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Method for co-producing parachlorobenzoyl chloride and hexanoyl chloride and acyl chloride product thereof

A technology for p-chlorobenzoyl chloride and hexanoyl chloride is applied to the method and its acyl chloride product, in the field of co-production of p-chlorobenzoyl chloride and hexanoyl chloride, can solve problems such as non-conformance, reduce the yield of acyl chloride products, waste of resources, etc. Yield, reduce the generation of by-products and waste residue, reduce the effect of resource consumption

Pending Publication Date: 2022-07-05
河南特格纳特科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this type of Lewis acid still has good catalytic activity after the reaction is over, and can continue to promote the Friedel-Crafts acylation reaction of the acid chloride product to generate a by-product aromatic ketone, which not only greatly reduces the yield of the acid chloride product, but also forms a large amount of waste residue And the waste of resources is not in line with the current national requirements for the development of green chemical industry

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] The present embodiment provides a method for co-producing p-chlorobenzoyl chloride and hexanoyl chloride, which specifically includes the following steps:

[0045] (1) drop into p-chlorotrichlorobenzyl, hexanoic acid and Lewis acid in there-necked flask, be warming up to 120 ℃, be incubated 20min, obtain reaction product;

[0046] (2) get 1000 grams of reaction product in step (1), then add 100ppm auxiliary agent, use simple distillation apparatus to carry out vacuum distillation, distill until there is no more liquid to steam out, draw product 983 grams, residue 17 grams.

[0047] In step (1), the weight ratio of p-chlorotrichlorobenzyl to hexanoic acid is 1:0.6, the added amount of Lewis acid is 0.05% of the weight content of p-chlorotrichlorobenzyl, and the Lewis acid is ferric chloride.

[0048] In step (2), the auxiliary agent is amino trimethylidene phosphonate.

[0049] The conditions of vacuum distillation in step (2) are: pressure-0.9MPa, temperature 140°C.

Embodiment 2

[0051] The present embodiment provides a method for co-producing p-chlorobenzoyl chloride and hexanoyl chloride, which specifically includes the following steps:

[0052] (1) drop into p-chlorotrichlorobenzyl, hexanoic acid and Lewis acid in there-necked flask, be warming up to 110 DEG C, be incubated 30min, obtain reaction product;

[0053] (2) get 1000 grams of reaction product in step (1), then add 50ppm auxiliary agent, use simple distillation apparatus to carry out underpressure distillation, distill until there is no more liquid to steam out, draw product 970 grams, residue 30 grams.

[0054] In step (1), the weight ratio of p-chlorotrichlorobenzyl to hexanoic acid is 1:0.5, the added amount of Lewis acid is 0.04% of the weight content of p-chlorotrichlorobenzyl, and the Lewis acid is ferric chloride.

[0055] In step (2), the auxiliary agent is amino trimethylidene phosphonate.

[0056] The conditions of vacuum distillation in step (2) are: pressure-0.9MPa, temperature...

Embodiment 3

[0058] The present embodiment provides a method for co-producing p-chlorobenzoyl chloride and hexanoyl chloride, which specifically includes the following steps:

[0059] (1) drop into p-chlorotrichlorobenzyl, hexanoic acid and Lewis acid in there-necked flask, be warming up to 130 ℃, be incubated 10min, obtain reaction product;

[0060] (2) get 1000 grams of reaction product in step (1), then add 150ppm auxiliary agent, use simple distillation apparatus to carry out underpressure distillation, distill until there is no more liquid to steam out, draw product 975 grams, residue 25 grams.

[0061] In step (1), the weight ratio of p-chlorotrichlorobenzyl to hexanoic acid is 1:0.7, the added amount of Lewis acid is 0.06% of the weight content of p-chlorotrichlorobenzyl, and the Lewis acid is ferric chloride.

[0062] In step (2), the auxiliary agent is amino trimethylidene phosphonate.

[0063] The conditions of vacuum distillation in step (2) are: pressure-0.9MPa, temperature 14...

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Abstract

The invention relates to the field of fine chemical engineering, and particularly discloses a method for co-producing parachlorobenzoyl chloride and hexanoyl chloride and an acyl chloride product thereof, and the method comprises the following steps: adding parachlorotrichlorobenzyl, hexanoic acid and lewis acid into a reaction container, heating, carrying out a heat preservation reaction to obtain a reaction product, adding an auxiliary agent into the reaction product, and then distilling to obtain the parachlorobenzoyl chloride and hexanoyl chloride. And 4-chlorobenzoyl chloride and hexanoyl chloride products are obtained. According to the method, the addition amount and types of p-chlorotrichlorobenzyl, hexanoic acid and lewis acid are controlled, then production conditions are regulated and controlled, and then a special auxiliary agent is added into a reaction product, so that the activity of the lewis acid serving as a catalyst can be well inhibited, the Friedel-Crafts acylation reaction of an acyl chloride product under the condition of the catalyst is further prevented, and the yield of the product is improved. Therefore, the generation of byproducts and waste residues is reduced, the yield of the product is improved, the resource consumption is reduced, and the requirements of current national development of green chemical industry are met.

Description

technical field [0001] The invention belongs to the field of fine chemicals, and particularly relates to a method for co-producing p-chlorobenzoyl chloride and hexanoyl chloride and an acid chloride product thereof. Background technique [0002] A main production method of acid chloride products is to react benzyl trichloride with a certain carboxylic acid to obtain one or two acid chloride products, and Lewis acid is required as a catalyst in the synthesis process of such products. However, such Lewis acids still have good catalytic activity after the reaction, and can continue to promote the Friedel-Crafts acylation reaction of acid chloride products to generate by-product aromatic ketones, which not only greatly reduces the yield of acid chloride products, but also forms a large amount of waste residue. The waste of resources is not in line with the current national requirements for the development of green chemical industry. SUMMARY OF THE INVENTION [0003] In view o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/58C07C51/60C07C51/64C07C53/42C07C63/70
CPCC07C51/58C07C51/60C07C51/64C07C53/42C07C63/70
Inventor 李淑丽王兵权李涛
Owner 河南特格纳特科技有限公司