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Composite catalyst and application

A composite catalyst and chlorination reaction technology, applied in physical/chemical process catalysts, organic compound/hydride/coordination complex catalysts, organic chemistry, etc., can solve the problem of long synthesis reaction time, difficult reaction, low yield, etc. problem, achieve the effect of reducing the generation of high boiling point raffinate, the effect is obvious, and the quality and yield are improved

Inactive Publication Date: 2011-01-19
ZHEJIANG KANGFENG CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The invention aims at the problems of long synthesis reaction time, low yield, difficult reaction and many impurities in the synthesis of ditrichloromethylbenzene in the existing catalytic chlorination technology, and provides a composite catalyst for catalytic chlorination reaction of benzene ring side chain

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] The preparation of embodiment 1 m-ditrichloromethylbenzene

[0023] Preparation of the composite catalyst: Take 100 g of m-trichloromethylbenzene (also available as m-xylene), add 3.6 g of BPO (provided by Jiangsu Yuanyang Chemical Co., Ltd.) to dissolve, and then add 0.04 g of analytically pure diethanolamine (provided by Chengdu Kelong Chemical Reagent Factory), after mixing, let stand, separate the water layer and the organic layer, and prepare the composite catalyst. In this embodiment, the mass ratio of m-ditrichloromethylbenzene:BPO:diethanolamine is 1:0.036:0.0004.

[0024] Catalyze m-xylene to generate ditrichloromethylbenzene: heat 212.34g (2mol) m-xylene to 60°C, drop about 0.5g of the composite catalyst prepared by the above method, and react with chlorine gas, the flow rate of chlorine gas is 0.5 L / min, the temperature at the initial stage of the reaction is controlled within the range of 80-90°C, and the reaction temperature is gradually increased as the ...

Embodiment 2

[0026] The preparation of embodiment 2 o-chlorotrichloromethylbenzene

[0027] Preparation of composite catalyst: Take 100 g of o-chlorotrichloromethylbenzene (ortho-chlorotoluene can also be used), add 3.2 g of BPO (provided by Jiangsu Yuanyang Chemical Co., Ltd.) to dissolve, and then add 0.03 g of analytically pure diethanolamine (provided by Chengdu Kelong Chemical Reagent Factory), after mixing, let stand, separate the water layer and the organic layer, and prepare the composite catalyst. In this embodiment, the mass ratio of o-chlorotrichloromethylbenzene:BPO:diethanolamine is 1:0.032:0.0003.

[0028] Catalyze o-chlorotoluene to produce o-chlorotrichloromethylbenzene: put in 253.18g (2mol) o-chlorotoluene, raise the temperature to 80°C, drop in about 0.5g of the composite catalyst prepared by the above method, and react with chlorine gas, the flow rate of chlorine gas is 0.4 L / min, the initial temperature of the reaction is 80~90°C, gradually increase the temperature as...

Embodiment 3

[0030] Embodiment 3 Preparation of p-chlorotrichloromethylbenzene

[0031]Preparation of the composite catalyst: Take 100 g of p-chlorotrichloromethylbenzene (p-chlorotoluene can also be used), add 3.0 g of BPO (provided by Jiangsu Yuanyang Chemical Co., Ltd.) to dissolve, and then add 0.03 g of analytically pure diethanolamine (provided by Chengdu Kelong provided by Chemical Reagent Factory), mixed evenly and left to stand, separated the water layer and the organic layer, and prepared the composite catalyst for future use. In this embodiment, the mass ratio of p-chlorotrichloromethylbenzene:BPO:diethanolamine is 1:0.030:0.0003.

[0032] Catalyze p-chlorotoluene to generate p-chlorotrichloromethylbenzene: heat up 253.18g (2mol) p-chlorotoluene to 80°C, drop about 0.5g of the composite catalyst prepared by the above method, and react with chlorine gas, the flow rate of chlorine gas is 0.4 L / min, the initial temperature of the reaction is 80~90°C, gradually increase the temper...

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Abstract

The invention belongs to the field of organic synthesis, in particular to a composite catalyst and an application thereof in synthesizing benzo-trichloride. The method for preparing the composite catalyst comprises the following steps: adding 1 to 4 parts of initiators into 100 parts of chlorinated raw materials or chlorinated products so as to obtain a mixture A after the initiators are dissolved; adding alcohol-amine compounds into the mixture A, wherein the addition of the alcohol-amine compounds accounts for 0.02 to 0.05% of the mixture A; evenly mixing the alcohol-amine compounds and the mixture A, and standing so as to separate a water layer from an organic layer, then obtaining the organic layer, namely, the composite catalyst. The composite catalyst can be used for generating bis(trichloromethyl) benzene or 2-(trichloromethyl) benzene by catalyzing xylene or chlorotoluene, and solves the problems of long synthesis time, low yield, difficult reaction and a large amount of impurities for the bis(trichloromethyl) benzene in existing catalytic / chlorinated technology.

Description

technical field [0001] The invention belongs to the field of organic synthesis, and in particular relates to a composite catalyst and the application of the composite catalyst in the synthesis of trichlorotoluene. Background technique [0002] The reaction in which the hydrogen atom of the methyl group on the benzene ring is replaced by chlorine is called benzene ring side chain substitution chlorination. It is a free radical chain reaction, and its reaction mechanism is composed of three parts: chain initiation, chain transfer and chain termination. composition. Illumination or addition of initiators (commonly known as catalysts) are beneficial to the free radical reaction. The reaction formula is: [0003] The chlorination reaction with the addition of an initiator is usually called catalytic chlorination. Compared with photochlorination, catalytic chlorination often has the following advantages: wide application range, simple equipment, low operation requirements, low...

Claims

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Application Information

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IPC IPC(8): B01J31/02C07C17/14C07C22/04C07C25/02
Inventor 张位德吴永良吴向峰吴康吴金桥
Owner ZHEJIANG KANGFENG CHEM
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