyl group Chemical group [H]C1([H])C([H])([H])C([H])([H])C([H])(*)C([H])([H])C1([H])[H] 0.000 claims description 2
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims 3
- 238000010025 steaming Methods 0.000 claims 2
- 238000004042 decolorization Methods 0.000 claims 1
- 238000011084 recovery Methods 0.000 abstract description 6
- 239000002904 solvent Substances 0.000 abstract description 3
- 238000005086 pumping Methods 0.000 description 8
- 238000007599 discharging Methods 0.000 description 7
- 238000001816 cooling Methods 0.000 description 6
- 238000001704 evaporation Methods 0.000 description 5
- 239000008122 artificial sweetener Substances 0.000 description 2
- 235000021311 artificial sweeteners Nutrition 0.000 description 2
- 235000019658 bitter taste Nutrition 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 235000003599 food sweetener Nutrition 0.000 description 2
- 239000003765 sweetening agent Substances 0.000 description 2
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical group OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 208000002925 dental caries Diseases 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 201000006549 dyspepsia Diseases 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 235000013373 food additive Nutrition 0.000 description 1
- 239000002778 food additive Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 235000019640 taste Nutrition 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H5/00—Compounds containing saccharide radicals in which the hetero bonds to oxygen have been replaced by the same number of hetero bonds to halogen, nitrogen, sulfur, selenium, or tellurium
- C07H5/02—Compounds containing saccharide radicals in which the hetero bonds to oxygen have been replaced by the same number of hetero bonds to halogen, nitrogen, sulfur, selenium, or tellurium to halogen
-
- 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)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Extraction Or Liquid Replacement (AREA)
Abstract
The invention provides a method for purifying and treating sucralose crystallization mother liquor, which comprises four steps of butyl acetate extraction, ethyl acetate extraction, wastewater concentration and butyl acetate layer treatment, and has the advantages of high recovery rate, less solvent consumption, less wastewater generation and good economic and social benefits.
Description
Technical Field
The invention belongs to the field of food additives, and particularly relates to a purification treatment method of sucralose crystallization mother liquor.
Background
Sucralose (TGS), commonly known as sucralose, is a novel artificial sweetener developed by Teley, England, Inc. (Tate & Lyle) and filed in 1976 with the university of London. Is a functional sweetener only using sucrose as raw material, the original trade name is Splenda, and the sweetness can reach 320 to 1,000 times of that of the sucrose. The artificial sweetener has the characteristics of no calorie, high sweetness, pure sweetness, high safety and the like. However, sucralose may decompose during food processing (mainly due to thermal decomposition, boiling water is still within safe range), and produce toxic products harmful to human body.
The sweetness profile of sucralose almost overlaps that of sucrose, with no bitterness. Low heat content, difficult digestion and absorption, and difficult generation of dental caries. The sucralose does not affect food in the using process, and can cover unpleasant tastes such as bitterness and the like. The sucralose can be used alone or mixed with other sweeteners, is easily dissolved in water, and does not foam in the dissolving process.
At present, the crystallization method of sucralose in industrial production mainly uses water as a solvent for crystallization, and the process of water crystallization necessarily generates mother liquor. The solubility of the sucralose in water is high, the concentration of the sucralose remained in the mother liquor can reach about 30% after water crystallization, and the purity of the sucralose in the mother liquor of the water crystallization is only about 92%, which cannot reach the standard of fine sucralose, so that the purity of the sucralose in the mother liquor of the water crystallization is improved by an organic solvent extraction method, the mother liquor of the sucralose water crystallization can be recycled for many times, and the method plays an important role in improving the purity and the crystallization rate of the sucralose. However, the existing purification treatment method can generate a large amount of wastewater, and the high requirements of environmental protection are difficult to meet under the condition that the environmental protection is increasingly emphasized at present.
Disclosure of Invention
The invention aims to overcome the defect that a purification treatment method of sucralose crystallization mother liquor in the prior art can generate a large amount of wastewater, and provides the purification treatment method of the sucralose crystallization mother liquor, which has the advantages of low wastewater yield and high sucralose recovery rate.
The invention provides a purification treatment method of sucralose crystallization mother liquor, which is characterized by comprising the following steps:
(1) adding sucralose mother liquor into the extraction kettle, and adjusting the pH value to be nearly neutral; adding butyl acetate with the mass of 1/5-2/5 of sucralose mother liquor into an extraction kettle, stirring and standing, separating a lower layer of water into a transfer tank, separating an upper layer of butyl acetate into a butyl acetate storage tank, and repeatedly extracting for 2-4 times in total;
(2) transferring the water layer obtained by layering in the step (1) into an extraction kettle, adding ethyl acetate with the mass of 2/5-3/5 of the mother liquor of sucralose, stirring, standing, separating the lower-layer water layer into a mother liquor transfer tank, separating the upper-layer ethyl acetate layer into a distillation kettle, repeatedly extracting for 2-4 times, sampling to determine that the content of sucralose in the water layer is less than 5%, and pumping into a storage tank for concentration;
(3) pumping the water layer obtained in the step (2) into a concentration kettle, distilling water under reduced pressure until the content of sucralose in the water layer is 25-30%, transferring the concentrated mother liquor back into an extraction kettle, adding ethyl acetate with the mass of the sucralose mother liquor being 2/5-3/5, extracting for 2-4 times, and discharging into a sewage tank when the content of the water layer is less than 2%; combining the ethyl acetate layer with the ethyl acetate layer obtained in the step (2) to evaporate ethyl acetate, and decoloring and distilling the ethyl acetate layer in a finished product workshop to produce sucralose;
(4) putting the butyl acetate layer after the mother liquor is extracted in the step (1) into a butyl acetate distillation kettle, evaporating 50-60% of butyl acetate by mass, cooling to 30-40 ℃, adding water, stirring, standing, and adding water with the mass being 20-25% of the mass of the residual butyl acetate; separating a water layer into a transfer tank, repeating the wastewater concentration in the step (3) again, and continuously washing the butyl acetate layer for 1-3 times; and (4) carrying out reduced pressure distillation on the residual butyl acetate after washing, and discharging the residual liquid into a sewage pool after cooling.
Preferably, the pH value to near neutrality in the step (1) is 6.5-7.5.
Preferably, in the steps (1), (2) and (4), the specific time for stirring and standing is 0.2-1 h for stirring and 0.2-1 h for standing.
Preferably, the mass of the butyl acetate added in the step (1) is 1/5-1/3 of the mass of the sucralose mother liquor.
Preferably, after the extraction in the step (1) is finished, the pH is adjusted to 6.5-7.5 again.
Preferably, the extraction in step (1) is repeated a total of 3 times.
Preferably, the adding amount of the ethyl acetate in each step in the steps (2) and (3) is 1/2-3/5 of the mass of the sucralose mother liquor.
Preferably, the aqueous layer obtained in the step (2) is extracted with a low-polarity organic solvent for 1-3 times before being pumped into a concentration kettle.
Preferably, the low polarity organic solvent is selected from cyclohexane, toluene or dichloromethane.
Preferably, the addition amount of the low-polarity organic solvent is 5-10%. After extraction by the low-polarity organic solvent, the content of volatile organic matters in the water layer is greatly reduced, and the water distilled in the step (3) can be recycled, so that the yield of the wastewater is greatly reduced.
The invention has the beneficial effects that: the purification treatment method of the sucralose crystallization mother liquor provided by the invention has the advantages of high recovery rate, less solvent consumption, less wastewater generation and good economic and social benefits.
Detailed Description
The technical solutions of the present invention are described below by way of specific examples, but the scope of the present invention is not limited thereto.
Example 1
A purification treatment method of sucralose crystallization mother liquor comprises the following steps:
(1) adding 3000kg of sucralose mother liquor into the extraction kettle, and adjusting the pH to 7; adding 750kg of butyl acetate into an extraction kettle, stirring for 0.5h, standing for 0.5h, separating the lower layer of water into a transfer tank, separating the upper layer of butyl acetate into a butyl acetate storage tank, and repeatedly extracting for 3 times in total;
(2) transferring the water layer obtained by layering in the step (1) into an extraction kettle, adding ethyl acetate with the mass of 1800kg of sucralose mother liquor, stirring, standing, separating the lower-layer water layer into a mother liquor transfer tank, separating the upper-layer ethyl acetate layer into a distillation kettle, repeatedly extracting for 3 times, sampling to determine that the content of sucralose in the water layer is less than 5%, and pumping into a storage tank for concentration;
(3) pumping the water layer obtained in the step (2) into a concentration kettle, distilling water under reduced pressure until the content of sucralose in the water layer is about 25%, transferring 3000kg of concentrated mother liquor back into the extraction kettle, adding 1800kg of ethyl acetate, extracting for 3 times, and discharging the concentrated mother liquor into a sewage tank when the content of the water layer is less than 2%; combining the ethyl acetate layer with the ethyl acetate layer obtained in the step (2) to evaporate ethyl acetate, and decoloring and distilling the ethyl acetate layer in a finished product workshop to produce sucralose;
(4) adding about 9000kg of the three butyl acetate layers after mother liquor extraction in the step (1) into a butyl acetate distillation kettle, evaporating 5000kg of butyl acetate, cooling to 35 ℃, adding water, stirring, standing, adding 900kg of water, stirring for 0.5h, and standing for 0.5 h; separating the water layer into a transfer tank, repeating the step (3) of wastewater concentration again, and continuously washing the butyl acetate layer with 500kg of water for 2 times; and (4) carrying out reduced pressure distillation on the residual butyl acetate after washing, and discharging the residual liquid into a sewage pool after cooling.
Through calculation, the recovery rate of the sucralose in the sucralose crystallization mother liquor operated according to the method in the embodiment 1 is more than or equal to 98.5 percent, and the purity of the obtained sucralose is more than or equal to 99.6 percent.
Example 2
A purification treatment method of sucralose crystallization mother liquor comprises the following steps:
(1) adding 3000kg of sucralose mother liquor into the extraction kettle, and adjusting the pH to 7; adding 750kg of butyl acetate into an extraction kettle, stirring for 0.5h, standing for 0.5h, separating the lower layer of water into a transfer tank, separating the upper layer of butyl acetate into a butyl acetate storage tank, and repeatedly extracting for 4 times in total;
(2) transferring the water layer obtained by layering in the step (1) into an extraction kettle, adding ethyl acetate with the mass of 1800kg of the mother liquid of sucralose, stirring, standing, separating the lower-layer water layer into a mother liquid transfer tank, separating the upper-layer ethyl acetate layer into a distillation kettle, repeatedly extracting for 4 times, and sampling to determine that the content of sucralose in the water layer is less than 5%; adding 200kg of toluene into the water layer to extract ethyl acetate, extracting for 2 times in total, and pumping the water layer obtained by separation into a storage tank for concentration;
(3) pumping the water layer obtained in the step (2) into a concentration kettle, distilling water under reduced pressure until the content of sucralose in the water layer is about 30%, transferring 3000kg of concentrated mother liquor back into the extraction kettle, adding 1800kg of ethyl acetate, extracting for 4 times, specifically performing the same extraction operation as the step (2), and discharging the concentrated mother liquor into a sewage tank when the content of the water layer is less than 2%; combining the ethyl acetate layer with the ethyl acetate layer obtained in the step (2) to evaporate ethyl acetate, and decoloring and distilling the ethyl acetate layer in a finished product workshop to produce sucralose; the distilled water can be reused.
(4) Adding about 9000kg of the three butyl acetate layers after mother liquor extraction in the step (1) into a butyl acetate distillation kettle, evaporating 5000kg of butyl acetate, cooling to 35 ℃, adding water, stirring, standing, adding 900kg of water, stirring for 0.5h, and standing for 0.5 h; separating the water layer into a transfer tank, repeating the step (3) of wastewater concentration again, and continuously washing the butyl acetate layer with 500kg of water for 3 times; and (4) carrying out reduced pressure distillation on the residual butyl acetate after washing, and discharging the residual liquid into a sewage pool after cooling.
Through calculation, the recovery rate of the sucralose in the sucralose crystallization mother liquor operated according to the method in the embodiment 2 is more than or equal to 98.5 percent, and the purity of the obtained sucralose is more than or equal to 99.6 percent; the yield of the wastewater is about 20 percent of the volume of the sucralose mother liquor.
Comparative example
The novel sucralose mother liquor extraction process comprises the following steps:
(1) 2400kg of finished mother liquor and 600kg of butyl acetate are added into an extraction kettle, stirred for 30 minutes, kept stand for 30 minutes, then an upper butyl acetate layer is separated, a water layer is left, and the operations are repeated for 4 times;
(2) adding 1800kg of ethyl acetate into a water layer in the butyl acetate extraction step, stirring for 30 minutes, standing for 30 minutes, pouring an ethyl acetate layer after layering into a distillation still, continuously adding 1000kg of ethyl acetate into the water layer for extraction, repeating the extraction for two times, and leaving the ethyl acetate layer after the last extraction with 1800kg of ethyl acetate for processing next batch of mother liquor;
(3) concentrating the ethyl acetate layer in the ethyl acetate extraction step under reduced pressure, collecting ethyl acetate, recovering ethyl acetate, evaporating to dryness, adding water, decolorizing, and evaporating to obtain mother liquor;
(4) and (3) pumping the butyl acetate layer extracted for 4 times in the butyl acetate extraction step into a butyl acetate distillation kettle, adding 240kg of water, stirring for 30 minutes, standing for 30 minutes, separating a water layer into a transfer tank, continuously adding 240kg of water into the butyl acetate layer, repeating the process, distilling the butyl ester in the distillation kettle under reduced pressure until the butyl ester does not flow out basically, adding water to dissolve the butyl ester, discharging the butyl ester into a sewage pipe network, pumping the water layer into a finished product mother liquor head tank, and treating the finished product mother liquor.
Through calculation, the recovery rate of the sucralose in the sucralose crystallization mother liquor operated according to the comparative example method is about 90 percent, and the purity of the obtained sucralose is about 97 percent; the yield of the wastewater is about 120 percent of the volume of the sucralose mother liquor.
In light of the foregoing description of the preferred embodiment of the present invention, many modifications and variations will be apparent to those skilled in the art without departing from the spirit and scope of the invention. The technical scope of the present invention is not limited to the content of the specification, and must be determined according to the scope of the claims.
Claims (9)
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111499672B (en) * | 2019-01-30 | 2021-07-20 | 山东新和成精化科技有限公司 | Extraction method for purifying sucralose |
| CN112480186A (en) * | 2020-11-30 | 2021-03-12 | 安徽金禾实业股份有限公司 | Method for treating primary mother liquor of sucralose |
| CN114230620B (en) * | 2021-11-23 | 2023-05-16 | 安徽金禾实业股份有限公司 | Treatment method of sucralose crystallization mother liquor |
| CN114195837A (en) * | 2021-11-23 | 2022-03-18 | 安徽金禾实业股份有限公司 | Continuous treatment device and method for mother liquor of secondary crude sucralose ester product |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2008004246A1 (en) * | 2006-07-06 | 2008-01-10 | Alembic Limited | An improved process for the preparation of sucralose of high purity |
| CN103242384A (en) * | 2013-05-27 | 2013-08-14 | 南通市常海食品添加剂有限公司 | Novel sucralose mother liquor extraction process |
| CN104861003A (en) * | 2015-04-24 | 2015-08-26 | 吉安市新琪安科技有限公司 | Sucralose mother liquor processing method |
| CN106674292A (en) * | 2016-12-09 | 2017-05-17 | 福建科宏生物工程股份有限公司 | Method for purification treatment of sucralose water crystallization mother liquor |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| AR071134A1 (en) * | 2008-04-03 | 2010-05-26 | Tate & Lyle Technology Ltd | CRYSTALLIZATION OF SUCRALOSE FROM SQURALOSA CONTAINING |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2008004246A1 (en) * | 2006-07-06 | 2008-01-10 | Alembic Limited | An improved process for the preparation of sucralose of high purity |
| CN103242384A (en) * | 2013-05-27 | 2013-08-14 | 南通市常海食品添加剂有限公司 | Novel sucralose mother liquor extraction process |
| CN104861003A (en) * | 2015-04-24 | 2015-08-26 | 吉安市新琪安科技有限公司 | Sucralose mother liquor processing method |
| CN106674292A (en) * | 2016-12-09 | 2017-05-17 | 福建科宏生物工程股份有限公司 | Method for purification treatment of sucralose water crystallization mother liquor |
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