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Method for producing benzyl trichloride by directional chlorination of alkylbenzene and benzyl trichloride

A technology of alkylbenzene and trichlorobenzyl, which is applied in the field of organic synthesis of fine chemicals, can solve problems such as difficulty in controlling the depth of chlorination, affecting the yield of trichlorobenzyl, side reactions of benzene ring, etc., and achieves lower temperature, strong selectivity, and cyclic polychlorinated compounds reduce the effect of

Pending Publication Date: 2022-03-25
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

[0002] Benzylbenzene is an aromatic hydrocarbon compound formed by the chlorination of alkylbenzene. Trichlorobenzyl, also known as trichlorotoluene, is in the form of light yellow or colorless liquid. It is usually used as an intermediate in organic synthesis, a raw material for dyes or ultraviolet absorbers, but During the chlorination process, with the deepening of the chlorination depth and the increase of the reaction temperature, not only a series of chlorination reactions will be carried out on the side chain molecules of alkylbenzene, but also side reactions will occur on the benzene ring, and the chlorination depth It is not easy to control, so it is easy to generate by-products such as monochlorobenzyl, dichlorobenzyl and ring-substituted polychlorides, which not only affects the yield of trichlorobenzyl, but also affects the subsequent separation
[0003] In addition, in the production process, some metals and their compounds will inevitably be introduced due to equipment or materials, resulting in the inability to proceed in the early stage of the reaction, resulting in a large amount of benzyl plastic, resulting in a large loss of materials

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] A method for producing trichlorobenzyl by directional chlorination of alkylbenzenes, specifically comprising the following steps:

[0027] Put 500g of chlorotoluene, 1ppm compound phosphine and 0.3g of benzoyl peroxide into a four-necked flask with a tail gas absorption device, close the reaction device, start to heat up, after the temperature rises to 60°C, pass chlorine gas, pass through The chlorine rate is controlled at 550ml / min, and the product is obtained after the temperature rises to 140°C and the reaction is kept for 4 hours.

[0028] The composite phosphine compound includes a mixture of benzyl diphenyl phosphine, dibenzyl phenyl phosphine and dibenzyl phenyl phosphine oxide, and the weight ratio is 1:3:4.

Embodiment 2

[0030] A method for producing trichlorobenzyl by directional chlorination of alkylbenzenes, specifically comprising the following steps:

[0031] Put 500 g of chlorotoluene, 2 ppm compound phosphine and 0.3 g of benzoyl peroxide into a four-necked flask with a tail gas absorption device, seal the reaction device, and start to heat up. After the temperature rises to 60 ° C, pass chlorine gas, pass The chlorine rate is controlled at 500ml / min, and the product is obtained after the temperature rises to 150°C and the reaction is kept for 3.5 hours.

[0032] The composite phosphine compound includes a mixture of benzyl diphenyl phosphine, dibenzyl phenyl phosphine and dibenzyl phenyl phosphine oxide, and the weight ratio is 1:3:4.

Embodiment 3

[0034] A method for producing trichlorobenzyl by directional chlorination of alkylbenzenes, specifically comprising the following steps:

[0035] Put 500g of chlorinated toluene, 5ppm compound phosphine and 0.3g of benzoyl peroxide into a four-necked flask with a tail gas absorption device, close the reaction device, start to heat up, after the temperature rises to 60°C, pass chlorine gas, pass The chlorine rate is controlled at 600ml / min, and the product is obtained after the temperature rises to 180°C and the reaction is kept for 3.5 hours.

[0036] The composite phosphine compound includes a mixture of benzyl diphenyl phosphine, dibenzyl phenyl phosphine and dibenzyl phenyl phosphine oxide, and the weight ratio is 1:3:4.

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PUM

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Abstract

The invention relates to the technical field of organic synthesis in fine chemical engineering, in particular to a method for producing benzyl trichloride by directional chlorination of alkylbenzene, which at least comprises the following steps: placing alkylbenzene, composite phosphinate and benzoyl peroxide in a container for closed reaction, heating to a target temperature, introducing chlorine, then continuously heating, and carrying out heat preservation reaction to obtain a product. According to the invention, by adding the specific composite phosphinate in the chlorination process of alkylbenzene and controlling the conditions in the production process, the directional substitution effect is obvious, the conversion speed is high, the selectivity is strong, benzyl plastics and cyclic polychlorides are obviously reduced, the yield of the prepared benzyl trichloride is high, and the amount of cyclic chloride is controlled to be below 2%; in addition, the reaction temperature is effectively reduced, the directional chlorination reaction can still be smoothly carried out even in the presence of metal and compounds thereof, and the loss of materials is remarkably reduced.

Description

technical field [0001] The invention relates to the technical field of fine chemical organic synthesis, in particular to a method for producing trichlorobenzyl by directional chlorination of alkylbenzene and trichlorobenzyl. Background technique [0002] Benzylbenzene is an aromatic hydrocarbon compound formed by the chlorination of alkylbenzene. Trichlorobenzyl, also known as trichlorotoluene, is in the form of light yellow or colorless liquid. It is usually used as an intermediate in organic synthesis, a raw material for dyes or ultraviolet absorbers, but During the chlorination process, with the deepening of the chlorination depth and the increase of the reaction temperature, not only a series of chlorination reactions will be carried out on the side chain molecules of alkylbenzene, but also side reactions will occur on the benzene ring, and the chlorination depth It is not easy to control, so it is easy to generate by-products such as monochlorobenzyl, dichlorobenzyl and...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C17/14C07C22/04
CPCC07C17/14C07C22/04
Inventor 王兵权李淑丽李涛
Owner 河南特格纳特科技有限公司