CN102336786A - High-efficiency crystallization method of trichlorosucrose - Google Patents
High-efficiency crystallization method of trichlorosucrose Download PDFInfo
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- CN102336786A CN102336786A CN2011103403034A CN201110340303A CN102336786A CN 102336786 A CN102336786 A CN 102336786A CN 2011103403034 A CN2011103403034 A CN 2011103403034A CN 201110340303 A CN201110340303 A CN 201110340303A CN 102336786 A CN102336786 A CN 102336786A
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Abstract
The invention discloses a high-efficiency crystallization method of trichlorosucrose, belonging to the field of compound treatment. The method comprises the following steps: holding trichlorosucrose solution with a certain of sugar degree within a certain temperature range to promote nucleation, and cooling according to a periodic procedure to promote crystal nucleus to grow quickly, thereby achieving the goal of high-efficiency crystallization. The invention solves the problems of incomplete crystallization, irregular crystal shape and low yield in the trichlorosucrose crystallization process, has the advantages of simple steps and high efficiency, and is very suitable for industrial production.
Description
Technical field
The present invention relates to the treatment process of compound, more specifically, is a kind of efficient crystallization method of TGS.
Background technology
TGS i.e. 4,1 ', 6 '-three chloro-4,1 '; 6 '-three deoxidation sucralose are a kind of novel sweeteners, are exactly with sucrose 4,1 '; 6 ' hydroxyl selectivity chloro makes, and its sugariness is 600 times of sucrose, and it does not participate in body metabolism, and making us interested especially is the lower calorie of its tool; Can substitute the used asccharin in the variant prodn (like food, candy, beverage, cough drop) fully; The chemicalstability of TGS is good, is difficult for pyrolysis or hydrolysis reaction take place, and in acidic solution, has good stability especially, is a kind of rising sweeting agent.
In the production process of TGS, crystallisation step is very crucial, directly has influence on product gas purity, production efficiency and yield, thereby further production cost of products is impacted.Have in traditional crystallization method for trichlorosucrose that crystallization is incomplete, crystalline form is irregular, yield is on the low side and problem such as color is bad, influence the quality of product.
Summary of the invention
The object of the invention is to provide a kind of efficient crystallization method of TGS, has that technology is simple, yield is high and the characteristics of good product quality.
The present invention realizes through following technique means: to TGS crystal low more characteristics of solubleness under the low more situation of temperature; Sucralose solution with certain pol is incubated to form nucleus earlier; Belong to the secondary nucleation process; Below programmed cooling to 25 ℃, guarantee sufficient crystallising, efficient is high, yield is high and good product quality.
The efficient crystallization method of TGS of the present invention comprises the steps:
(1) formation of nucleus: it is 68～72% that sucralose solution is concentrated into pol, and putting into chuck and keeping jacket temperature is 54～56 ℃, is incubated 1 hour, promotes the formation of nucleus, obtains forming the sucralose solution of nucleus;
(2) growth of nucleus: the sucralose solution to forming nucleus carries out programmed cooling, and at first the speed with 1 ℃/10min is lowered the temperature in 55～50 ℃ scope; Speed with 0.5 ℃/10min is lowered the temperature in 50～45 ℃ scope then, and in the time of 45 ℃, is incubated 1 hour; Again in 45～35 ℃ scope with the cooling of the speed of 1 ℃/6min, after circulating water cooling to 25 ℃, obtain crystal after centrifugal and dry.
According to method of the present invention TGS is carried out crystallization; Promote that earlier nucleus forms the quick growth that promotes nucleus again; Guarantee sufficient crystallising at a certain temperature; Can effectively avoid crystallization not exclusively, problem such as the product crystalline form is irregular and color is bad, and efficient is high, yield is high, product purity is high, has effectively shortened the production cycle of product and has reduced production cost; Step is simple, and mild condition is low for equipment requirements, is fit to very much suitability for industrialized production.
Embodiment
Below describe several preferred implementation of the present invention, but be not in order to limit the present invention.
Embodiment 1:
According to following method TGS is carried out crystallization:
(1) formation of nucleus: it is 72% that sucralose solution is concentrated into pol, and putting into chuck and keeping jacket temperature is 55 ℃, is incubated 1 hour, promotes the formation of nucleus, obtains forming the sucralose solution of nucleus;
(2) growth of nucleus: the sucralose solution to forming nucleus carries out programmed cooling, and at first the speed with 1 ℃/10min is lowered the temperature in 55～50 ℃ scope; Speed with 0.5 ℃/10min is lowered the temperature in 50～45 ℃ scope then, and in the time of 45 ℃, is incubated 1 hour; Again in 45～35 ℃ scope with the cooling of the speed of 1 ℃/6min, after circulating water cooling to 25 ℃, obtain crystal after centrifugal and dry.
For the effect of crystallization method of the present invention is described; Adopt direct decrease temperature crystalline method of the prior art embodiment 1 and spontaneous nucleation method embodiment 2 as a comparison as a comparison; Test comparison from aspects such as productive rate, purity, production cycle and yields, the result is as shown in table 1:
Table 1
Facts have proved; The crystallization method of TGS of the present invention compared to prior art, has that technology is simple, treatment condition are gentle, efficient is high, productive rate is high, with short production cycle, product purity is high and yield is high characteristics; And production cost is low, is fit to very much suitability for industrialized production.
Claims (1)
1. the efficient crystallization method of a TGS is characterized in that, comprises the steps:
(1) formation of nucleus: it is 68～72% that sucralose solution is concentrated into pol, and putting into chuck and keeping jacket temperature is 54～56 ℃, is incubated 1 hour, promotes the formation of nucleus, obtains forming the sucralose solution of nucleus;
(2) growth of nucleus: the sucralose solution to forming nucleus carries out programmed cooling, and at first the speed with 1 ℃/10min is lowered the temperature in 55～50 ℃ scope; Speed with 0.5 ℃/10min is lowered the temperature in 50～45 ℃ scope then, and in the time of 45 ℃, is incubated 1 hour; Again in 45～35 ℃ scope with the cooling of the speed of 1 ℃/6min, after circulating water cooling to 25 ℃, obtain crystal after centrifugal and dry.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2011103403034A CN102336786A (en) | 2011-11-01 | 2011-11-01 | High-efficiency crystallization method of trichlorosucrose |
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| CN2011103403034A CN102336786A (en) | 2011-11-01 | 2011-11-01 | High-efficiency crystallization method of trichlorosucrose |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112424176A (en) * | 2020-09-21 | 2021-02-26 | 安徽金禾实业股份有限公司 | Refining method of acesulfame potassium |
| CN112543760A (en) * | 2020-09-30 | 2021-03-23 | 安徽金禾实业股份有限公司 | Method for purifying sucralose |
| CN112961201A (en) * | 2021-03-29 | 2021-06-15 | 福州大学 | Crystallization method of spherical sucralose |
| CN114989231A (en) * | 2022-06-20 | 2022-09-02 | 新琪安科技股份有限公司 | Crystallization method of sucralose |
Citations (7)
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| US4343934A (en) * | 1979-12-18 | 1982-08-10 | Talres Development (N.A.) N.V. | Crystalline 4,1',6'-trichloro-4,1',6'-trideoxy-galactosucrose |
| US4362869A (en) * | 1907-12-02 | 1982-12-07 | Talres Development (N.A.) N.V. | Process for the preparation of 4,1',6'-trichloro-4,1',6'-trideoxygalactosucrose |
| WO2008012831A2 (en) * | 2006-03-22 | 2008-01-31 | V. B. Medicare Pvt. Ltd. | Novel crystallization methods and novel crystalline and amorphous forms of halogenated sugars |
| CN101210034A (en) * | 2006-12-27 | 2008-07-02 | 盐城捷康三氯蔗糖制造有限公司 | Crystallization method for trichlorosucrose |
| CN101284850A (en) * | 2008-05-27 | 2008-10-15 | 沈怀庭 | Purification and crystallization process of sucralose |
| WO2008150379A1 (en) * | 2007-06-04 | 2008-12-11 | Polymed Therapeutics, Inc. | Novel chlorination process for preparing sucralose |
| CN101759728A (en) * | 2010-01-08 | 2010-06-30 | 江苏巨邦制药有限公司 | Method for preparing and refining sucralose |
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2011
- 2011-11-01 CN CN2011103403034A patent/CN102336786A/en active Pending
Patent Citations (7)
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|---|---|---|---|---|
| US4362869A (en) * | 1907-12-02 | 1982-12-07 | Talres Development (N.A.) N.V. | Process for the preparation of 4,1',6'-trichloro-4,1',6'-trideoxygalactosucrose |
| US4343934A (en) * | 1979-12-18 | 1982-08-10 | Talres Development (N.A.) N.V. | Crystalline 4,1',6'-trichloro-4,1',6'-trideoxy-galactosucrose |
| WO2008012831A2 (en) * | 2006-03-22 | 2008-01-31 | V. B. Medicare Pvt. Ltd. | Novel crystallization methods and novel crystalline and amorphous forms of halogenated sugars |
| CN101210034A (en) * | 2006-12-27 | 2008-07-02 | 盐城捷康三氯蔗糖制造有限公司 | Crystallization method for trichlorosucrose |
| WO2008150379A1 (en) * | 2007-06-04 | 2008-12-11 | Polymed Therapeutics, Inc. | Novel chlorination process for preparing sucralose |
| CN101284850A (en) * | 2008-05-27 | 2008-10-15 | 沈怀庭 | Purification and crystallization process of sucralose |
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Non-Patent Citations (2)
| Title |
|---|
| N. BALAMURUGAN，等: "Growth of TGS crystals using uniaxially solution-crystallization method of Sankaranarayanan-Ramasamy", 《CRYST. RES. TECHNOL.》, vol. 42, no. 2, 10 January 2007 (2007-01-10), pages 151 - 156 * |
| 王国宇，等: "超声波对三氯蔗糖结晶过程的影响", 《食品科技》, vol. 36, no. 6, 30 June 2011 (2011-06-30), pages 108 - 111 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112424176A (en) * | 2020-09-21 | 2021-02-26 | 安徽金禾实业股份有限公司 | Refining method of acesulfame potassium |
| CN112543760A (en) * | 2020-09-30 | 2021-03-23 | 安徽金禾实业股份有限公司 | Method for purifying sucralose |
| WO2022067621A1 (en) * | 2020-09-30 | 2022-04-07 | 安徽金禾实业股份有限公司 | Sucralose purification method |
| CN112961201A (en) * | 2021-03-29 | 2021-06-15 | 福州大学 | Crystallization method of spherical sucralose |
| CN114989231A (en) * | 2022-06-20 | 2022-09-02 | 新琪安科技股份有限公司 | Crystallization method of sucralose |
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Application publication date: 20120201 |