CN105037449A - Crystallization method for sucralose - Google Patents
Crystallization method for sucralose Download PDFInfo
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- CN105037449A CN105037449A CN201510554216.7A CN201510554216A CN105037449A CN 105037449 A CN105037449 A CN 105037449A CN 201510554216 A CN201510554216 A CN 201510554216A CN 105037449 A CN105037449 A CN 105037449A
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Abstract
The invention relates to a crystallization method for sucralose and belongs to the technical field of production and processing of food additives. The method includes the steps that firstly, sucralose is dissolved and subjected to impurity removal, then, stir cooling is conducted, after an obtained solution is subjected to pressure reduction and water is steamed out, a 0.8 g/mL sucralose solution is prepared through deionized water, stir heat preservation is conducted, crystallization is conducted through ultrasound, and finally water is removed and sucralose crystals are obtained. The crystallization method has the advantages that the crystallization time is shortened by one time, the water content of the crystals is reduced by 3-4%, the obtained crystals are large in particle and glossy, and the operation steps are simple.
Description
Technical field
The present invention relates to a kind of crystallization method of Sucralose, belong to the process for processing technical field of foodstuff additive.
Background technology
Sucralose is the one of chloro sucrose, and it is a kind of novel sweeting agent, the functional sweetener of to be unique with sucrose be raw material, its sugariness is 600 times of sucrose, and it does not participate in body metabolism, and security is high, antagonism acid hydrolysis ability is strong, and these advantages make it become the preferred product in market.
At present, the crystallization method of Sucralose is mainly that solvent carries out crystallization with water, but this method also exists problems, crystallization time is long, usually needs a couple of days, and crystallization is incomplete, normal containing large-tonnage product in crystalline mother solution, the recovery of mother liquor is more loaded down with trivial details, and in product, moisture content is higher, and have impact on the stability of product.As publication number CN100567319, patent name " a kind of crystallization method of Sucralose ", set forth the organic solvent crystallization of Sucralose, make crystallization time shortening, yield raising, but find through us, this invention still also exists shortcoming: crystalline particle is comparatively thin, tarnish, can not get oarse-grained Sucralose.
Summary of the invention
The technical problem that the present invention mainly solves: for the method for existing Sucralose crystallization, crystallization time is long, and in crystallization, moisture content is low, the crystalline matt obtained, the problem that particle is little, provide a kind of crystallization method of Sucralose, the method passes through first decon, ultrasonic crystallization, the step crystallization Sucralose such as anhydrate, the method crystallization time is short, and the water ratio in product is low, and gained crystal grain is large.
In order to solve the problems of the technologies described above, the technical solution adopted in the present invention is, a kind of crystallization method of Sucralose, it is characterized in that concrete operation step is:
(1) weigh 200g purity be 95% Sucralose be placed in 500mL beaker, and add 250mL distilled water and dissolve at 70 ~ 75 DEG C, after end to be dissolved, cross after constant temperature 30 ~ 35min and filter insoluble impurities;
(2) sucralose solution at above-mentioned 70 ~ 75 DEG C being stirred cooling 2 ~ 3h to temperature is 55 DEG C, subsequently, carries out cooling stir with the speed of 5 DEG C/h, cooling is stopped when temperature is down to 18 DEG C, for subsequent use, when described cooling scope is 55 ~ 75 DEG C, stirring velocity is 50 ~ 55rpm; When cooling scope is 30 ~ 55 DEG C, stirring velocity is 40 ~ 45rpm; When cooling scope is 18 ~ 30 DEG C, stirring velocity is 30 ~ 35rpm;
(3) solution in the above-mentioned steps (2) of 100mL is got, after decompression steams the water of 50mL, the sucralose solution of 0.8g/mL is formed with deionized water preparation, it is 18 DEG C in temperature, stirring velocity is insulated and stirred 6h under the condition of 33 ~ 36rpm, after having stirred, stirring velocity is brought up to 40 ~ 45rpm insulated and stirred 3h, the ultrasonic field simultaneously above-mentioned sucralose solution being placed in 40kHz carries out crystallization;
(4) open whipping appts, occur namely slowly reducing stirring velocity with the speed of 2rpm/min until naked eyes can observe nucleus, until stop completely, crystal structure;
(5) to be crystallized complete after, the centrifuge through 4000r/min is separated after 10min, and being separated after supernatant liquid in temperature is 40 ~ 45 DEG C, and under vacuum tightness 0.09MPa, vacuum-drying 4 ~ 5h can obtain Sucralose xln.
The invention has the beneficial effects as follows:
(1) crystallization time shortens 1 times, and in crystal, water content reduces by 3 ~ 4%;
(2) crystal grain of gained is large, glossy;
(3) operation steps is simple.
Embodiment
First weigh 200g purity be 95% Sucralose be placed in 500mL beaker, and add 250mL distilled water and dissolve at 70 ~ 75 DEG C, after end to be dissolved, cross after constant temperature 30 ~ 35min and filter insoluble impurities; It is 55 DEG C that sucralose solution at above-mentioned 70 ~ 75 DEG C is stirred cooling 2 ~ 3h to temperature, subsequently, carries out cooling stir with the speed of 5 DEG C/h, cooling is stopped when temperature is down to 18 DEG C, for subsequent use, when described cooling scope is 55 ~ 75 DEG C, stirring velocity is 50 ~ 55rpm; When cooling scope is 30 ~ 55 DEG C, stirring velocity is 40 ~ 45rpm; When cooling scope is 18 ~ 30 DEG C, stirring velocity is 30 ~ 35rpm; Get the above-mentioned solution of 100mL again, after decompression steams the water of 50mL, the sucralose solution of 0.8g/mL is formed with deionized water preparation, it is 18 DEG C in temperature, stirring velocity is insulated and stirred 6h under the condition of 33 ~ 36rpm, after having stirred, stirring velocity is brought up to 40 ~ 45rpm, insulated and stirred 3h, the ultrasonic field simultaneously above-mentioned sucralose solution being placed in 40kHz carries out crystallization; Open whipping appts, occur namely slowly reducing stirring velocity with the speed of 2rpm/min until naked eyes can observe nucleus, until stop completely, crystal structure; To be crystallized complete after, the centrifuge through 4000r/min is separated after 10min, and being separated after supernatant liquid in temperature is 40 ~ 45 DEG C, and under vacuum tightness 0.09MPa, vacuum-drying 4 ~ 5h can obtain Sucralose xln.
Example 1
First weigh 200g purity be 95% Sucralose be placed in 500mL beaker, and add 250mL distilled water and dissolve at 75 DEG C, after end to be dissolved, cross after constant temperature 35min and filter insoluble impurities; Sucralose solution at above-mentioned 75 DEG C being stirred cooling 3h is 55 DEG C to temperature, and subsequently, carry out cooling stir with the speed of 5 DEG C/h, when temperature is down to 18 DEG C, stop cooling, for subsequent use, when described cooling is 55 DEG C, stirring velocity is 50rpm; Get the above-mentioned solution of 100mL again, after decompression steams the water of 50mL, the sucralose solution of 0.8g/mL is formed with deionized water preparation, it is 18 DEG C in temperature, stirring velocity is insulated and stirred 6h under the condition of 36rpm, after having stirred, stirring velocity is brought up to 45rpm, insulated and stirred 3h, the ultrasonic field simultaneously above-mentioned sucralose solution being placed in 40kHz carries out crystallization; Open whipping appts, occur namely slowly reducing stirring velocity with the speed of 2rpm/min until naked eyes can observe nucleus, until stop completely, crystal structure; To be crystallized complete after, the centrifuge through 4000r/min is separated after 10min, and being separated after supernatant liquid in temperature is 45 DEG C, under vacuum tightness 0.09MPa, vacuum-drying 4h can obtain Sucralose xln, and the crystal grain of gained is large, glossy, required time is short, only needs 1 day.
Example 2
First weigh 200g purity be 95% Sucralose be placed in 500mL beaker, and add 250mL distilled water and dissolve at 70 DEG C, after end to be dissolved, cross after constant temperature 30min and filter insoluble impurities; Sucralose solution at above-mentioned 70 DEG C being stirred cooling 2h is 55 DEG C to temperature, and subsequently, carry out cooling stir with the speed of 5 DEG C/h, when temperature is down to 18 DEG C, stop cooling, for subsequent use, when described cooling is 30 DEG C, stirring velocity is 40rpm; Get the above-mentioned solution of 100mL again, after decompression steams the water of 50mL, the sucralose solution of 0.8g/mL is formed with deionized water preparation, it is 18 DEG C in temperature, stirring velocity is under the condition of 33rpm, insulated and stirred 6h, brings up to 40rpm insulated and stirred 3h by stirring velocity after having stirred, and the ultrasonic field simultaneously above-mentioned sucralose solution being placed in 40kHz carries out crystallization; Open whipping appts, occur namely slowly reducing stirring velocity with the speed of 2rpm/min until naked eyes can observe nucleus, until stop completely, crystal structure; To be crystallized complete after, the centrifuge through 4000r/min is separated after 10min, and being separated after supernatant liquid in temperature is 40 DEG C, and under vacuum tightness 0.09MPa, vacuum-drying 4h can obtain Sucralose xln.The crystal grain of gained is large, and glossy, required time is short, only needs 20h.
Example 3
First weigh 200g purity be 95% Sucralose be placed in 500mL beaker, and add 250mL distilled water and dissolve at 72 DEG C, after end to be dissolved, cross after constant temperature 34min and filter insoluble impurities; Sucralose solution at above-mentioned 72 DEG C being stirred cooling 2h is 55 DEG C to temperature, and subsequently, carry out cooling stir with the speed of 5 DEG C/h, when temperature is down to 18 DEG C, stop cooling, for subsequent use, during described cooling 18 DEG C, stirring velocity is 30rpm; Get the above-mentioned solution of 100mL again, after decompression steams the water of 50mL, the sucralose solution of 0.8g/mL is formed with deionized water preparation, it is 18 DEG C in temperature, stirring velocity is insulated and stirred 6h under the condition of 34rpm, after having stirred, stirring velocity is brought up to 42rpm, insulated and stirred 3h, the ultrasonic field simultaneously above-mentioned sucralose solution being placed in 40kHz carries out crystallization; Open whipping appts, occur namely slowly reducing stirring velocity with the speed of 2rpm/min until naked eyes can observe nucleus, until stop completely, crystal structure; To be crystallized complete after, the centrifuge through 4000r/min is separated after 10min, and being separated after supernatant liquid in temperature is 42 DEG C, and under vacuum tightness 0.09MPa, vacuum-drying 4h can obtain Sucralose xln.The crystal grain of gained is large, and glossy, required time is short, only needs 21h.
Claims (1)
1. a crystallization method for Sucralose, is characterized in that concrete operation step is:
(1) weigh 200g purity be 95% Sucralose be placed in 500mL beaker, and add 250mL distilled water and dissolve at 70 ~ 75 DEG C, after end to be dissolved, cross after constant temperature 30 ~ 35min and filter insoluble impurities;
(2) sucralose solution at above-mentioned 70 ~ 75 DEG C being stirred cooling 2 ~ 3h to temperature is 55 DEG C, subsequently, carries out cooling stir with the speed of 5 DEG C/h, cooling is stopped when temperature is down to 18 DEG C, for subsequent use, when described cooling scope is 55 ~ 75 DEG C, stirring velocity is 50 ~ 55rpm; When cooling scope is 30 ~ 55 DEG C, stirring velocity is 40 ~ 45rpm; When cooling scope is 18 ~ 30 DEG C, stirring velocity is 30 ~ 35rpm;
(3) solution in the above-mentioned steps (2) of 100mL is got, after decompression steams the water of 50mL, the sucralose solution of 0.8g/mL is formed with deionized water preparation, it is 18 DEG C in temperature, stirring velocity is insulated and stirred 6h under the condition of 33 ~ 36rpm, after having stirred, stirring velocity is brought up to 40 ~ 45rpm, insulated and stirred 3h, the ultrasonic field simultaneously above-mentioned sucralose solution being placed in 40kHz carries out crystallization;
(4) open whipping appts, occur namely slowly reducing stirring velocity with the speed of 2rpm/min until naked eyes can observe nucleus, until stop completely, crystal structure;
(5) to be crystallized complete after, the centrifuge through 4000r/min is separated after 10min, and being separated after supernatant liquid in temperature is 40 ~ 45 DEG C, and under vacuum tightness 0.09MPa, vacuum-drying 4 ~ 5h can obtain Sucralose xln.
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| CN201510554216.7A CN105037449A (en) | 2015-09-02 | 2015-09-02 | Crystallization method for sucralose |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106474766A (en) * | 2016-11-30 | 2017-03-08 | 广东技术师范学院 | A kind of sucralose low energy consumption extraction equipment |
| CN109762030A (en) * | 2019-03-06 | 2019-05-17 | 福州大学 | A kind of method for crystallising of Sucralose |
| CN111138502A (en) * | 2019-12-31 | 2020-05-12 | 山东三和维信生物科技有限公司 | Crystallization process of large-particle sucralose |
| 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 |
| CN115433245A (en) * | 2022-09-13 | 2022-12-06 | 天津大学 | Crystallization method for improving flowability of sucralose |
-
2015
- 2015-09-02 CN CN201510554216.7A patent/CN105037449A/en not_active Withdrawn
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106474766A (en) * | 2016-11-30 | 2017-03-08 | 广东技术师范学院 | A kind of sucralose low energy consumption extraction equipment |
| CN109762030A (en) * | 2019-03-06 | 2019-05-17 | 福州大学 | A kind of method for crystallising of Sucralose |
| CN111138502A (en) * | 2019-12-31 | 2020-05-12 | 山东三和维信生物科技有限公司 | Crystallization process of large-particle sucralose |
| CN111138502B (en) * | 2019-12-31 | 2022-01-11 | 山东三和维信生物科技有限公司 | Crystallization process of large-particle sucralose |
| 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 |
| CN115433245A (en) * | 2022-09-13 | 2022-12-06 | 天津大学 | Crystallization method for improving flowability of sucralose |
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