A kind of purification method of sucrose-6-acetate

A purification method and an acetate technology are applied in the field of purification of sucrose-6-acetate, which can solve the problems of not too high purity, troublesome ion exchange resin processing, large amount of solvent, etc. The effect of large-scale industrial production and low equipment requirements

Active Publication Date: 2015-09-23
天津北方食品有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] US7626016 purifies sucrose-6-acetate by ion exchange method. This method uses strong acidic ion-exchange resin with a particle size of 50mesh to 100mesh as an adsorbent, and uses 70% acetone aqueous solution as an eluent to separate and purify sucrose-6-acetate Esters, this method requires a large amount of solvent, and the treatment of ion exchange resins is troublesome, and the purity is not too high; US20070227897 uses anhydrous methanol for recrystallization under heating and reflux conditions, then cools to room

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] A kind of purification method of sucrose-6-acetate, concrete steps are:

[0021] Remove most of the DMF from the DMF solution of sucrose-6-acetate under reduced pressure distillation to obtain the crude product of sucrose-6-acetate. Add isoamyl alcohol at 20°C, and a large amount of crystals are precipitated. Filtration, the precipitated crystals were dried in a vacuum oven, and the volume ratio of the used isoamyl alcohol to the crude product of sucrose-6-acetate was 3:1; 3.7 g of sucrose-6-acetate was obtained with a yield of 82%. The product was analyzed by phase chromatography, and the purity of sucrose-6-acetate was 92%.

[0022] Wherein, according to liquid chromatography, referring to the reference document US4889928, the sucrose-6-acetate is confirmed according to the retention time, and its content value is obtained according to the peak area ratio. Specific conditions are as follows: Zorbax NH 2 Column, mobile phase is V (water): V (acetonitrile) = 85:15, fl...

Embodiment 2

[0024] A kind of purification method of sucrose-6-acetate, concrete steps are:

[0025] Remove most of the DMF from the DMF solution of sucrose-6-acetate under reduced pressure distillation to obtain the crude product of sucrose-6-acetate. Add isoamyl alcohol at 20°C, and a large amount of crystals are precipitated. Filtration, the precipitated crystals were dried in a vacuum oven, the volume ratio of the used isoamyl alcohol to the crude product of sucrose-6-acetate was 2:1; 3.6g of sucrose-6-acetate was obtained, the yield was 80%, and the liquid The product was analyzed by phase chromatography, and the purity of sucrose-6-acetate was 90%.

Embodiment 3

[0027] A kind of purification method of sucrose-6-acetate, concrete steps are:

[0028] Remove most of the DMF from the DMF solution of sucrose-6-acetate under vacuum distillation to obtain the crude product of sucrose-6-acetate. Add isoamyl alcohol at 30°C, and a large amount of crystals are precipitated. Filtration, the precipitated crystals were dried in a vacuum oven, and the volume ratio of the used isoamyl alcohol to the crude sucrose-6-acetate was 2:1; 3.4 g of sucrose-6-acetate was obtained, with a yield of 76%. The product was analyzed by phase chromatography, and the purity of sucrose-6-acetate was 80%. The solubility of sucrose-6-acetate in isoamyl alcohol increases with increasing temperature.

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Abstract

The invention provides a purification method for cane sugar-6-acetate. The purification method comprises the specific steps of: adding isoamylol in a cane sugar-6-acetate crude product on the condition of a reaction temperature of 20-80 DEG C; separating out crystals, and filtering; and drying the separated crystals in a vacuum drying box, wherein the volume ratio of isoamylol to the cane sugar-6-acetate crude product is 1: 1 to 5: 1. According to the purification method, isoamylol is used as an extraction agent, isoamylol is a polar solvent, and the polarity of cane sugar is greater than the polarity of cane sugar-6-acetate, so that cane sugar-6-acetate can be separated from isoamylol; moreover, the needed amount is low, the required temperature is low, and the requirement on equipment in industrial production is low; simultaneously, the purification method is high in economic benefits and meets the need of large-scale industrial production.

Description

technical field [0001] The invention relates to a method for purifying an intermediate of sucralose, in particular to a method for purifying sucrose-6-acetate. Background technique [0002] Sucralose, the English name is Sucralose, is the only functional sweetener that uses sucrose as a raw material. The sweetness can reach more than 600 times that of sucrose. It is a non-nutritive, efficient and harmless sweetener. [0003] Sucralose is a non-hygroscopic white crystalline powder with high chemical stability in acidic solution and good stability under light and heat conditions. It is easily soluble in ethanol and has a good linear relationship between the refractive index and solubility. [0004] At present, the "single group protection method" is usually used to finally synthesize sucralose. The advantage of this method is that sucralose can be synthesized in three steps by the single-group protection method, with few steps, simple operation, and low requirements on proces...

Claims

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Application Information

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IPC IPC(8): C07H13/06C07H1/00
Inventor 赵温涛李胜彬谷正艳耿蔚华唐向阳曹世嘉齐欣常虹
Owner 天津北方食品有限公司
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