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Method for optical catalytic conversion of toluene into chloro-toluene

A technology of chlorotoluene and photocatalysis, which is applied in chemical instruments and methods, organic chemistry, preparation of halogenated hydrocarbons, etc., can solve the problems of increasing impurity residues, product use restrictions, and affecting product purity, etc., to achieve selectivity improvement, experimental Moderate conditions, conducive to the effect of popularization and application

Active Publication Date: 2016-04-27
FUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although the introduction of these initiators speeds up the reaction speed, it also increases the production cost and increases the residue of impurities at the same time, which affects the purity of the product and limits the use of the product to a certain extent.

Method used

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  • Method for optical catalytic conversion of toluene into chloro-toluene
  • Method for optical catalytic conversion of toluene into chloro-toluene
  • Method for optical catalytic conversion of toluene into chloro-toluene

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Experimental program
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Effect test

Embodiment 1

[0023] The effect of different times on the response

[0024] 1) 0.1mmolCuCl 2 , 1 mL of acetonitrile, 100 μL of toluene; add copper chloride to acetonitrile, stir at room temperature for 1 min, first prepare the copper chloride acetonitrile complex; then add toluene to it to obtain a toluene solution;

[0025] 2) Put the toluene solution prepared in step (1) into an atmospheric pressure batch reaction device. After sealing, use a vacuum pump to remove the air in the reactor, and then fill it with nitrogen to ensure anaerobic conditions for the reaction. Stir magnetically at room temperature ; The light intensity of visible light reaction is 300mW / cm -2 (Wavelength is 420~780nm);

[0026] 3) After the reaction is complete, the reactants and products are detected by the GC-MS6890N mass spectrometer. The chromatographic column is HP-5MS (5% polymethylsilane fixed solution, the specification is 30m×0.32mm×0.25μm) and the FID of the GCAgilent6890N chromatograph Detector Quantit...

Embodiment 2

[0029] Experimental results at different reaction temperatures (1h)

[0030] 1) 0.1mmolCuCl 2 , 1 mL of acetonitrile, 100 μL of toluene; add copper chloride to acetonitrile, stir at room temperature for 1 min, first prepare the copper chloride acetonitrile complex; then add toluene to it to obtain a toluene solution;

[0031] 2) Put the toluene solution prepared in step (1) into an atmospheric pressure batch reaction device. After sealing, use a vacuum pump to remove the air in the reactor, and then fill it with nitrogen to ensure anaerobic conditions for the reaction. Stir magnetically at room temperature ; The light intensity of visible light reaction is 300mW / cm -2 (Wavelength is 420~780nm);

[0032] 3) After the reaction is complete, the reactants and products are detected by the GC-MS6890N mass spectrometer. The chromatographic column is HP-5MS (5% polymethylsilane fixed solution, the specification is 30m×0.32mm×0.25μm) and the FID of the GCAgilent6890N chromatograph D...

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Abstract

The present invention relates to a method for optical catalytic conversion of toluene into chloro-toluene. The method is as follows: first copper chloride and toluene are dissolved in acetonitrile, a cupric chloride and acetonitrile complex can absorb visible light to generate free chlorine radicals, and then on the basis, the free chlorine radicals attack of the toluene to produce benzyl chloride. Compared with non-illumination thermal catalytic reaction, visible light plays a decisive factor in the optical catalytic conversion, and the optical catalytic conversion cannot be separated from the visible light. The benzyl chloride produced by the method has high efficiency, selectivity can reaches more than 95%, and the method is simple, and helps use in the preparation of the benzyl chloride under the visible light.

Description

technical field [0001] The invention relates to the field of toluene chlorobenzylation reaction, in particular to a method for photocatalytically converting toluene into chlorotoluene. Background technique [0002] There are many chlorinated hydrocarbon products, among which chlorinated aromatics account for a considerable proportion, mainly including chlorinated benzene, dichlorobenzene, trichlorobenzene, chlorotoluene and its main derivative nitrochlorinated benzene. Chlorinated hydrocarbon products are mainly used in medicine, pesticides, dyes, synthetic material additives and other fields. In recent years, the production capacity of chlorinated hydrocarbon products in my country has expanded rapidly, and the production capacity and output of major varieties rank first in the world, becoming the main producer and supplier of chlorinated hydrocarbon products in the world. However, due to the backward production technology of many downstream products in the production proc...

Claims

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Application Information

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IPC IPC(8): C07C17/14C07C22/04
CPCC07C17/14C07C22/04
Inventor 员汝胜孟超黄坤付贤智丁正新陈旬
Owner FUZHOU UNIV
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