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A kind of recycling method of acetone in the preparation of ethylhexylglycerin

A technology of ethylhexylglycerol and glycidyl ether, applied in ether preparation, organic chemistry and other directions, can solve the problem that the reaction conditions cannot be adapted to the recovery of acetone, etc., and achieve a sustainable green process, easy to scale production, and treatment process simple effect

Active Publication Date: 2022-04-29
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

The reaction conditions of primary acetone and alkyl glycidyl ether are no longer suitable for the recovery of acetone

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] 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, place the flask in a water bath, and control the temperature at 35 to 40°C while stirring. Add 360 grams of recovered acetone and 10 grams of boron trifluoride ethyl ether dropwise. The time for adding drops is 40 minutes. After maintaining for 80 minutes, add 10 grams of methylamine gas to make the pH of the reaction solution at 7-8. After maintaining for 10 minutes, filter Precipitate, distill the remaining acetone from the filtrate under reduced pressure; add 40 grams of formic acid and 50 grams of distilled water to the remaining reactants, heat the water bath at 50-55 ° C for 180 minutes, let stand to separate the liquids, and neutralize the oil phase with sodium bicarbonate to Neutral, after washing twice with water, carry out short-range distillation, control the vacuum degree at 40-50Pa, collect the fraction with disti...

Embodiment 2

[0037] Replace the methylamine in example 1 with 10 grams of liquid ammonia as terminator, all the other steps are with embodiment 1, obtain high-purity ethylhexylglycerin of the present invention, through gas chromatography analysis, purity 99.3%, yield 88.2%, colorless tasteless.

Embodiment 3

[0038] Example 3 (mixed application of recycled acetone and fresh acetone at a weight ratio of 1:1)

[0039]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, place the flask in a water bath, and control the temperature at 35 to 40°C while stirring. Add dropwise the mixture of 360 g of recycled acetone and fresh acetone and 10 g of boron trifluoride ether, the time for the dropwise addition is 40 minutes, and after keeping for 80 minutes, add 10 g of liquid ammonia to make the pH of the reaction solution at 7-8 and keep it for 10 minutes. Minutes later, filter the precipitate, and distill the remaining acetone from the filtrate under reduced pressure; add 40 grams of formic acid and 50 grams of distilled water to the remaining reactants, heat the water bath at 50-55 ° C for 180 minutes, let stand to separate the liquids, and use bicarbonate for the oil phase Sodium is neutralized to...

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PUM

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Abstract

A method for recycling acetone in the preparation of ethylhexylglycerin. The acetone obtained by distillation can be reacted with 2-ethylhexyl glycidyl ether again at 35-45°C in the presence of a catalyst after being treated with a dehydrating agent and an organic acid to form Intermediate, add anhydrous terminator at the right time and filter to remove the solid residue formed by the catalyst and terminator; the excess acetone distilled from the filtrate under reduced pressure is recycled after treatment, and acid is added to the remaining system for hydrolysis reaction, after neutralization, water washing, Molecular distillation obtains high-purity daily chemical grade ethylhexylglycerin. The recycling of acetone in the production process is realized, which is economical, safe and environmentally friendly, and meets the needs of industrial production.

Description

technical field [0001] The invention belongs to the field of daily chemical preservatives, and in particular relates to a method for recycling acetone in the preparation of ethylhexylglycerin. Background technique [0002] Ethylhexylglycerin is a new multifunctional cosmetic additive with antiseptic effect and moisturizing and deodorizing effect. As the toxicological safety of traditional preservatives has been questioned more and more, the emergence of ethylhexylglycerin, which is green, non-irritating and antiseptic, brings hope to people, especially the synergistic effect of it and other traditional preservatives Used in the daily chemical product system, it can greatly reduce the amount of traditional preservatives added, and can significantly reduce the toxicity of the preservative system. It has antiseptic effect, no irritation to the skin, moisturizing and moisturizing, and can enhance the antiseptic ability of traditional preservatives, making ethylhexylglycerin pla...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C41/01C07C43/13
CPCC07C41/01C07D317/22C07C43/13
Inventor 李程碑杨淑玮李辉武小祥
Owner SHAANXI RES DESIGN INST OF PETROLEUM CHEM IND