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Acyl chloride co-production method

A technology of acryloyl chloride and process method, which is applied in chemical instruments and methods, preparation of acyl halide, preparation of carboxylate, etc., which can solve problems such as difficult separation and treatment, low yield, large amount of acid waste discharge, etc.

Active Publication Date: 2017-05-17
SHENZHEN UV-CHEMTECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The common problems of the above processes are harsh process conditions, huge discharge of solid waste and acid waste (especially the by-product aluminum chloride wastewater and SO2 acid gas that is difficult to absorb and reuse), and the production efficiency and environmental issues are very prominent
[0006] There are three kinds of synthetic (meth)acryloyl chloride known in the literature, all starting from (meth)acrylic acid, using different acylating reagents such as phosphine trichloride, phosphine oxychloride, and thionyl chloride, all of which are separated Difficult to deal with, low yield (generally less than 70%), poor product quality, and large amount of acid waste discharge. There are a small amount of sales in the market, but there is no successful practice of using the above-mentioned technology for industrialized large-scale production. A review Please refer to the representative article: Preparation and Application of Acryloyl Chloride, China Chlor-Alkali, Issue 9, 2006, page 23

Method used

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Embodiment 1

[0023] 47.4 grams of 1,3,5-trimethyl-2-(trichloromethyl)-benzene, 0.15 grams of ferric chloride, and 0.25 grams of 2,6-di-tert-butyl-4-methylphenol Place in a reaction flask, heat to 105°C, add 14.4 grams of acrylic acid dropwise, and distill the generated acryloyl chloride while adding dropwise, and absorb the generated hydrogen chloride gas with water, add the acrylic acid dropwise in about 1 hour, and then slowly raise the temperature The acryloyl chloride was distilled off steadily at 180° C. to obtain 12.8 g of acryloyl chloride, and then 33.8 g of 2,4,6-trimethylbenzoyl chloride were obtained by distillation under reduced pressure.

Embodiment 2

[0025] 47.4 grams of 1,3,5-trimethyl-2-(trichloromethyl)-benzene, 0.1 grams of zinc oxide, and 0.25 grams of 2,6-di-tert-butyl-4-methylphenol In the reaction flask, heat to 105°C, add 14.4 grams of acrylic acid dropwise, distill off the generated acryloyl chloride while adding dropwise, absorb the generated hydrogen chloride gas with water, finish adding the acrylic acid dropwise in about 1 hour, and then slowly raise the temperature to At 180°C, acryloyl chloride was distilled out steadily to obtain 12.5 g of acryloyl chloride, and then 30.8 g of 2,4,6-trimethylbenzoyl chloride were obtained by distillation under reduced pressure.

Embodiment 3

[0027] 47.4 grams of 1,3,5-trimethyl-2-(trichloromethyl)-benzene, 0.34 grams of anhydrous aluminum chloride, and 0.26 grams of 2,6-di-tert-butyl-4- Place methyl phenol in a reaction flask, heat it to 125°C, add 14.4 grams of methacrylic acid dropwise, distill off the generated acryloyl chloride while adding dropwise, absorb the generated hydrogen chloride gas with water, finish adding acrylic acid dropwise in about 1 hour, add After completion, slowly raise the temperature to 180°C, apply a vacuum of 0.3 atmospheres, and keep steady to distill methacryloyl chloride to obtain 16.0 grams of methacryloyl chloride, and then high vacuum oil pump decompression distillation to obtain 32.7 grams of 2,4,6 - Trimethylbenzoyl chloride.

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Abstract

The invention relates to the field of fine chemical materials and especially relates to a novel co-production technology of important industrial chemicals such as 2, 4, 6-trimethylbenzoyl chloride and (methyl)acryloyl chloride.

Description

[0001] 【Technical field】 [0002] The invention relates to the field of fine chemical materials, in particular to a new technology for co-production of important industrial chemicals of 2,4,6-trimethylbenzoyl chloride and (meth)acryloyl chloride. [0003] 【Background technique】 [0004] 2,4,6-trimethylbenzoyl chloride and (meth)acryloyl chloride are widely used fine organic chemical materials, especially in the field of light curing technology, 2,4,6-trimethylbenzoyl chloride is The grade is a common key raw material for photoinitiators Darocur TPO and Irgacure 819, while (meth)acryloyl chloride is an important raw material for the synthesis of various acrylate monomers and several pharmaceutical intermediates. [0005] The known synthetic 2 of literature, 4, the 6-trimethylbenzoyl chloride has following three kinds, and one of them is patent EP-A0554679, discloses to generate chlorine by 1,3,5-trimethylbenzene and chloroacetyl chloride reaction. substituted trimethylacetophen...

Claims

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Application Information

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IPC IPC(8): C07C51/60C07C51/58C07C57/66C07C63/04
CPCC07C51/58C07C51/60C07C57/66C07C63/04
Inventor 郑成
Owner SHENZHEN UV-CHEMTECH CO LTD
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