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Preparation method of 2, 4, 6-trimethylbenzoyl chloride

A technology for trimethylbenzoyl chloride and crude trimethylbenzoyl chloride is applied in the field of chemical industry, can solve problems such as low reaction yield, sharp reaction, high cost organic waste liquid, etc. The effect of simplifying operations

Inactive Publication Date: 2020-09-11
宁波海曙琼杰化工技术研发工作室
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the current synthesis technique of 2,4,6-trimethylbenzoic acid, the technological process is complicated, the yield of 2,4,6-trimethylbenzoic acid is low, and the recycling of raw materials cannot be realized; In the chemical process, toluene or n-hexane is usually used as the reaction solvent or direct solid-liquid reaction without solvent. Using toluene or n-hexane as the reaction solvent is costly and will produce a large amount of organic waste liquid, which does not conform to the theory of green chemistry. Direct reaction without solvent The yield of solid-liquid reaction is low and there are great safety hazards such as stirring stuck, sharp reaction leading to material flushing accidents

Method used

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  • Preparation method of 2, 4, 6-trimethylbenzoyl chloride
  • Preparation method of 2, 4, 6-trimethylbenzoyl chloride

Examples

Experimental program
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Effect test

Embodiment 1

[0029] (1) Friedel-Crafts reaction: add 368g aluminum chloride and 662g mesitylene in the autoclave, stir, then pass into carbon dioxide and react at 25°C under 0.35MPa;

[0030] (2) Hydrolysis and post-treatment: Add the reaction solution after the reaction in step (1) dropwise to the hydrolyzate, wherein the hydrolyzate is a mixed solution of 150g hydrochloric acid and 900g water, and carry out at a temperature not higher than 80°C Hydrolysis reaction, static separation after hydrolysis; take the organic layer and add 900g of water to the organic layer to obtain a distilled mixed solution, heat up to 98°C and azeotropically reflux to distill out the mesitylene, wherein the distilled mesitylene is passed After freezing and dehydration, circulate it as the solvent for the next batch of Friedel-Crafts reaction. During the reflux process, stir the distillation mixture at a speed of 650r / min. When no mesitylene is distilled out, keep the temperature at 100°C for 45 minutes, then c...

Embodiment 2

[0033] (1) Friedel-Crafts reaction: add 368g aluminum chloride and 405g mesitylene in the autoclave, stir, then pass into carbon dioxide to react at 30 ℃ under 0.3MPa;

[0034] (2) Hydrolysis and post-treatment: Add the reaction solution after the reaction in step (1) dropwise to the hydrolyzate, wherein the hydrolyzate is a mixed solution of 150g hydrochloric acid and 900g water, and carry out at a temperature not higher than 80°C Hydrolysis reaction, static separation after hydrolysis; take the organic layer and add 900g of water to the organic layer to obtain a distilled mixed solution, heat up to 95°C and azeotropically reflux to evaporate mesitylene, wherein, the steamed mesitylene is passed After freezing and dehydration, it can be used as the next batch of Friedel-Crafts reaction solvent. During the reflux process, the distillation mixture is stirred at a speed of 500r / min. When no mesitylene is distilled out, keep the temperature at 100°C for 30 minutes, then cool to ro...

Embodiment 3

[0037] (1) Friedel-Crafts reaction: add 368g aluminum chloride and 1100g mesitylene to the autoclave, stir, then feed carbon dioxide to react at 20°C under 0.4MPa;

[0038] (2) Hydrolysis and post-treatment: Add the reaction solution after the reaction in step (1) dropwise to the hydrolyzate, wherein the hydrolyzate is a mixed solution of 150g hydrochloric acid and 900g water, and carry out at a temperature not higher than 80°C Hydrolysis reaction, static separation after hydrolysis; take the organic layer and add 900g of water to the organic layer to obtain a distilled mixed solution, heat up to 98°C and azeotropically reflux to distill out the mesitylene, wherein the distilled mesitylene is passed After freezing and dehydration, it can be used as the next batch of Friedel-Crafts reaction solvent. During the reflux process, the distillation mixture is stirred at a speed of 800r / min. When no mesitylene is distilled out, keep the temperature at 100°C for 60 minutes, then cool to...

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Abstract

The invention discloses a preparation method of 2, 4, 6-trimethylbenzoyl chloride, and belongs to the technical field of chemical engineering. The preparation method comprises the following steps: firstly, reacting mesitylene with carbon dioxide under the catalysis of aluminum trichloride, dropwise adding a reaction solution obtained after the reaction into a hydrolysate, carrying out a hydrolysisreaction at a temperature not higher than 80 DEG C, and standing for layering after the hydrolysis is finished; taking an organic layer, adding water into the organic layer to obtain a distillation mixed solution, heating to 95-100 DEG C, and performing azeotropic reflux to evaporate the mesitylene to obtain 2, 4, 6-trimethylbenzoic acid; and adding the obtained 2, 4, 6-trimethylbenzoic acid intosolvent 2, 4, 6-trimethylbenzoyl chloride and catalyst DMF, adding a chlorination reagent to carry out an acylating chlorination reaction, taking the upper layer 2, 4, 6-trimethylbenzoyl chloride crude product after the reaction is finished, and carrying out reduced pressure distillation to obtain the target product. The method is simple to operate, the yield of the intermediate 2, 4, 6-trimethylbenzoic acid and the product 2, 4, 6-trimethylbenzoyl chloride can be increased, raw materials can be recycled, and the method is economical and environmentally friendly.

Description

technical field [0001] The invention relates to a preparation method of 2,4,6-trimethylbenzoyl chloride, which belongs to the technical field of chemical industry. Background technique [0002] 2,4,6-Trimethylbenzoyl chloride has a wide range of uses. It can be used as a photoinitiator in photopolymerizable materials, unsaturated resin models and recording materials, and can be used as a stabilizer in plastics and paints to improve light resistance , heat resistance, can be used in medicine to prepare antibiotics and antihistamines, and can also be used to prepare coatings, dyes, moldings, adhesives, composite fiber materials, etc. In addition, it can also be used as a photoinitiator An important raw material for TPO and TPO-L. [0003] The preparation process of 2,4,6-trimethylbenzoyl chloride usually includes two steps: first, the intermediate 2,4,6-trimethylbenzene is prepared by reacting mesitylene and carbon dioxide under the catalysis of aluminum trichloride Formic a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/60C07C63/70C07C51/64
CPCC07C51/15C07C51/60C07C51/64C07C63/04C07C63/70
Inventor 刘碧见
Owner 宁波海曙琼杰化工技术研发工作室
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