CN109762030A - A kind of method for crystallising of Sucralose - Google Patents
A kind of method for crystallising of Sucralose Download PDFInfo
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- CN109762030A CN109762030A CN201910168241.XA CN201910168241A CN109762030A CN 109762030 A CN109762030 A CN 109762030A CN 201910168241 A CN201910168241 A CN 201910168241A CN 109762030 A CN109762030 A CN 109762030A
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- sucralose
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Abstract
The invention discloses a kind of method for crystallising of Sucralose, includes the following steps: for a kind of pure solvent and the thick solution of Sucralose to be mixed, be filtered to remove impurity, obtain Sucralose coarse raw materials；A kind of mixed solvent is added in Sucralose coarse raw materials, after heating is stirred to react a period of time, is cooled down with certain rate；It is stood after cooling, Sucralose crystalline solid is obtained by filtration.4 Crystallization of the invention is simply mild, and crystallization time is short, and production cost is low, is conducive to industrialized production, and obtained sucralose purity is high, and crystal grain is big, has a vast market application prospect.
Description
Technical field
The invention belongs to food applications fields, and in particular to a kind of method for crystallising of Sucralose.
Background technique
Sucralose is a kind of novel non-nutritive sweeteners, chemistry entitled 4,1 ', 6 '-three chloro- 4,1 ', 6 '-three
Deoxy-galactose, three hydroxyls for 4,1 ', 6 ' positions on sucrose molecule are replaced by three chlorine atoms, have high sugariness,
The advantages that empty calory, is widely used in the food industry.
US5298611 elaborates that a kind of method using pelletizer manufacture Sucralose spheroidal cementite, the method effectively increase
Add the mobility of Sucralose, reduce dust, but increases processing step and production cost；CN101260126 elaborates one
The side that kind crystallizes Sucralose solid or concentrate with the mixed solvent that alcohols solvent or alcohols and other solvents form
Method, but this method requires the production time long, reduces production efficiency；CN101210034 elaborates one kind with two kinds of boiling point differences
The method that biggish mixed solvent is crystallized, volatilize low boiling point solvent at temperature appropriate and vacuum degree condition, stood
Filter is dried to obtain Sucralose crystallization, but since this crosses range request vacuum degree condition, more demanding to reaction unit.
Summary of the invention
It is an object of the invention to overcome the deficiencies of the prior art and provide a kind of Sucralose crystallization sides being simple and efficient
Method.
The method for crystallising of Sucralose provided by the invention includes the following steps:
4 h are mixed in a kind of pure solvent and the thick solution of Sucralose under room temperature, impurity is filtered to remove, obtains Sucralose
Coarse raw materials；A kind of mixed solvent is added in Sucralose coarse raw materials, after heating is stirred to react a period of time, with certain rate
It is cooled to 20oC；2 h are stood after cooling, filtering vacuum is dried to obtain Sucralose crystalline solid.
A kind of above-mentioned pure solvent is appointing in methyl acetate, ethyl acetate, isopropyl ester, butyl acetate or sec-butyl acetate
It is a kind of.
The volume ratio of a kind of above-mentioned pure solvent and the thick solution of Sucralose is 2:1.
Above-mentioned mixed solvent is water and a kind of organic solvent；Wherein organic solvent is methanol, ethyl alcohol, isopropanol or Zhong Ding
Any one of alcohol.
The volume ratio of above-mentioned mixed solvent and Sucralose coarse raw materials is 1:1.
The mol ratio of above-mentioned in the mixed solvent water and organic solvent is 3:7 ~ 7:3.
The reaction temperature of above-mentioned heating stirring is 60 ~ 80oC；Reaction time is 2-6 hours.
Above-mentioned rate of temperature fall is 5-10 oC/ hours.
4 Crystallization of the invention is simply mild, and crystallization time is short, and production cost is low, is conducive to industrialized production,
Obtained sucralose purity is high, and crystal grain is big, has a vast market application prospect.
The problem of for existing crystallization method for trichlorosucrose, inventor purify trichlorine sugarcane using a kind of pure solvent
The thick solution of sugar.After pure solvent is added, the solubility property of Sucralose is not exposed to influences, but its weaker polarity, hydrogen bond for by
Body tendency and lesser cohesion energy density can effectively weaken the interaction of itself and impurity in the thick solution of Sucralose, reduce impurity
Solubility in sucralose solution improves the crystallization purity of Sucralose so that impurity be precipitated.It is described in the present invention
Pure solvent is preferably any one of methyl acetate, ethyl acetate, isopropyl ester, butyl acetate, sec-butyl acetate, more preferably
Any one of methyl acetate, ethyl acetate, sec-butyl acetate.
Further, the present invention crystallizes Sucralose using a kind of mixed solvent, using between solvent molecule altogether it is molten
Agent effect enhances the interaction of solvent and Sucralose, be conducive to improve Sucralose in the mixed solvent solubility,
Improve the crystallization yield of Sucralose.In the present invention, the mixed solvent is water and a kind of organic solvent；Organic solvent is first
Any one of alcohol, ethyl alcohol, isopropanol or sec-butyl alcohol.
Further, for the mol ratio of in the mixed solvent water and organic solvent in 3:7 ~ 7:3, mixed solvent is to trichlorine
Sucrose can generate a unique co -solvent effect, cause the solubility of Sucralose small at low temperature, at high temperature greatly, thus
Be conducive to crystallize；When the mol ratio of solvent is less than 3:7 or is greater than 7:3, co -solvent effect is destroyed, the dissolution of Sucralose
Degree variation tends towards stability as the temperature increases, is unfavorable for crystallizing.
Further, the crystallization rate of temperature fall range in the present invention is 5-10oC/ hours.When rate of temperature fall is small lower than 5oC/
Constantly, Metastable zone width is narrow, causes crystallization operation condition harsh, is unfavorable for industrial operation；When cooling rate is higher than 10 o
At C/ hours, the degree of supersaturation of system quickly exceeds the supersaturated point of crystal nucleation, causes the induction period of crystal nucleation to increase, makes
Increased costs.
Beneficial effects of the present invention:
The 4 Crystallization of Sucralose of the present invention is simple, mild, and crystallization time is short, and production cost is low, is conducive to industrialize
Production, obtained sucralose purity is high, and crystal grain is big, has a vast market application prospect.
Detailed description of the invention
Fig. 1 is Sucralose crystal scanning electron microscope (SEM) photograph.
Fig. 2 is the relationship of solubility and temperature of the Sucralose in methanol and sec-butyl acetate.
Fig. 3 is the relationship of solubility and proportion of the Sucralose in water-methanol mixed solution.
Specific embodiment
The present invention is explained in detail below with reference to specific example.
Embodiment 1
20 mL(24g) the thick solution of Sucralose is added methyl acetate 40mL and 4 h is mixed under room temperature, it is filtered to remove impurity；
The 20mL water-methanol mixed solution that mol ratio is 3:7 is added, is warming up to 60oC, after being stirred to react 6 hours, per hour with 5oC
Rate, be cooled to 20 oC；It is filtered after standing 2 h, vacuum drying obtains Sucralose crystal 20.4g, and crystallization yield is
85.0%, purity 98.2%, 40 mesh of average grain diameter.The scanning electron microscope (SEM) photograph of preparation gained Sucralose crystal is shown in Fig. 1.
Embodiment 2
20 mL(24g) the thick solution of Sucralose is added sec-butyl acetate 40mL and 4 h is mixed under room temperature, be filtered to remove miscellaneous
Matter；The 20mL water-ethanol mixed solution that mol ratio is 7:3 is added, is warming up to 80oC, is stirred to react 2.5 hours, it is every with 10oC
The rate of hour, is cooled to 20 oC；It is filtered after standing 2 h, vacuum drying obtains Sucralose crystal 19.5g.Crystallization yield is
81.25%, purity 98.5%, 45 mesh of average grain diameter.
Embodiment 3
20 mL(24g) the thick solution of Sucralose is added ethyl acetate 40mL and 4 h is mixed under room temperature, it is filtered to remove impurity；
The 20mL water-methanol mixed solution that mol ratio is 5:5 is added, is warming up to 75oC, is stirred to react 4 hours, per hour with 8 oC
Rate, be cooled to 20 oC；It is filtered after standing 2 h, vacuum drying obtains Sucralose crystal 22.1g, and crystallization yield is
92.08%, purity 98.8%, 38 mesh of average grain diameter.
The relationship of solubility and temperature of 4 Sucralose of embodiment in methanol and sec-butyl acetate
The Sucralose solid of excessive addition, constant temperature in the solid-liquid phase equilibrium still for being preinstalled with 10 mL methanol or sec-butyl acetate
Water-bath control stops stirring after solution reaches saturation, stands 2 h, take supernatant liquor, efficiently in 30oC, 4 h of magnetic agitation
Liquid chromatogram carries out quantitative analysis, obtains molar solubility of the Sucralose under 30 oC in methanol or sec-butyl acetate.It takes
It is warming room every the above-mentioned experimental procedure of repetition, temperature stops reaction when rising to 60 oC that sample, which is finished using 5 oC,.
The relationship of solubility and temperature of the Sucralose in methanol and sec-butyl acetate is shown in Fig. 2.Fig. 2 is the result shows that trichlorine
Solubility of the sucrose in methanol and sec-butyl acetate all increases as temperature increases, and the dissolution of Sucralose in methyl alcohol
Degree is greater than its solubility in sec-butyl acetate.
The relationship of solubility and proportion of 5 Sucralose of embodiment in water-methanol mixed solution
The trichlorine of excessive addition in the solid-liquid phase equilibrium still for be preinstalled with 10mL water-methanol mixed solution (mol ratio 1:9)
Sucrose solids, water bath with thermostatic control control stop stirring after solution reaches saturation, stand 2 h, take in 45oC, 4 h of magnetic agitation
Supernatant liquor, high performance liquid chromatography carry out quantitative analysis, and it is molten in the water-methanol mixing that mol ratio is 1:9 to obtain Sucralose
Solubility in liquid.Sampling finishes, successively change water-methanol mixed solution mol ratio (1:9,2:8,3:7,4:6,5:5,
6:4,7:3,8:2,9:1) above-mentioned experimental procedure is repeated, until stopping reaction when mol ratio is 9:1.
The relationship of solubility and proportion of the Sucralose in water-methanol mixed solution is shown in Fig. 3.Fig. 3 is the result shows that trichlorine
Solubility of the sucrose in the range that the mol ratio of water-methanol mixed solution is 3:7 ~ 7:3 is good.
Claims (8)
1. a kind of method for crystallising of Sucralose, which comprises the steps of: by a kind of pure solvent and Sucralose
Thick solution is mixed, and is filtered to remove impurity, obtains Sucralose coarse raw materials；A kind of mixing is added in Sucralose coarse raw materials
Solvent after heating is stirred to react a period of time, is cooled down with certain rate；It is stood after cooling, Sucralose knot is obtained by filtration
Crystal.
2. method according to claim 1, it is characterised in that: a kind of pure solvent is methyl acetate, acetic acid second
Any one of ester, isopropyl ester, butyl acetate or sec-butyl acetate.
3. method according to claim 1, it is characterised in that: a kind of body of pure solvent and the thick solution of Sucralose
Product is than being 2:1.
4. method according to claim 1, it is characterised in that: the mixed solvent is water and a kind of organic solvent；Have
Solvent is any one of methanol, ethyl alcohol, isopropanol or sec-butyl alcohol.
5. method according to claim 1, it is characterised in that: the volume of the mixed solvent and Sucralose coarse raw materials
Than for 1:1.
6. method according to claim 4, it is characterised in that: the in the mixed solvent water and organic solvent mole are matched
Than for 3:7 ~ 7:3.
7. method according to claim 1, it is characterised in that: the reaction temperature of the heating stirring is 60 ~ 80oC；Instead
It is 2-6 hours between seasonable.
8. method according to claim 1, it is characterised in that: the rate of temperature fall be 5-10 oC per hour.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114014897A (en) * | 2021-12-20 | 2022-02-08 | 安徽金禾实业股份有限公司 | Purification and crystallization method of sucralose |
| CN115433245A (en) * | 2022-09-13 | 2022-12-06 | 天津大学 | Crystallization method for improving flowability of sucralose |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1486326A (en) * | 2000-11-17 | 2004-03-31 | 麦克尼尔-Ppc公司 | Sucralose composition and process for its preparation |
| CN101104626A (en) * | 2006-07-12 | 2008-01-16 | 上海迪赛诺维生素有限公司 | Crystallization method for sucrose trichloride |
| 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 |
| CN101260126A (en) * | 2007-03-06 | 2008-09-10 | 盐城捷康三氯蔗糖制造有限公司 | Crystallization method for trichlorosucrose |
| WO2009124113A1 (en) * | 2008-04-03 | 2009-10-08 | Tate & Lyle Technology Ltd. | Extraction of less polar impurities from sucralose containing aqueous feed streams |
| CN102391319A (en) * | 2011-10-14 | 2012-03-28 | 溧阳维信化学有限公司 | Trichlorosucrose crystallizing method |
| CN105037449A (en) * | 2015-09-02 | 2015-11-11 | 常州市长宇实用气体有限公司 | Crystallization method for sucralose |
-
2019
- 2019-03-06 CN CN201910168241.XA patent/CN109762030A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1486326A (en) * | 2000-11-17 | 2004-03-31 | 麦克尼尔-Ppc公司 | Sucralose composition and process for its preparation |
| CN101104626A (en) * | 2006-07-12 | 2008-01-16 | 上海迪赛诺维生素有限公司 | Crystallization method for sucrose trichloride |
| 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 |
| CN101260126A (en) * | 2007-03-06 | 2008-09-10 | 盐城捷康三氯蔗糖制造有限公司 | Crystallization method for trichlorosucrose |
| WO2009124113A1 (en) * | 2008-04-03 | 2009-10-08 | Tate & Lyle Technology Ltd. | Extraction of less polar impurities from sucralose containing aqueous feed streams |
| CN102391319A (en) * | 2011-10-14 | 2012-03-28 | 溧阳维信化学有限公司 | Trichlorosucrose crystallizing method |
| CN105037449A (en) * | 2015-09-02 | 2015-11-11 | 常州市长宇实用气体有限公司 | Crystallization method for sucralose |
Non-Patent Citations (2)
| Title |
|---|
| 关志宇主编: "《药物制剂辅料与包装材料》", 31 January 2017, 中国医药科技出版社 * |
| 潘浩然等: ""三氯蔗糖-6-乙酸酯醇解制三氯蔗糖及结晶工艺优化"", 《食品工业科技》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114014897A (en) * | 2021-12-20 | 2022-02-08 | 安徽金禾实业股份有限公司 | Purification and 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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