CN103044498A - Production system of sucralose - Google Patents
Production system of sucralose Download PDFInfo
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- CN103044498A CN103044498A CN2013100048932A CN201310004893A CN103044498A CN 103044498 A CN103044498 A CN 103044498A CN 2013100048932 A CN2013100048932 A CN 2013100048932A CN 201310004893 A CN201310004893 A CN 201310004893A CN 103044498 A CN103044498 A CN 103044498A
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- sucralose
- acetic ester
- synthesis system
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Abstract
The invention discloses a production system of sucralose. The production system adopts a monoester method to produce sucralose, and mainly comprises a sucrose-6-acetate synthetic system, a sucralose-6-acetate synthetic system, and a sucralose synthetic system. The production system is simple, clear and high in practicability; the content of produced sucralose can reach 99.8%; the yield can reach 46-49%; and the annual throughput can reach 300t.
Description
Technical field
The present invention relates to a kind of production system of Sucralose.
Background technology
Sucralose (TGS) is by (the Tate﹠amp of Britain Tai Lai company; Lyie) with a kind of novel sweetener of London University in common development in 1976, be unique functional sweetener take sucrose as raw material, original trade(brand)name is Splenda; The Chinese another name: Sucralose, sucrose is brilliant, tri-chloro galactose type sugar; English name: Sucralose; Chemical name: Sucralose.Sucralose is a kind of white powder product, very easily water-soluble, ethanol and methyl alcohol.Compare it with other sweeting agent and possess multinomial unrivaled superior character: sugariness is 600-650 times of sucrose; Without any peculiar smell or bitter taste; Absolute security; Caloric value is extremely low, can supply the diabetics, and Patients with Cardiovascular/Cerebrovascular Diseases and the elderly use; Can not cause carious tooth; Has good solvability and stability; Acid and alkali-resistance, high temperature resistant, shelf-lives is long.Sucralose can also be sheltered the astringent taste that various VITAMIN and functional material produce, pungent mouthfeel that can the alleviation of alcohol beverage.Tart flavour and saline taste there is the desalination effect; Astringent taste, bitter taste, vinosity are covered effect; Pungent, milk flavor there is synergism.Because Sucralose has good stability at aspects such as heating, sterilization, prolonged preservation and has been widely used in beverage, chewing gum, milk-product, syrup, bread, cake, ice-creams, jelly, pudding, flavored milk, sauce and jam product, vinegar, oyster sauce, soy sauce, wasabi breakfast cereals, sweet milk powder, candy, jam; The food technology that is used for high temperature process, can overcome that the sugariness that this class beverage presents reduces when high temperature, degradation phenomenon under the sweet taste mouthfeel, in the processed foods such as hot worked fruit or dehydrated fruits, bakery, fruit filling, solid beverage, concentrated garden spgarden stuff, salad dressing; Leavened food is such as fermented wine etc.; Low sugar product for obesity, cardiovascular disorder and diabetic subject; The production of fruit can, candied food has the good reputation of the sweeting agent on the dining table, can be used for simultaneously in protective foods and the medicine.Therefore, this product is current optimal intense sweetener, can be for children, teenager, youth, middle age, old age and various diseases patient, without any nutritional problem.Now more than 120 state approvals such as the existing U.S., Canada, Australia, Russia, China use.Canada took the lead in ratifying the use Sucralose in 1991, and the inland of China is in approval use on July 1st, 1997, and U.S. food Drug Administration approval on March 21st, 1998 Sucralose uses as foodstuff additive.At present, the world market annual requirement is 4,600,000,000 yuans, and increases sharply with annual 20% speed.
At present, the novel high-grade foodstuff additive are one of China's emphasis New Product Development Item, and synthetic sweetener is one of foodstuff additive the most active in studying in the world and selling.For a long time, sugar is the main source that the mankind obtain confectionery always, about 100,000,000 tons of year consumption of present Global Sugar, and year consumption is about 22 kilograms per capita.China is populous, and the food consumption numerical quantity is surprising, at present take sugar as raw material or the food of auxiliary material kind more than 3000 is arranged, wherein especially increase rapidly with beverage, 2000 annual production surpass 1,250 ten thousand tons, as seen China's sweeting agent potential of demand is huge.Sucralose is good and cheap, has the very strong market competitiveness, and development prospect is very wide.Along with country proposes the strategy of sustainable development and the development of satisfying domestic health diet culture, the development and production Sucralose meets the trend of current sweeting agent, has important social effect and economic worth.Raising along with living standards of the people, develop low in calories, high sugariness and have functional non-nutritive sweeting agent and seem particularly urgent to satisfy food development and Adjustment of diet, to adapting to the international food trend, improving the domestic food additive level also has positive meaning.Insider's prediction, China is within following considerable time, and Sucralose will occupy prominent position as special-purpose sweeting agent in foodstuffs industry, and will be greatly developed and widespread use.
Present synthetic method mainly contains the monoesters method, group transfer method (full ester method), enzyme-chemically method.1) chemical synthesis; as raw material take sucrose; at first at 6 of sucrose; acetylize behind the hydroxyl tritylation on 1 ' and 6 ' three primary carbon positions; make 8 hydroxyl total overall reactions of sucrose molecules, then slough trityl group and form penta-acetyl sucrose, then with on the acetyl group migration to 6 on 4; carry out again chlorination, last deacetylation and obtain Sucralose.2) chemistry-enzymic synthesis method; it is the radical protection method on having adopted 6; it is take dextrose plus saccharose as raw material; at first glucose fermentation generates glucose-6-acetic ester; then after purifying, chromatographic separation under the effect of sucrose at enzyme, generates cane sugar-6-acetic ester; obtain sucralose-6-acetic ester through chlorination again, last deacetylate namely obtains Sucralose.3) monoesters method, this is in recent years for valued method.It is as raw material take sucrose; make the hydroxyl on 6 of the sucrose generate monoesters with chemical process, namely cane sugar-6-acetic ester carries out selective chlorination and generates sucralose-6-acetic ester with suitable chlorizating agent again; last deacetylate obtains Sucralose through crystallization and purification.The industrial method of at present tool development prospect is as raw material take sucrose; under catalyzer P-TOLUENE SULFO ACID 99's effect; sucrose and trimethyl orthoacetate reaction generate cane sugar-6-acetic ester; carry out selective chlorination and generate sucralose-6-acetic ester with sulfur oxychloride again; last deacetylate obtains Sucralose.
Summary of the invention
First: the synthesis system of cane sugar-6-acetic ester, this system mainly is comprised of following equipment: A
1-2000L glassed steel reaction vessels; A
2-6m
2Stainless steel straight tube condenser; A
3-500LPVC scale tank; A
4The iron receptor of-2000L; A
5-leading to one overlaps secondary high vacuum unit, X-6 water-circulating pump, jz-lobe pump; A
6-pumping solvent to 40 ton withdrawing can; B
1-3000L chlorination glassed steel reaction vessels; B
2-2000L chlorination reagent preparing tank; B
3-10m chip Stainless Steel Condenser; B
4-500LPVC scale tank; B
5-absorption tower; C
1-5000L glassed steel reaction vessels; C
2-500LPVC scale tank; C
3-whizzer; C
4-3m
3Hopper; C
5-take away pump; D
1-3000L glassed steel reaction vessels; D
2-500LPVC scale tank; D
3-10m
2Stainless steel straight tube condenser; D
4-3m
3Iron receptor; D
5-leading to one overlaps secondary high vacuum unit, X-6 water-circulating pump, jz-lobe pump; D
6-pumping solvent to 40 ton withdrawing can; D
7-feeding is to extractor; D
8-100L pressure filter.
Second: the synthesis system of sucralose-6-acetic ester, this system mainly is comprised of following equipment: E
1-3000L ethyl acetate extraction tank; E
2-2m
3Geosyncline; E
3-extractant feed; E
4-feeding is to bleacher; F
1-3000L ethyl acetate withdrawing can, the crystallization of muriate crude product; F
2-20m
2Stainless steel straight tube condenser; F
3-3m
3Band condensation chuck solvent receiver; F
4-500LPVC scale tank; F
5-vacuum pump; F
6-feeding is to extractor; F
7-whizzer; F
8-2m
3Geosyncline; G
1-2000L muriate treatment tank; G
2-500LPVC scale tank; H
1-1000L sucralose-6-acetic ester finished product charging tank; H
2-500LPVC scale tank; H
3-500L the groove that connects material; H
4-feeding is to I
1Tank.
The 3rd: the synthesis system of Sucralose, this system mainly is comprised of following equipment: I
1-1000L bleacher; I
2-6m
2Stainless steel straight tube condenser; I
3The iron receptor of-500L; I
4-100L pressure filter; J
1-1000L Sucralose crystallizer; J
2-6m
2Stainless steel straight tube condenser; J
3-whizzer; J
4The iron receptor of-500L; J
5-500L geosyncline; K
1-1000L sucralose purification crystallizer; K
2-6m
2Stainless steel straight tube condenser; K
3The iron receptor of-500L; K
4-high vacuum unit.
The monoesters method, this is in recent years for valued method.It is take sucrose as raw material, uses chemical process, makes the hydroxyl on 6 of the sucrose generate monoesters, it is cane sugar-6-acetic ester, carry out selective chlorination and generate sucralose-6-acetic ester with suitable chlorizating agent again, slough at last ester group, namely obtain Sucralose through crystallization and purification.
The invention accompanying drawing
The synthesis system of Fig. 1 cane sugar-6-acetic ester
The synthesis system of Fig. 2 sucralose-6-acetic ester
The synthesis system of Fig. 3 Sucralose
Embodiment
Cane sugar-6-acetic ester is synthetic: in the 1000mL three-necked bottle, add 400mL DMF and the sucrose 100g of drying (60～70 ℃ are dried by the fire 40h, dry by the fire behind elder generation's powder), 85～90 ℃ of heating for dissolving, all be cooled to 40 ℃ after the dissolving, add 2.2g tosic acid and 95mL trimethyl orthoacetate, at 32 ℃ of stirring reaction 4h; Then add water 90mL, stirring reaction 5h; Add again TERTIARY BUTYL AMINE 26mL, transfer pH 10, stirring reaction 4h.After reaction finished, high vacuum reclaim under reduced pressure DMF must evaporate to dryness, and the foaming of steaming adds 1000mLDMF behind the evaporate to dryness, and while hot dissolving is chilled to-10 ℃ after molten entirely, waits until chlorination.
Sucralose-6-acetic ester is synthetic: the chlorination reagent configuration: add 600mLDMF in the 1000mL flask, be chilled to-10 ℃, drip sulfur oxychloride 100g, dropwising below 10 ℃, stir 3h at 20 ℃.The above chlorination reagent that configures is added drop-wise in the DMF feed liquid, is dropwising below-10 ℃, at 10 ℃ of insulated and stirred reaction 2h; Be warming up to 30 ℃, insulated and stirred reaction 2h; Slowly be warming up to again 38 ℃, insulated and stirred reaction 2h; Slowly be warming up to again 58 ℃, insulated and stirred reaction 2h; Slowly be warming up to again 78 ℃, insulated and stirred reaction 2h; Slowly be warming up to again 110 ℃, insulated and stirred reaction 2h; Be chilled to rapidly below 30 ℃ after reaction finishes, drip 20%NaOH and transfer pH10, transfer pH neutral with 25%HCL again, suction filtration immediately, filtrate high vacuum reclaim under reduced pressure DMF (temperature is no more than 50 ℃) must be steamed into pulpous state.Add while hot the 200mL water dissolution, complete molten rear suction filtration, filtrate is with ethyl acetate extraction 4 times, 20min is stirred in each extraction, leaves standstill 30min, and acetic acid ethyl fluid is concentrated into a small amount of rear 10g of adding gac, at 80 ℃ of insulation 30min, suction filtration, filtrate is concentrated into dried, add water 800mL, dissolving is chilled to 25 ℃ of crystallizations while hot, suction filtration, mother liquor are again concentrated, crystallization, merge crystallisate, at 60～80 ℃ of baking 24h, can get dry product 80～90g.
Synthesizing of Sucralose: add anhydrous methanol 250mL dissolving in the muriate of above 50g, complete molten rear under 40 ℃, transfer pH to 11 with anhydrous methanol sodium, 50 ℃ of insulated and stirred reaction 8h, the 732 type resin cation (R.C.)s that adding had been dried after reaction finished transfer pH to neutral, suction filtration, and filtrate adds the 6g gac, be incubated 30min after being heated to 50 ℃, be concentrated into driedly under the suction filtration, 60 ℃ of filtrates, it is complete to add the 70mL acetic acid ethyl dissolution, use water cooling, add 45mL 1,2-ethylene dichloride and a small amount of seeded crystallization are 30 ℃ of crystallizations again, suction filtration is dried to get product.
Claims (2)
1. the production system of a Sucralose is characterized in that, comprises the cane sugar-6-acetic ester synthesis system, the sucralose-6-acetic ester synthesis system, and the Sucralose synthesis system:
Described cane sugar-6-acetic ester synthesis system comprises glassed steel reaction vessels, stainless steel straight tube condenser, scale tank, receptor, water-circulating pump, jz-lobe pump, withdrawing can, reagent preparing tank, chip Stainless Steel Condenser, the absorption tower, whizzer, hopper, iron receptor, the high vacuum unit, extractor, the compositions such as pressure filter.
Described sucralose-6-acetic ester synthesis system comprises extractor, geosyncline, and bleacher, withdrawing can, stainless steel straight tube condenser, band condensation chuck solvent receiver, scale tank, vacuum pump, whizzer, treatment tank, the compositions such as groove connect material.
Described Sucralose synthesis system comprises bleacher, stainless steel straight tube condenser, iron receptor, pressure filter, crystallizer, whizzer, geosyncline, the compositions such as high vacuum unit.
2. the production system of a kind of Sucralose as claimed in claim 1 is characterized in that, the Sucralose content of producing through this system can reach 99.8%, and yield reaches 46～49%, and annual production can reach 300 tons.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2013100048932A CN103044498A (en) | 2013-01-07 | 2013-01-07 | Production system of sucralose |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2013100048932A CN103044498A (en) | 2013-01-07 | 2013-01-07 | Production system of sucralose |
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| CN103044498A true CN103044498A (en) | 2013-04-17 |
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| CN2013100048932A Pending CN103044498A (en) | 2013-01-07 | 2013-01-07 | Production system of sucralose |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105669784A (en) * | 2016-03-04 | 2016-06-15 | 李云军 | Chlorination method of sucrose-6-acetate |
-
2013
- 2013-01-07 CN CN2013100048932A patent/CN103044498A/en active Pending
Non-Patent Citations (1)
| Title |
|---|
| 豆丁网: ""300吨/年三氯蔗糖项目简介"", 《HTTP://WWW.DOCIN.COM/P-82788700.HTML》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105669784A (en) * | 2016-03-04 | 2016-06-15 | 李云军 | Chlorination method of sucrose-6-acetate |
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Address after: Huxian 710309 Shaanxi province Xi'an city qinduzhen Street Applicant after: Li Yushan Address before: 710075 Shaanxi Province, Xi'an City High Road No. 25 building 16D enjoye Applicant before: Li Yushan |
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Application publication date: 20130417 |