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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 alkali catalysis requires a long reaction time and many impurities. The third method is to use alkali hydrolysis after the addition reaction of acid anhydride and glycidyl ether, but it is very easy to generate the self-polymerized by-product of glycidyl ether, and The important disadvantages of these existing methods are that there are many side reactions, odor, low purity, and luster. The subsequent refining and purification rely on traditional rectification methods and activated carbon decolorization. The investment in equipment is large, the cost is high, and the purity is low. It cannot be used as cosmetics and household care products. Additive use

Method used

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

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] In a 2000 ml four-neck flask equipped with a mechanical stirrer, a thermometer, and a dropping funnel, add 330 g of 2-ethylhexyl glycidyl ether, place the flask in a water bath, and control the temperature at 10 to 20°C while stirring. Add 175 grams of acetone and 10 grams of catalyst dropwise, and the time for dropping is 40 minutes. After keeping for 120 minutes, add 15 grams of methylamine aqueous solution and keep for 10 minutes to distill the remaining acetone under reduced pressure, and add 40 grams of formic acid to the remaining reactants. 50 grams of distilled water, heated in a water bath at 50-55 ° C for 180 minutes, let stand to separate the liquid, neutralized the oil phase with sodium bicarbonate to neutral, washed twice with water, added a stabilizer, and then carried out short-path distillation, the vacuum degree was controlled at 40 ~50Pa, collect the distillate with distillation temperature in the range of 135~145°C to obtain the high-purity ethylhexylg...

Embodiment 2

[0034] Replace the methylamine aqueous solution in example 1 with 20 grams of ammoniacal liquor, and it is with embodiment 1 with step, obtains high-purity ethylhexylglycerin of the present invention, through gas chromatography analysis, purity 99.5%, yield 89.0%, colorless and tasteless.

Embodiment 3

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

[0037] In a 2000 ml four-neck flask equipped with a mechanical stirrer, a thermometer, and a dropping funnel, add 330 grams of 2-ethylhexyl glycidyl ether, and place the flask in a water bath. Under stirring, the temperature is controlled at 10-20°C, and 175 grams of acetone and 15 grams of boron trifluoride ether catalyst are added dropwise at the same time. The dropwise addition time is 40 minutes. The reaction solution is brown, and the subsequent steps are the same as in Example 1. Analysis, purity 48.3%, yield 56%, color and luster is light brown, and smell is big, can not be used as the additive of daily chemical product.

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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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