Method for preparing erucic acid sucrose ester

A technology of sucrose erucate and methyl erucate, which is applied in chemical instruments and methods, sugar derivatives, sugar derivatives, etc., can solve problems affecting product purity and color, difficulty in industrial production, and yield decline , to achieve the effect of good emulsifying performance, high monoester content, and simple separation and purification process

Inactive Publication Date: 2010-06-23
ZHEJIANG NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The solvents dimethylformamide and dimethyl sulfoxide used in the solvent method have a high boiling point and certain toxicity, and their residues in the product will directly affect the quality of the finished product and the use in food and medicine; the melting method uses more than The reaction at a high temperature of 160°C causes the sucrose to decompose and color, which not only affects the purity and color of the product, but also reduces the yield; US3205150 and US3312684 disclose the process of preparing by microbial methods, but there are still many ways to realize industrial production. No small difficulty

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] a. Add 100 grams of erucic acid and 9.6 grams of methanol in a 1000 ml flask, under the catalysis of 5 grams of concentrated sulfuric acid, reflux for 8 hours, add sodium carbonate to adjust the pH value to 7, distill and recover excess methanol, and wash the remaining liquid with water When the pH value of the aqueous layer was 7, the upper organic layer was dehydrated under reduced pressure to obtain 102 g of methyl erucate with an esterification rate of 97.9%.

[0024] B, in the there-necked flask with stirring of 1000 milliliters, add the methyl erucate 80 grams that step a makes and potassium erucate soap 8.5 grams (potassium erucate soap is made of erucic acid and potassium hydroxide according to the amount of substance 1 : 1 is prepared by neutralization reaction, the same below), vacuum degree -0.09~-0.1Mpa, warming up to 120 ± 2 ℃, then adding 94 grams of sucrose powder (above 100 mesh) and potassium carbonate 9.4 grams, raising the temperature to 122±2°C, main...

Embodiment 2

[0026] a. Add 100 grams of erucic acid and 96 grams of methanol in a 1000 ml flask, under the catalysis of 10 grams of concentrated sulfuric acid, reflux for 8 hours, add sodium carbonate to adjust the pH value to 7, distill and recover excess methanol, and wash the remaining liquid with water When the pH of the aqueous layer was 7, the upper organic layer was dehydrated under reduced pressure to obtain 102.5 g of methyl erucate with an esterification rate of 98.6%.

[0027] b. In a 1000 ml three-neck flask with stirring, add 80 grams of methyl erucate and 34 grams of potassium erucate soap prepared in step a, vacuum -0.09~-0.1Mpa, and heat up to 102±2°C, Then add 168 grams of sucrose powder (more than 100 mesh) and 16.8 grams of potassium carbonate, raise the temperature to 148 ± 2 ° C, keep the vacuum degree -0.095 ~ -0.1Mpa, stir and react for 5 hours to obtain 275 g of crude sucrose erucate. Then add 825 grams of 5wt% sodium chloride aqueous solution, stir evenly at 33 to ...

Embodiment 3

[0029] a. Add 100 grams of erucic acid and 9.6 grams of methanol in a 1000 ml flask, under the catalysis of 10 grams of concentrated sulfuric acid, reflux reaction for 10 hours, add sodium carbonate to adjust the pH value to 7, after distilling and recovering excess methanol, wash the remaining liquid with water When the pH value of the aqueous layer was 7, the upper organic layer was dehydrated under reduced pressure to obtain 103 g of methyl erucate with an esterification rate of 99%.

[0030] b. In a 1000 ml three-neck flask with stirring, add 80 grams of methyl erucate and 8.5 grams of potassium erucate soap prepared in step a, vacuum -0.09~-0.1Mpa, heat up to 120±2°C, Then add 94 grams of sucrose powder (above 100 mesh) and 4 grams of potassium methylate, raise the temperature to 148±2° C., keep a vacuum of -0.095~-0.1 Mpa, stir and react for 4 hours to obtain 179 g of crude sucrose erucate. Then add 360 grams of 30wt% aqueous sodium chloride solution, stir evenly at 37 t...

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PUM

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Abstract

The invention discloses a method for preparing erucic acid sucrose ester, and the method comprises the following steps: a. erucic acid and methyl alcohol are subjected to esterification reaction by using concentrated sulfuric acid as catalyst, reflux reaction is carried out for 6-10 hours, and after the reaction is finished, the reaction solution is post-processed to obtain erucic acid methyl ester; b. the erucic acid methyl ester obtained in step a is added with erucic acid potash soap and sucrose to react for 2-6 hours while stirring in the presence of alkali catalyst at the reaction temperature of 120-150 DEG C and under the vacuum degree of minus 0.09-minus 0.1MPa, thus obtaining crude product of the erucic acid sucrose ester which is then purified to obtain the erucic acid sucrose ester; and the alkali catalyst is potassium carbonate, potassium methoxide, potassium ethoxide, sodium methoxide or potassium hydroxide. The prepared erucic acid sucrose ester has high monoester content and good emulsifying property, and the separation and purification process is simple, thus being suitable for industrial production.

Description

(1) Technical field [0001] The invention relates to a preparation method of sucrose erucate. (2) Background technology [0002] Sucrose Erucate is a non-ionic surfactant synthesized from sucrose and erucic acid. It has good emulsifying, dispersing, wetting, foaming and washing properties, as well as adjusting viscosity, preventing aging and preventing crystallization. It is now Widely used in food, cosmetics, bioengineering enzyme preparations, medicines, synthetic resins, dyes, pesticides, daily chemicals and other fields. [0003] The chemical name of erucic acid is cis-22-13-enoic acid, which is widely found in cruciferous oils such as rapeseed and mustard. Sucrose and natural oils from animals and plants are renewable resources that are abundant in nature. The price is low, and the sugar-based natural surfactant derived from it has ideal biodegradation and human safety, so sucrose erucate is a green surfactant. In China, the production of sucrose fatty acid esters is m...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H13/06
Inventor 郑绍成严晓阳陈晓余晓红盛含晶
Owner ZHEJIANG NORMAL UNIVERSITY
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