Chloronitrobenzene preparation method

A technology for chloronitrobenzene and chlorobenzene is applied in the field of preparing chloronitrobenzene and can solve the problems of poor safety, waste acid pollution, poor atom economy and the like

Inactive Publication Date: 2015-01-28
王晓伟
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are still many defects in the application of this process method: the atom economy of the reaction is poor; the nitrification reaction has no regioselectivity, and a large amount of excess organic isomer waste is produced; a large amount of waste acid is processed, which requires high energy consumption, serious waste acid pollution, and poor safety.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] In the reactor, add 0.1mol chlorobenzene, 0.2g iron acetylacetonate, 30ml ethylene dichloride, stir evenly, feed dinitrogen tetroxide and ozone, and react for 7 hours at a pressure of 1.5MPa and a temperature of 100°C. After the reaction is finished, cool to room temperature, feed oxygen into the reaction mixture until nitrogen oxides completely escape from the reactor, and then remove the catalyst. The filtrate was washed with sodium carbonate aqueous solution until nearly neutral, and the organic phase was washed and concentrated by vacuum rotary evaporation. The content of product components was analyzed by gas chromatography with nitrobenzene as internal standard. The yield of chlorophenylnitrobenzene was 90.5%.

Embodiment 2

[0016] In the reactor, add 0.1mol chlorobenzene, 0.3g iron acetylacetonate, 30ml acetonitrile, stir evenly, feed dinitrogen tetroxide and ozone, and react for 7 hours at a pressure of 1.5MPa and a temperature of 100°C. After the reaction is finished, cool to room temperature, feed oxygen into the reaction mixture until nitrogen oxides completely escape from the reactor, and then remove the catalyst. The filtrate was washed with sodium carbonate aqueous solution until nearly neutral, and the organic phase was washed and concentrated by vacuum rotary evaporation. The content of product components was analyzed by gas chromatography with nitrobenzene as internal standard. The yield of chlorophenylnitrobenzene was 92.3%.

Embodiment 3

[0018] In the reactor, add 0.1mol chlorobenzene, 0.4g iron acetylacetonate, 30ml acetonitrile / dichloroethane (volume ratio 1:1), after stirring evenly, pass into dinitrogen tetroxide and ozone, under pressure 1.5MPa and The reaction was carried out at a temperature of 90° C. for 9 hours. After the reaction is finished, cool to room temperature, feed oxygen into the reaction mixture until nitrogen oxides completely escape from the reactor, and then remove the catalyst. The filtrate was washed with sodium carbonate aqueous solution until nearly neutral, and the organic phase was washed and concentrated by vacuum rotary evaporation. The content of product components was analyzed by gas chromatography with nitrobenzene as internal standard. The yield of chlorophenylnitrobenzene is 95%.

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PUM

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Abstract

The invention belongs to the technical field of fine chemical industry, and mainly relates to a method for preparation of a nitrocompound by use of nitrogen tetroxide / ozone as a nitrating agent; the method comprises the following steps: reaction raw material chlorobenzene, a solvent and a solid catalyst are added into a reactor; ozone and nitrogen tetroxide are introduced for reaction for 7-10h in the 0.011.5MPa and at 50 to 100 DEG C. After the reaction, the temperature is cooled to room temperature, oxygen is introduced into the reaction mixture until nitrogen oxides completely escape from the reactor, and the catalyst is filtered out. The filtrate is washed to neutral with sodium carbonate solution, an organic phase is washed, and vacuum rotary evaporation and concentration is performed.

Description

technical field [0001] The invention relates to a method for preparing nitro compounds, in particular to a method for preparing chloronitrobenzene by substituting dinitrogen tetroxide and ozone for mixed acid, in particular to a method for preparing chloronitrobenzene by using iron acetylacetonate as a catalyst. Background technique [0002] The easy conversion of nitro compounds and their nitro functional groups is widely used as chemicals such as dyes, drugs (such as medicine, pesticides), spices, high energy density materials, and their intermediates. Therefore, the wide application characteristics of nitro compounds It has long been concerned by the field of fine organic synthesis. [0003] At present, the industrial production of nitrochlorobenzene is mainly based on chlorinated benzene as the starting material, which is prepared by nitration reaction with a certain amount of nitric acid / sulfuric acid mixed acid. For the waste acid produced in the production of nitrochl...

Claims

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Application Information

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IPC IPC(8): C07C201/08C07C205/11
Inventor 王晓伟
Owner 王晓伟
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