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Preparation method of ethylhexylglycerin

A technology of ethylhexylglycerol and preparation steps is applied in the directions of ether preparation, ester reaction preparation of ether, ether separation/purification, etc., can solve problems such as high cost, numerous processes, complicated operation, etc., and achieve high synthesis yield and product purity , the effect of simple process

Active Publication Date: 2021-05-07
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

Because this process needs to use 2-ethylhexyl glycidyl ester with high cost as the initial raw material, the cost of the final product is too high, and there are many defects in the synthesis process, such as complex operation.
The above-mentioned defects have largely limited the popularization and use of ethylhexylglycerin as a new multifunctional additive in the cosmetics and daily chemical industry

Method used

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  • Preparation method of ethylhexylglycerin
  • Preparation method of ethylhexylglycerin
  • Preparation method of ethylhexylglycerin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Add 65g (0.5mol) of isooctyl alcohol and 60.8g (0.5mol) of 3-chloro-1,2-propanediol into a 250ml three-necked flask equipped with a spherical condenser and a thermometer, stir, keep warm to 20°C, and add dropwise for 30 minutes Complete 112g (0.5mol) of 25% potassium hydroxide aqueous solution, heat insulation reaction for 2h, stop the reaction, adjust the pH value to neutrality (pH value=7) with hydrochloric acid solution, at 20°C, use a separatory funnel to separate the product Carry out oil-water separation, let go of the water phase, wash the organic phase twice with 100ml of water, separate the organic phase, and collect fractions at 138±3°C through molecular distillation equipment at a vacuum degree of 40-50Pa to obtain 58g of colorless transparent liquid Shape ethylhexylglycerin, through gas chromatography analysis, the purity of ethylhexylglycerin is 99.0%, and the yield is 56.9%.

Embodiment 2

[0019] Add 65g (0.5mol) of isooctyl alcohol and 60.8g (0.5mol) of 3-chloro-1,2-propanediol into a 250ml three-necked flask equipped with a spherical condenser and a thermometer, stir, heat up to 40°C, and drop it over 30 minutes After adding 110g (0.55mol) of 20% aqueous sodium hydroxide solution, keep the reaction for 3h, stop the reaction, adjust the pH value to be neutral with hydrochloric acid solution, cool to 20°C, and use a separatory funnel to separate the product from water and oil. After letting go of the water phase, wash the organic phase twice with 100ml of water, separate the organic phase, and collect fractions at 138±3°C through molecular distillation equipment at a vacuum of 40 to 50 Pa to obtain 77.9 g of ethyl alcohol as a colorless and transparent liquid. Hexylglycerin, through gas chromatography analysis, the purity of ethylhexylglycerin is 99.1%, and the yield is 76.4%.

Embodiment 3

[0021] Add 65g (0.5mol) of isooctyl alcohol and 71.8g (0.65mol) of 3-chloro-1,2-propanediol into a 250ml three-necked flask equipped with a spherical condenser and a thermometer, stir, heat up to 50°C, and drop it over 30 minutes After adding 120g (0.6mol) of 20% aqueous sodium hydroxide solution, keep the reaction for 4h, stop the reaction, adjust the pH value to be neutral with hydrochloric acid solution, cool to 20°C, and use a separatory funnel to separate the product from water and oil. After letting go of the water phase, wash the organic phase twice with 100ml of water, separate the organic phase, and collect fractions at 138±3°C through molecular distillation equipment at a vacuum of 40 to 50 Pa to obtain 88 g of ethylhexyl in the form of a colorless and transparent liquid Glycerol, through gas chromatography analysis, the purity of ethylhexylglycerin is 99.5%, and the yield is 86.3%.

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Abstract

The invention discloses a preparation method of ethylhexylglycerin, wherein the preparation method comprises the steps: taking isooctanol, 3-chloro-1, 2-propylene glycol and common inorganic base as raw materials, preparing a target product through one-step reaction without adding a phase transfer catalyst, and then separating an organic phase, distilling and the like to obtain a high-purity ethylhexylglycerin product. The preparation method disclosed by the invention has the characteristics of simple process, mild reaction conditions, high selectivity, low energy consumption, green synthetic route, high product purity and the like, and is beneficial to popularization and application of ethylhexylglycerin in the industries of daily chemicals, cosmetics and the like.

Description

technical field [0001] The content of the invention belongs to the technical field of preparation technology of fine chemical products, and relates to a preparation method of ethylhexylglycerin. Background technique [0002] Ethylhexylglycerin (Ethylhexylglycerin) is an important representative of "no additives" preservatives, and it is also a multifunctional cosmetic additive recognized globally today. It is widely used in various bath products, cleaning products, deodorants, In products such as eye makeup, foundation, hair care products and sun care products. Ethylhexylglycerin can increase the moisturizing effect of emollients and humectants while increasing the smooth skin feel. Adding it to the cream system can improve the skin's absorption efficiency of the cream, and at the same time overcome stickiness and whitening. Sensitive shortcomings. Ethylhexylglycerin has a synergistic effect of mixing with antiseptic substances, some of which are used in combination with t...

Claims

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Application Information

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IPC IPC(8): C07C41/16C07C41/42C07C43/13
CPCC07C41/16C07C41/42C07C43/13Y02A50/30
Inventor 成西涛沈寒晰郭鹏涛南蓉彭逸峰杨淑玮白燕
Owner SHAANXI RES DESIGN INST OF PETROLEUM CHEM IND
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