Method for preparing high-purity ethylhexylglycerin

An ethylhexylglycerol, high-purity technology, applied in ether preparation, organic chemistry and other directions, can solve the problems of long reaction time, easy oxidation and discoloration, difficult separation and purification, etc., to reduce energy consumption and raw material costs, and facilitate large-scale production. , the effect of a good preparation process

Active Publication Date: 2015-08-05
SHAANXI RES DESIGN INST OF PETROLEUM CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Ethylhexylglycerin has a boiling point of about 300°C, is easy to oxidize and change color, is easy to polymerize during synthesis, and is difficult to separate and purify. In addition, ethylhexylglycerin with high impurity content has deep color and odor. Some impurities will affect toxicological safety and cannot be used as a daily At present, ethylhexylglycerin can be produced through etherification technology. One is to open the epoxy group of ethylhexyl glycidyl ether for carbonyl addition by catalysis, and then hydrolyze. The other method is to combine alcohol and glycidyl ether in The preparation of ethylhexylglycerin under acid or alk

Method used

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  • Method for preparing high-purity ethylhexylglycerin
  • Method for preparing high-purity ethylhexylglycerin

Examples

Experimental program
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Example Embodiment

[0031] Example 1

[0032] In a 2000 ml four-necked flask equipped with a mechanical stirrer, a thermometer and a dropping funnel, add 330 g of 2-ethylhexyl glycidyl ether. The flask is placed in a water bath and the temperature is controlled at 10-20°C while stirring. Add 175 grams of acetone and 10 grams of catalyst dropwise for 40 minutes. After holding for 120 minutes, add 15 grams of methylamine aqueous solution, hold for 10 minutes, and distill off the remaining acetone under reduced pressure. Add 40 grams of formic acid to the remaining reactants. Distilled water 50 grams, heated water bath at 50 ~ 55 ℃ to react for 180 minutes, stand still to separate the liquid, the oil phase is neutralized with sodium bicarbonate to neutrality, after washing twice with water, add stabilizer, and then perform short-path distillation, the vacuum degree is controlled at 40 ~50Pa, collect fractions with a distillation temperature in the range of 135-145°C to obtain the high-purity ethylhexyl...

Example Embodiment

[0033] Example 2

[0034] Using 20 grams of ammonia to replace the methylamine aqueous solution in Example 1, the same steps as in Example 1 were used to obtain the high-purity ethylhexyl glycerol of the present invention. After gas chromatography analysis, the purity was 99.5%, the yield was 89.0%, and it was colorless and tasteless.

Example Embodiment

[0035] Example 3

[0036] Compared with Example 1, no terminator was added.

[0037] In a 2000 ml four-necked flask equipped with a mechanical stirrer, a thermometer, and a dropping funnel, 330 g of 2-ethylhexyl glycidyl ether was added, and the flask was placed in a water bath. While stirring, the temperature was controlled at 10-20℃, and 175g of acetone and 15g of boron trifluoride ether catalyst were added dropwise. The addition time was 40 minutes. The reaction solution was brown. The subsequent steps were the same as in Example 1. The product was subjected to gas chromatography. Analysis shows that the purity is 48.3%, the yield is 56%, the color is light brown, the smell is big, and it cannot be used as an additive for daily chemical products.

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Abstract

The invention provides a method for preparing high-purity ethylhexylglycerin. According to the method, an intermediate 4-alkoxymethyl-1,3-dioxoane is generated from 2-ethylhexylglycidyl ether and acetone under the action of boron trifluoride diethyl etherate, a terminator is added in good time before hydrolysis, and after liquid separation, an oil-phase substance is neutralized by use of sodium hydrogen carbonate and then washed, next, a stabilizer is added, and finally, the high-purity ethylhexylglycerin is obtained by use of short-path distillation. The method is suitable for cosmetic additives and suitable for large-scale industrial production, and has the advantages of simple process, small energy consumption, product yield of greater than 88%, purity of 99.3%, no color and no taste, and the like.

Description

technical field [0001] The invention belongs to the field of preservatives and relates to a method for preparing high-purity ethylhexylglycerin. Background technique [0002] Ethylhexylglycerin is a new multifunctional cosmetic additive with antiseptic effect and moisturizing and deodorizing effect. As the toxicological safety of various traditional preservatives has been questioned more and more, as a green, non-irritating, antiseptic effect The emergence of ethylhexylglycerin brings hope to people, especially the use of its synergistic effect with other traditional preservatives in daily chemical product systems can greatly reduce the amount of traditional preservatives added and significantly reduce the toxicity of the preservative system. Its biggest highlight is its antiseptic effect, non-irritating skin characteristics, moisturizing and moisturizing effect, and can enhance the ability of traditional preservatives, so that ethylhexylglycerin will play an important role ...

Claims

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Application Information

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IPC IPC(8): C07C41/01C07C43/13
CPCC07C41/01C07D317/22C07C43/13
Inventor 李程碑杨杰王和平杨俊伟
Owner SHAANXI RES DESIGN INST OF PETROLEUM CHEM IND
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