CN102807594A - Method for refining sucralose-6-ethyl ester - Google Patents
Method for refining sucralose-6-ethyl ester Download PDFInfo
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Abstract
The invention relates to a method for refining sucralose-6-ethyl ester. The method comprises the following steps of: refining a sucralose-6-ethyl ester crude product obtained by concentration for the first time by using an alcohol-ether mixed solvent to remove most impurities; and refining the crude product for the second time by using an ester-alkane mixed solvent to remove trace impurities so as to obtain a high-purity sucralose-6-ethyl ester fine product. By using special mixed solvents, an impurity separation effect is improved, the purity of the sucralose-6-ethyl ester fine product is over 99.5 percent, single-pass crystallization yield is high, and the method is easy and convenient to operate and is suitable for industrial production.
Description
Technical field
The present invention relates to a kind of process for purification of trichloro-cane-6-ethyl ester, belong to the fine chemical technology field.
Background technology
TGS has another name called Sucralose (Sucralose), is a kind of novel type of sucrose chlorinated derivatives product, its chemistry by name 4; 1 ＇, 6 ＇-three chloro-, 4,1 ＇, 6 ＇-three deoxidation gala type sucrose (being called for short TGS); Be a kind of white powder product, because of it has the sugariness height, flavor matter is good, and the shelf lives is long; Advantages such as empty calory and security height become the substitute of sugar gradually, and have represented the developing direction of intense sweetener.The at present main compound method of TGS comprises: 1. chemical synthesis; 2. chemistry-enzymic synthesis method; 3. monoesters method.Wherein, the chemical synthesis step is more, and technical process is complicated, is not suitable for suitability for industrialized production.Chemistry-enzymic synthesis method, fermentation is complicated, and purification intermediate product difficulty, and cost is high.The monoesters method only needs the reaction of 3 steps, and yield is high, and cost is low, and intermediate product is easy to separate, and is the desirable technology of synthesizing trichloro, and most of manufacturers generally adopt by countries in the world.
Mainly contain three steps with monoesters method synthesizing trichloro: 1. esterification: sucrose 6-position hydroxyl is carried out the ethyl ester protection, obtain carboxylate (sucrose-6-ethyl ester); 2. chlorination: the chlorination of sucrose-6-ethyl ester, with 4,1 ＇, 6 ＇-three the hydroxyl chlorinations in position obtain muriate (4,1 ＇, 6 ＇-trichloro-cane-6-ethyl ester); 3. take off ester: muriate is sloughed 6-position protection base under alkaline condition, obtain the TGS product.
In monoesters method synthesizing trichloro process, second one-step chlorination reaction is that synthetic is crucial, owing to have except that the 6-position 7 not protected hydroxyl on the sucrose molecules; Though 4,1 ＇, 3 hydroxyl activities of 6 ＇-positions are stronger; Preferentially by chlorination; But the difference of reaction conditions and chlorizating agent optionally difference all possibly cause more side reaction, make this step gained midbody trichloro-cane-6-ethyl ester contain more impurity, thereby directly influence the quality of TGS finished product.Therefore, the research to the trichloro-cane-6-ethyl ester process for purification has important practical significance.
Zhejiang Polytechnical University's patent " a kind of compound method of trichloro-cane-6-ethyl ester (200610051994.5) " adopts single ethyl acetate solvent extraction, activated carbon decolorizing, recrystallization to obtain trichloro-cane-6-ethyl ester crystalline method; Its patent " a kind of novel method of separation and purification trichloro-cane-6-ethyl ester (200910101477.8) " has been reported the method for purification of " earlier TGS-6 ethyl ester bullion being processed the aqueous solution; with ETHYLE ACETATE or n-butyl acetate extraction, concentrated, obtain the trichloro-cane-6-ethyl ester crystal through crystallization, recrystallization more then ".This method is purified with organic solvent extraction, and the organic solvent consumption is big, and extracting operation is loaded down with trivial details, has strengthened environmental protection pressure, and the purification separating effect is not good.Empirical tests, elaboration purity is not high.
Changzhou Niutang Chemical Industry Co., Ltd.'s patent " preparation method of trichloro-cane-6-ethyl ester (200710020699.8) " has reported that " add the entry heating for dissolving, go out impurity with organic solvent extraction, extraction liquid is used water washing to concentrating the bullion employing that obtains; With the cooling of the aqueous solution and water washing liquor, separate out the trichloro-cane-6-ethyl ester crystallization, filtering drying " method refining, this method is used organic solvent extraction impurity; extracting phase (water) crystallisation by cooling, crystallizing system is the aqueous solution, and the solubleness of trichloro-cane-6-ethyl ester in water is quite big, even can crystallization separate out; once through yield will be very low, mother liquor must be applied mechanically repeatedly, this will have a strong impact on impurity-eliminating effect; cause elaboration purity lower, therefore, this method is not suitable for suitability for industrialized production.
Mamtek International Limited's patent " is used to extract the method (200980136925.6) with the purified sucralose midbody " has reported a kind of method for purification of trichloro-cane-6-ethyl ester; This method adopts water-ether (or alkane) mixed solvent to carry out once refining to the trichloro-cane-6-ethyl ester bullion with the ethyl acetate extraction gained; Adopt the ETHYLE ACETATE single solvent that an elaboration is carried out secondary refining then, obtain refining finished product.The first step is made with extra care water-ether (or alkane) and is made solvent, and the product speed of separating out is too fast, causes more a large amount of impurity to be separated out by double team, can't effectively remove; For the second time refiningly use the ETHYLE ACETATE single solvent, the impurity separating effect is relatively poor, cause to contain small amount of impurities in the finished product and can't remove, and the finished product appearance color is darker.Therefore, the application of this method is restricted.
Summary of the invention
In order to solve the problem of the not high and complicated operation of above-mentioned trichloro-cane-6-ethyl ester purity; The present invention is taking all factors into consideration on the basis of various refining influence factors, adopts different mixed solvents to carry out twice and makes with extra care, and treating process only need reclaim organic solvent; Needn't apply mechanically crystalline mother solution repeatedly; Therefore product purity can reach more than 99.5%, and the crystallization once through yield is higher, working method is easy, is fit to very much industry and goes up scale operation.
Technical scheme of the present invention is carried out once refining for adopting alcohol-ethers mixed solvent to the trichloro-cane-6-ethyl ester syrupy shape bullion that concentrates gained; Remove most of impurity; Adopt ester-mixed alkane solvent to carry out secondary refining then, remove trace impurity, specifically may further comprise the steps:
(1) refining step:
In the trichloro-cane-6-ethyl ester bullion, add alcoholic solvent, be heated with stirring to this trichloro-cane-6-ethyl ester bullion and fully dissolve, form the first trichloro-cane-6-ethyl ester solution;
This first trichloro-cane-6-ethyl ester solution is cooled to 10～40 ℃, and disposable joining in the ether organic solvent, be stirred to and separate out solid; And naturally cooling; Left standstill crystallization 1～10 hour, spinning, drying in-5～20 ℃; Obtain the once wet elaboration of trichloro-cane-6-ethyl ester, the filtrating distillation is reclaimed and is obtained alcohol organic solvent and ether organic solvent;
(2) secondary refining operation:
The once wet elaboration of above-mentioned trichloro-cane-6-ethyl ester is put in ester-mixed alkane solvent, stirred and be warming up to dissolving fully, form the second trichloro-cane-6-ethyl ester solution;
In this second trichloro-cane-6-ethyl ester solution, add discoloring agent, heat up reflux decolour 0.5 hour; Press filtration while hot, filtrating 1～3.5h is cooled to room temperature, leaves standstill crystallization 2～18h in-5～20 ℃; Spinning; Filter cake forms the dried elaboration of trichloro-cane-6-ethyl ester secondary in 30～65 ℃ of vacuum-dryings, and the filtrating distillation is reclaimed and formed ester-mixed alkane solvent.
In the technical scheme of the present invention, also can alcohol organic solvent and the ether organic solvent that obtains be reclaimed in distillation in the step (1), recycled in refining step; Ester-the mixed alkane solvent that obtains is reclaimed in distillation in the step (2), at secondary refining operation recycled.
Preferably, the mass ratio of trichloro-cane-6-ethyl ester bullion and alcoholic solvent is 1:1～20 in the technical scheme of the present invention; Ether organic solvent is 0.1～3:1 with the volume mass ratio of trichloro-cane-6-ethyl ester bullion; Ester-mixed alkane solvent and trichloro-cane-6-ethyl ester once the volume mass ratio of wet elaboration are 1～10:1.
Alcohol organic solvent can be methyl alcohol, ethanol, n-propyl alcohol, Virahol, propyl carbinol, isopropylcarbinol in the technical scheme of the present invention; Ether organic solvent can be ether, di-n-propyl ether, DIPE, ethyl n-butyl ether or 2-methyl furan.
Ester-mixed alkane solvent comprises single ester and single alkane in the technical scheme of the present invention, and single ester can be methyl-formiate, ethyl formate, methyl acetate, ETHYLE ACETATE, propyl acetate; Single alkane is sherwood oil, propane, butane, trichloromethane, methylene dichloride, ethylene dichloride; Wherein single ester and single alkane volume ratio are 1～15:1.
Discoloring agent in the technical scheme of the present invention can be gac, and gac and the trichloro-cane-6-ethyl ester once mass ratio of wet elaboration are 0.05～0.25:1.
Process for purification provided by the invention is different from traditional single solvent process for purification, uses different mixed solvents to carry out twice respectively and makes with extra care, and has not only significantly improved the impurity separating effect, and has guaranteed higher refining yield.The industriallization of present method will effectively promote the quality of TGS to promote and Development and Production, have originality and realistic meaning.
Description of drawings
Fig. 1 is the synoptic diagram of trichloro-cane-6-ethyl ester process for purification of the present invention.
Embodiment
Below in conjunction with accompanying drawing 1 and embodiment, the present invention is elaborated.
Embodiment 1
(1) refining step
In the syrupy shape enriched material of trichloro-cane-6-ethyl ester bullion, according to the ratio adding methyl alcohol of enriched material: methyl alcohol=1:1 (m/m), stirring heating is warming up to 63 ℃, and the syrupy shape enriched material is fully dissolved.Cool to 40 ℃ then, be transferred to fast and added ether and having started in the crystallization kettle that reflux exchanger is housed of stirring, wherein ether: enriched material=0.4:1 (v/m).After waiting to separate out a large amount of solids, stop to stir naturally cooling, left standstill crystallization 6 hours, spinning, drying in 5 ℃.Filter cake is the once wet elaboration of trichloro-cane-6-ethyl ester; Methyl alcohol, ether are reclaimed in the filtrating distillation, and recycled is to this one-step refining.
(2) secondary refining operation
The once wet elaboration of gained in the step (1) is put in ETHYLE ACETATE-ethylene dichloride mixed solvent, wherein mixed solvent: once wet elaboration=2:1 (v/m), ETHYLE ACETATE in the mixed solvent: ethylene dichloride=3:1 (v/v); Add gac, gac is 0.05:1 with the elaboration mass ratio that once wets, and continues to heat up; Reflux decolour 0.5 hour, press filtration while hot naturally cools to room temperature in the filtrating 1.5h; Leave standstill crystallization 5h, spinning in 8 ℃.Filter cake gets the dried elaboration of trichloro-cane-6-ethyl ester secondary in 45 ℃ of vacuum-dryings; ETHYLE ACETATE-ethylene dichloride mixed solvent is reclaimed in the filtrating distillation, and recycled is to this one-step refining.
Detect through HPLC, the purity of the dried elaboration of trichloro-cane-6-ethyl ester secondary is: 99.67%.
Embodiment 2
(1) refining step
In the syrupy shape enriched material of trichloro-cane-6-ethyl ester bullion, according to the ratio adding absolute ethyl alcohol of enriched material: absolute ethyl alcohol=1:6 (m/m), stirring heating is warming up to 62 ℃, and the syrupy shape enriched material is fully dissolved.Cool to 35 ℃ then, be transferred to fast and added di-n-propyl ether and having started in the crystallization kettle that reflux exchanger is housed of stirring, wherein di-n-propyl ether: enriched material=0.5:1 (v/m).After waiting to separate out a large amount of solids, stop to stir naturally cooling, left standstill crystallization 10 hours, spinning, drying in 0 ℃.Filter cake is the once wet elaboration of trichloro-cane-6-ethyl ester; Ethanol, di-n-propyl ether are reclaimed in the filtrating distillation, and recycled is to this one-step refining.
(2) secondary refining operation
The once wet elaboration of gained in the step (1) is put in methyl-formiate-chloroform mixed solvent, wherein mixed solvent: once wet elaboration=4.5:1 (v/m), methyl-formiate in the mixed solvent: chloroform=7:1 (v/v); Add gac, gac is 0.1:1 with the elaboration mass ratio that once wets, and continues to heat up; Reflux decolour 0.5 hour, press filtration while hot naturally cools to room temperature in the filtrating 2h; Leave standstill crystallization 13h, spinning in 12 ℃.Filter cake gets the dried elaboration of trichloro-cane-6-ethyl ester secondary in 42 ℃ of vacuum-dryings; Methyl-formiate-chloroform mixed solvent is reclaimed in the filtrating distillation, and recycled is to this one-step refining.
Detect through HPLC, the purity of the dried elaboration of trichloro-cane-6-ethyl ester secondary is: 99.73%.
Embodiment 3
(1) refining step
In the syrupy shape enriched material of trichloro-cane-6-ethyl ester bullion, according to the ratio adding n-propyl alcohol of enriched material: n-propyl alcohol=1:12 (m/m), stirring heating is warming up to 58 ℃, and the syrupy shape enriched material is fully dissolved.Cool to 30 ℃ then; Be transferred to fast and added DIPE and having started in the crystallization kettle that reflux exchanger is housed of stirring, DIPE: enriched material=0.45:1 (v/m) wherein, wait to separate out a large amount of solids after; Stop to stir naturally cooling; Left standstill crystallization 8 hours, spinning, drying in 10 ℃.Filter cake is the once wet elaboration of trichloro-cane-6-ethyl ester; N-propyl alcohol, DIPE are reclaimed in the filtrating distillation, and recycled is to this one-step refining.
(2) secondary refining operation
The once wet elaboration of gained in the step (1) is put in methyl acetate-propane mixed solvent, wherein mixed solvent: once wet elaboration=5.7:1 (v/m), methyl acetate in the mixed solvent: propane=8.5:1 (v/v); Stirring is warming up to dissolving fully, adds gac, and gac is 0.07:1 with the elaboration mass ratio that once wets; Continue to heat up reflux decolour 0.5 hour, press filtration while hot; Filtrating 2h internal cooling leaves standstill crystallization 9h, spinning to room temperature in 5 ℃.Filter cake gets the dried elaboration of trichloro-cane-6-ethyl ester secondary in 45 ℃ of vacuum-dryings; Methyl acetate-propane mixed solvent is reclaimed in the filtrating distillation, and recycled is to this one-step refining.
Detect through HPLC, the purity of the dried elaboration of trichloro-cane-6-ethyl ester secondary is: 99.53%.
Embodiment 4
(1) refining step
In the syrupy shape enriched material of trichloro-cane-6-ethyl ester bullion, according to the ratio adding Virahol of enriched material: Virahol=1:15 (m/m), stirring heating is warming up to 55 ℃, and the syrupy shape enriched material is fully dissolved.Cool to 20 ℃ then; Be transferred to fast and added ethyl n-butyl ether and having started in the crystallization kettle that reflux exchanger is housed of stirring, ethyl n-butyl ether: enriched material=3:1 (v/m) wherein, wait to separate out a large amount of solids after; Stop to stir naturally cooling; Left standstill crystallization 7 hours, spinning, drying in 11 ℃.Filter cake is the once wet elaboration of trichloro-cane-6-ethyl ester; Virahol, ethyl n-butyl ether are reclaimed in the filtrating distillation, and recycled is to this one-step refining.
(2) secondary refining operation
The once wet elaboration of gained in the step (1) is put in methyl-formiate-butane mixed solvent, wherein mixed solvent: once wet elaboration=9.5:1 (v/m), methyl-formiate in the mixed solvent: butane=15:1 (v/v); Stirring is warming up to dissolving fully, adds gac, the gac and the elaboration mass ratio 0.05:1 that once wets; Continue to heat up reflux decolour 0.5 hour, press filtration while hot; Be chilled to room temperature in the filtrating 1.5h, leave standstill crystallization 8h, spinning in 8 ℃.Filter cake gets the dried elaboration of trichloro-cane-6-ethyl ester secondary in 35 ℃ of vacuum-dryings; Ester-mixed alkane solvent is reclaimed in the filtrating distillation, and recycled is to this one-step refining.
Detect through HPLC, the purity of the dried elaboration of trichloro-cane-6-ethyl ester secondary is: 99.63%.
Embodiment 5
(1) refining step
In the syrupy shape enriched material of trichloro-cane-6-ethyl ester bullion, according to the ratio adding propyl carbinol of enriched material: propyl carbinol=1:20 (m/m), stirring heating is warming up to 55 ℃, and the syrupy shape enriched material is fully dissolved.Cool to 10 ℃ then, be transferred to fast and added ether and having started in the crystallization kettle that reflux exchanger is housed of stirring, wherein ether: enriched material=1.7:1 (v/m); After waiting to separate out a large amount of solids, stop to stir naturally cooling, left standstill crystallization 6 hours in-5 ℃; Spinning dries.Filter cake is the once wet elaboration of trichloro-cane-6-ethyl ester.Propyl carbinol, ether are reclaimed in the filtrating distillation, and recycled is to this one-step refining.
(2) secondary refining operation
The once wet elaboration of gained in the step (1) is put in propyl acetate-sherwood oil mixed solvent, wherein mixed solvent: once wet elaboration=6.5:1 (v/m), propyl acetate in the mixed solvent: sherwood oil (boiling range 30-60 ℃)=15:1 (v/v); Stirring is warming up to dissolving fully, adds gac, and gac is 0.25:1 with the elaboration mass ratio that once wets; Continue to heat up reflux decolour 0.5 hour, press filtration while hot; Be chilled to room temperature in the filtrating 3.5h, leave standstill crystallization 11h, spinning in 5 ℃.Filter cake gets the dried elaboration of trichloro-cane-6-ethyl ester secondary in 35 ℃ of vacuum-dryings; Propyl acetate-sherwood oil mixed solvent is reclaimed in the filtrating distillation, and recycled is to this one-step refining.
Detect through HPLC, the purity of the dried elaboration of trichloro-cane-6-ethyl ester secondary is: 99.70%.
In addition, those skilled in the art also can do other variation in spirit of the present invention, and certainly, these all should be included within the present invention's scope required for protection according to the variation that the present invention's spirit is done.
Claims (10)
1. the process for purification of a trichloro-cane-6-ethyl ester may further comprise the steps:
(1) refining step:
In the trichloro-cane-6-ethyl ester bullion, add alcoholic solvent, be heated with stirring to this trichloro-cane-6-ethyl ester bullion and fully dissolve, form the first trichloro-cane-6-ethyl ester solution;
This first trichloro-cane-6-ethyl ester solution is cooled to 10～40 ℃, and disposable joining in the ether organic solvent, be stirred to and separate out solid; And naturally cooling; Left standstill crystallization 1～10 hour, spinning, drying in-5～20 ℃; Obtain the once wet elaboration of trichloro-cane-6-ethyl ester, the filtrating distillation is reclaimed and is obtained alcohol organic solvent and ether organic solvent;
(2) secondary refining operation:
The once wet elaboration of above-mentioned trichloro-cane-6-ethyl ester is put in ester-mixed alkane solvent, stirred and be warming up to dissolving fully, form the second trichloro-cane-6-ethyl ester solution;
In this second trichloro-cane-6-ethyl ester solution, add discoloring agent, heat up reflux decolour 0.5 hour; Press filtration while hot, filtrating 1～3.5h is cooled to room temperature, leaves standstill crystallization 2～18h in-5～20 ℃; Spinning; Filter cake forms the dried elaboration of trichloro-cane-6-ethyl ester secondary in 30～65 ℃ of vacuum-dryings, and the filtrating distillation is reclaimed and obtained ester-mixed alkane solvent.
2. process for purification according to claim 1 also comprises the steps: alcohol organic solvent and the ether organic solvent that obtains reclaimed in distillation in the step (1), recycled in refining step; Ester-the mixed alkane solvent that obtains is reclaimed in distillation in the step (2), at secondary refining operation recycled.
3. process for purification according to claim 1 is characterized in that: the mass ratio of said trichloro-cane-6-ethyl ester bullion and alcoholic solvent is 1:1～20.
4. process for purification according to claim 1 is characterized in that: said alcohol organic solvent is methyl alcohol, ethanol, n-propyl alcohol, Virahol, propyl carbinol or isopropylcarbinol.
5. process for purification according to claim 1 is characterized in that: said ether organic solvent is 0.1～3:1 with the volume mass of trichloro-cane-6-ethyl ester bullion than (v/m).
6. process for purification according to claim 1 is characterized in that: said ether organic solvent is ether, di-n-propyl ether, DIPE, ethyl n-butyl ether or 2-methyl furan.
7. process for purification according to claim 1 is characterized in that: said ester-mixed alkane solvent and the trichloro-cane-6-ethyl ester once volume mass of wet elaboration are 1～10:1
than (v/m).
8. process for purification according to claim 1 is characterized in that: said ester-mixed alkane solvent comprises single ester and single alkane, and wherein single ester and single alkane volume ratio are 1～15:1
.
9. process for purification according to claim 8 is characterized in that: said single ester is methyl-formiate, ethyl formate, methyl acetate, ETHYLE ACETATE or propyl acetate; Said single alkane is sherwood oil, propane, butane, trichloromethane, methylene dichloride or ethylene dichloride.
10. process for purification according to claim 1 is characterized in that: said discoloring agent is a gac, and gac and the trichloro-cane-6-ethyl ester once mass ratio of wet elaboration are 0.05～0.25:1.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106957345A (en) * | 2017-04-10 | 2017-07-18 | 王满堂 | Improve the production method of the ethyl ester yield of Sucralose 6 |
| CN108250255A (en) * | 2018-01-24 | 2018-07-06 | 山东康宝生化科技有限公司 | A kind of method for improving trichloro-cane-6-ethyl ester crystallization yield |
| CN109734755A (en) * | 2018-12-28 | 2019-05-10 | 山东三和维信生物科技有限公司 | A kind of Sucralose crystallization processes |
| EP4215539A4 (en) * | 2020-11-27 | 2024-01-17 | Anhui Jinhe Industrial Co., Ltd. | Method for purifying sucralose-6-ethyl ester |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101709069A (en) * | 2009-08-06 | 2010-05-19 | 浙江工业大学 | Novel method for separating and purifying sucralose-6-ethyl ester |
| CN102164938A (en) * | 2008-07-23 | 2011-08-24 | 玛特科国际有限公司 | Methods for extracting and purifying sucralose intermediate |
-
2012
- 2012-07-25 CN CN201210259307.4A patent/CN102807594B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102164938A (en) * | 2008-07-23 | 2011-08-24 | 玛特科国际有限公司 | Methods for extracting and purifying sucralose intermediate |
| CN101709069A (en) * | 2009-08-06 | 2010-05-19 | 浙江工业大学 | Novel method for separating and purifying sucralose-6-ethyl ester |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106957345A (en) * | 2017-04-10 | 2017-07-18 | 王满堂 | Improve the production method of the ethyl ester yield of Sucralose 6 |
| CN106957345B (en) * | 2017-04-10 | 2019-07-09 | 王满堂 | Improve the production method of trichloro-cane-6-ethyl ester yield |
| CN108250255A (en) * | 2018-01-24 | 2018-07-06 | 山东康宝生化科技有限公司 | A kind of method for improving trichloro-cane-6-ethyl ester crystallization yield |
| CN109734755A (en) * | 2018-12-28 | 2019-05-10 | 山东三和维信生物科技有限公司 | A kind of Sucralose crystallization processes |
| EP4215539A4 (en) * | 2020-11-27 | 2024-01-17 | Anhui Jinhe Industrial Co., Ltd. | Method for purifying sucralose-6-ethyl ester |
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