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A kind of method that photocatalytic toluene is converted into chlorinated toluene

A chlorotoluene, photocatalytic technology, applied in chemical instruments and methods, organic chemistry, halogenated hydrocarbon preparation, etc., can solve the problem of product use limitation, increase impurity residue, affect product purity and other problems, achieve mild experimental conditions, selectable The effect of improving the performance and promoting the application

Active Publication Date: 2018-05-04
FUZHOU UNIV
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  • 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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  • A kind of method that photocatalytic toluene is converted into chlorinated toluene
  • A kind of method that photocatalytic toluene is converted into chlorinated toluene
  • A kind of method that photocatalytic toluene is converted into chlorinated 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) 0.1mmol CuCl 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 obtained 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 the anaerobic condition of the reaction. Stir magnetically at room temperature ; The light intensity of the visible light reaction is 300 mW / cm -2 (Wavelength is 420~780 nm);

[0026] 3) After the reaction is complete, the reactants and products are detected by GC-MS 6890N mass spectrometer. Quantitative analysis with 6890N chromatograph FID detector. The chromatographic column is HP-5 (5% polymethylsilane fixed solution, the specification is 30 m × 0.32 mm ×...

Embodiment 2

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

[0030] 1) 0.1mmol CuCl 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 obtained 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 the anaerobic condition of the reaction. Stir magnetically at room temperature ; The light intensity of the visible light reaction is 300 mW / cm -2 (Wavelength is 420~780 nm);

[0032] 3) After the reaction is complete, the reactants and products are detected by GC-MS 6890N mass spectrometer. Quantitative analysis with 6890N chromatograph FID detector. The chromatographic column is HP-5 (5% polymethylsilane fixed solution, the specification is 3...

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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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Patent Type & Authority Patents(China)
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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