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Purification method of sucrose fatty acid ester

A technology of sucrose fatty acid ester and purification method, applied in the field of purification of sucrose fatty acid ester, can solve the problems of ineffective removal of impurities, difficult removal of impurities, unstable sucrose ester, etc., and achieves short heating time, convenient environmental protection treatment, Good product color

Inactive Publication Date: 2010-07-21
浙江合糖科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] At present, the industrial production method of sucrose ester is sucrose ester transesterification method. The synthesis of sucrose ester by transesterification method is divided into solvent method and solvent-free method, but the products produced by these two methods contain sucrose monoester, sucrose diester and sucrose polyester. And impurities such as unreacted sucrose, fatty acid soap, fatty acid, fatty acid methyl ester and / or monoglyceride and / or fatty acid propylene glycol ester, catalyst, a kind of purified sucrose ester described in Chinese patent ZL200510006011.1 and European patent EP0448996 respectively The method is that the crude sucrose ester is dissolved in an organic solvent capable of dissolving it, and then 20 to 200 parts by weight of an alkaline earth metal compound is added to 100 parts of the crude sucrose ester to react; the alkaline earth metal compound is added in excess to make the sucrose ester After the purification reaction, the possibility of hydrolysis is very high, and the sucrose ester is unstable, which is not conducive to obtaining high-purity sucrose ester; alkaline earth metal compounds are generally insoluble in organic solvents, and directly react with impurity fatty acid soap or stearic acid in organic solvents, and the reaction is very fast. Difficult to carry out, impurities are not easy to remove, the reaction is not complete, and impurities cannot be effectively removed

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] 1. Synthesis of crude sucrose fatty acid ester by solvent-free method

[0020] 171 grams of sucrose, 150 grams of methyl stearate, 54 grams of potassium stearate and 22.5 grams of potassium carbonate were heated and stirred for 8 hours at a temperature of 140 to 145 ° C and a pressure of 2000 Pa, and cooled to obtain sucrose fatty acid Ester crude product 372.5 grams

[0021] 2. Pretreatment of the crude product of sucrose fatty acid ester

[0022] Take 300 grams of the above-mentioned crude product of sucrose fatty acid ester, add 200 milliliters of ethyl acetate and 200 milliliters of water, stir at 50° C. to dissolve it; adjust the pH to 3 with 10% citric acid in mass concentration, let stand, and remove the lower layer water; then add 100 milliliters of water to wash twice to remove residual sucrose, salt and water-soluble pigment; the upper organic solvent layer is distilled under reduced pressure at 95° C. to remove the organic solvent to obtain 176 grams of sucr...

Embodiment 2

[0032] 1. Synthesis of crude sucrose fatty acid ester by solvent-free method

[0033] 200 grams of sucrose, 150 grams of methyl stearate, 50 grams of potassium stearate and 25 grams of potassium carbonate were heated and stirred for 8 hours at a temperature of 140-145 °C and a pressure of 2000 Pa, and cooled to obtain a sucrose fatty acid product 398 grams.

[0034] 2. Pretreatment of the crude product of sucrose fatty acid ester: take 300 grams of the crude product of sucrose fatty acid ester, add 400 milliliters of methyl ethyl ketone and 200 milliliters of water, stir at 50°C to dissolve it; adjust the pH with 5% hydrochloric acid After 4, let it stand, and remove the lower layer of water; then add 200 ml of water to wash twice to remove residual sucrose, salt and water-soluble pigment; the upper organic solvent layer is distilled under reduced pressure at 95°C to remove the organic solvent to obtain sucrose 170 grams of fatty acid ester crude product, described sucrose fa...

Embodiment 3

[0044] 1. The crude product of sucrose fatty acid ester synthesized by dimethyl sulfoxide as a solvent

[0045] Get 250 grams of sucrose and dissolve in 750 milliliters of dimethyl sulfoxide, and add 75 grams of methyl stearate therein. 4 g of potassium carbonate was added to the mixture, and the reaction was carried out at 85°C for 4.5 hours, while the methanol generated in the reaction was distilled off under reduced pressure. 17 grams of stearic acid was added immediately after the reaction was completed, and it was concentrated and then dried under reduced pressure at 80° C. to obtain 345 grams of the crude product of sucrose fatty acid ester.

[0046] 2. Pretreatment of the crude product of sucrose fatty acid ester: take 300 grams of the above crude product of sucrose fatty acid ester, add 3000 milliliters of n-butanol and 200 milliliters of water, stir at 50°C to dissolve it; adjust the pH to 3 with 20% sulfuric acid After that, let it stand, and remove the lower layer ...

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Abstract

The invention relates to a purification method of a mixture containing sucrose fatty acid ester; the mixture containing sucrose fatty acid ester is prepared from a sucrose fatty acid ester crude product which is prepared from the preparation of sucrose fatty acid ester with solvent or without solvent; the sucrose fatty acid ester crude product is pre-treated and prepared, and then is purified to prepare the sucrose fatty acid ester; the purification step is to carry out secondary molecular distillation to the sucrose fatty acid ester crude product; the temperature of primary distillation is 100 to 140DEG C, the distillation pressure is 600 to 800Pa, the temperature of secondary distillation is 100 to 150DEG C and the pressure is 0.01 to 1Pa; light phase and heavy phase of secondary distillation are separated, and the heavy phase prepared is the purified sucrose fatty acid ester product. The purification process of the method of the invention has the advantages of short product heating time, good product color, high vacuum degree, little solvent residue in the product, reasonable production process, wastewater containing sugar and salt produced in the production process, and convenient environmental-friendly treatment.

Description

(1) Technical field [0001] The invention relates to a method for purifying sucrose fatty acid ester, in particular to a method for purifying sucrose fatty acid ester by molecular distillation. (2) Background technology [0002] Sucrose fatty acid ester (sucrose fatty acid ester) is an emulsifier with wide range of HLB (hydrophilic-lipophilic balance), good effect, high safety and wide application range. It is usually used in chemical products and daily chemical products. It is used as an additive in the production and processing of food and medicine. The World Health Organization (WHO), the Food Organization of the United Nations (FAO), the European Community, Japan, China and the United States have all approved sucrose ester as a food additive. [0003] Molecular distillation is a special liquid-liquid separation technology. It is different from traditional distillation which relies on the separation principle of boiling point difference, but relies on the difference in the...

Claims

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Application Information

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IPC IPC(8): C07H13/06C07H1/06
Inventor 姜国平严晓阳朱霄鹏
Owner 浙江合糖科技有限公司
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