Method for extracting sucrose fatty acid ester

The technology of a sucrose fatty acid ester and a purification method, which is applied in the field of purification of sucrose fatty acid ester, can solve the problems of large amount of alkaline earth metal compound added, impurity cannot be effectively removed, and impurity is difficult to remove, so as to achieve less impurity and low production cost , the effect of fast response time

Active Publication Date: 2005-08-17
杭州瑞霖化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] At present, the industrialized method of synthesizing sucrose esters is the transesterification method. The synthesis of sucrose esters by the transesterification method is divided into solvent method and solventless method, but the products produced by these two methods contain sucrose monoester, sucrose diester, sucrose polyester and Impurities such as unreacted residual sugar, soap body, fatty acid, fatty acid methyl ester, catalyzer, have described a kind of method of purifying sucrose ester in the European Patent Application of 1991, and this method is to dissolve sucrose ester crude product in can dissolving it In the organic solvent of 100 parts by weight of sucrose ester crude product, add 20 to 200 parts by weight of alkaline earth metal compound and react; Sucrose esters are unstable, which is not conducive to obtaining high-purity sucrose esters; alkaline earth metal compounds directly react with impurity soaps, the reaction is difficult to carry out, impurities are not easy to remove, the reaction is not thorough, and impurities cannot be effectively removed, so it can only be processed. Crude sucrose esters below 5%

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0017] The sucrose industrialized product A synthesized by the solventless transesterification method has the following crude product components:

[0018] Component Content (%)

[0019] Sucrose esters 48.0

[0020] Unreacted free sugar 30.1

[0021] Soap body 13.5

[0022] Fatty acids 3.8

[0023] Fatty acid methyl esters 2.7

[0024] Impurities such as catalysts 1.9

[0025] The monoester content of sucrose ester is 50.2%, the diester is 30.1%, and the polyester is 19.7%.

[0026] To 100 g of the above crude sucrose ester A, add 380 ml of butanone (c, p) and 220 ml of 8% Nacl aqueous solution, stir the mixture at 35° C. for 25 minutes, and separate the water layer. Adjust the pH to 5.9±0.3 with dilute sulfuric acid at 55°C, stir for 12 minutes, and remove the lower aqueous layer. Use anhydrous sodium sulfate to remove excess water in the organic phase, add 1 g of calcium oxide to the organic phase under stirring at 45°C for 40 minutes, filter and evaporate the clear li...

example 2

[0028] The sucrose industrialized product B synthesized by the solventless transesterification method has the following crude product components:

[0029] Component Content (%)

[0030] Sucrose esters 53.5

[0031] Unreacted free sugar 23.0

[0032] Soap body 16.1

[0033] Fatty acids 3.8

[0034] Fatty acid methyl ester 1.9

[0035] Impurities such as catalysts 1.7

[0036] The monoester content of sucrose ester is 60.2%, the diester is 23.7%, and the polyester is 16.1%.

[0037] To 100 g of the above crude sucrose ester B, add 400 ml of ethyl acetate (c, p) and 250 ml of 5% NaCl aqueous solution, stir the mixture at 60° C. for 25 minutes, and separate the water layer. Adjust the pH to 5.9±0.3 with dilute hydrochloric acid at 55°C, react for 12 minutes, and remove the lower aqueous layer. Use anhydrous sodium sulfate to remove excess water in the organic phase, add a total of 11 grams of a mixture of calcium oxide and calcium hydroxide (1: 2W / W) to the organic phase un...

example 3

[0039] The sucrose industrialized product C synthesized by the solventless transesterification method has the following crude product components:

[0040] Component Content (%)

[0041] Sucrose esters 60.2

[0042] Unreacted free sugar 18.8

[0043] Soap body 11.2

[0044] Fatty acids 3.9

[0045] Fatty acid methyl esters 4.0

[0046] Impurities such as catalysts 1.9

[0047] The monoester content of sucrose ester is 40.7%, the diester is 31.6%, and the polyester is 23.7%.

[0048]To 100 g of the above crude sucrose ester C, add 400 ml of n-butanol (c, p) and 220 ml of 4% NaCl aqueous solution, stir the mixture at 65° C. for 25 minutes, and separate the water layer. Adjust the pH to 6.2±0.3 with acetic acid at 55°C, react for 15 minutes, and remove the lower aqueous layer. Add 20% calcium chloride solution to the organic phase at 100°C until the pH reaches 6.5±0.3, stir and react for 25 minutes, obtain the clear liquid of the organic phase by centrifugation, and evapora...

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Abstract

The sucrose fatty acid ester purifying process includes the following steps: dissolving crude sucrose fatty acid ester in organic solvent capable of being separated from water to obtain crude product solution, dripping dilute acid solution while stirring at 30-80 deg.c to pH 5.5-6.5, eliminating water to obtain acidified crude product solution, adding alkali earth metal compound while stirring for reaction at 40-110 deg.c of 10-180 min, centrifugating, depositing or filtering to eliminate produced solid aliphatic salt, and heating and decompressing distillation to obtain purified sucrose fatty acid ester product. The process is reasonable, high in purifying effect, short in reaction time, less in side reaction, wide in application range and low in production cost.

Description

technical field [0001] The invention relates to a method for purifying esters, in particular to a method for purifying sucrose fatty acid esters. Background technique [0002] At present, the industrialized method of synthesizing sucrose esters is the transesterification method. The synthesis of sucrose esters by the transesterification method is divided into solvent method and solventless method, but the products produced by these two methods contain sucrose monoester, sucrose diester, sucrose polyester and Impurities such as unreacted residual sugar, soap body, fatty acid, fatty acid methyl ester, catalyzer, have described a kind of method of purifying sucrose ester in the European Patent Application of 1991, and this method is to dissolve sucrose ester crude product in can dissolving it In the organic solvent of 100 parts by weight of sucrose ester crude product, add 20 to 200 parts by weight of alkaline earth metal compound and react; Sucrose esters are unstable, which ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H1/06C07H13/06
Inventor 袁长贵
Owner 杭州瑞霖化工有限公司
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