Synthesis process of chloroacetyl chloride

A technology of chloroacetyl chloride and synthesis process, which is applied in directions such as the preparation of acyl halides, the preparation of organic compounds, the preparation of carboxylates, etc., can solve the problems of low quality of chloroacetyl chloride, low purity of chloroacetyl chloride, limited application fields and the like, Achieve the effect of low dichloride content, less rectification residue and high purity

CN110343039AInactive Publication Date: 2019-10-18CHENGWU CHENHUI ENVIRONMENTAL PROTECTION TECH CO LTD
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Patent Information

Authority / Receiving Office
CN · China
Current Assignee / Owner
Publication Date
2019-10-18
Estimated Expiration
Not applicable · inactive patent
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Abstract

The invention belongs to the technical field of fine chemical engineering products, and particularly relates to a synthesis process of chloroacetyl chloride. 10-20 parts of chloroacetic acid are addedinto a reaction bulb, zinc oxide is added at the same time, the mixture is heated to 100-120 DEG C and constantly stirred to melt the chloroacetic acid, the temperature is kept at 100-120 DEG C, 20-40 parts of benzenyltrichloride with the purity being 94-98% are slowly added into the molten chloroacetic acid for about 8-9 h, and after a heat preservation reaction for 1-2 h, through rectificationunder vacuum and separation, 10-20 parts of the chloroacetyl chloride with the purity being 99.3-99.5%, 15-25 parts of benzoyl chloride with the purity being 99.3-99.8% and rectification residual liquid are obtained. A traditional sulphur method is replaced with the process, use of sulphur is not needed, and the process cannot produce sulfur dioxide polluting the environment; the produced chloroacetyl chloride has the high purity, the low dichloride content and no sulfur; a catalyst selected by the process can be applied, the amount of rectification residue is very low, and active components in the rectification residue can be effectively recycled; and by-product hydrochloric acid of the process basically contains no sulfate radicals, and can be directly and externally sold.
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Description

technical field

[0001] The invention belongs to the technical field of fine chemical products, in particular to a synthesis process of chloroacetyl chloride. Background technique

[0002] Chloroacetyl chloride is an important organic chemical intermediate, which is widely used in the fields of pesticides, medicines, dyes, and various auxiliaries. As an acylating agent with excellent performance, the current commercial products are fine Chemicals and chemical reagents.

[0003] At present, the sulfur method is widely used in China to synthesize chloroacetyl chloride, but the purity of chloroacetyl chloride synthesized by this method is not high (95%±2%), which leads to low quality of chloroacetyl chloride and limited application fields. Contents of the invention

[0004] The present invention is achieved through the following technical solutions:

[0005] Add 10~20 parts of chloroacetic acid into the reaction bottle, add zinc oxide catalyst at the same time, heat to 100~1...

Examples

Embodiment 1

[0009] Add 96.4g of chloroacetic acid into the reaction bottle, and add zinc oxide catalyst at the same time, heat to 100°C, and keep stirring to melt the chloroacetic acid, keep the temperature at 100°C, slowly add 203.6g of trichlorobenzyl with a purity of 94% to the reaction flask In the molten chloroacetic acid, the addition was completed in about 8 hours, and after the heat preservation reaction for 1 hour, 108 g of chloroacetyl chloride with a purity of 99.3%, 132 g of benzoyl chloride with a purity of 99.3% and a rectification raffinate were obtained.

Embodiment 2

[0011] Add 144.6g of chloroacetic acid into the reaction bottle, and add zinc oxide catalyst at the same time, heat to 110°C, and keep stirring to melt the chloroacetic acid, keep the temperature at 110°C, slowly add 305.4g of trichlorobenzyl with a purity of 96% In the molten chloroacetic acid, the addition was completed in about 8.5 hours, and after 1.5 hours of heat preservation reaction, 162 g of chloroacetyl chloride with a purity of 99.4%, 198 g of benzoyl chloride with a purity of 99.5% and the rectification raffinate were obtained.

Embodiment 3

[0013] Add 189.2g of chloroacetic acid into the reaction bottle, and add zinc oxide catalyst at the same time, heat to 120°C, and keep stirring to melt the chloroacetic acid, keep the temperature at 120°C, slowly add 407.2g of trichlorobenzyl with a purity of 98% to the reaction flask In the molten chloroacetic acid, the addition was completed in about 9 hours, and after the heat preservation reaction for 2 hours, 108 g of chloroacetyl chloride with a purity of 99.5%, 264 g of benzoyl chloride with a purity of 99.8% and a rectification raffinate were obtained.