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Preparation method of 3, 4-dichloronitrobenzene by solid acid catalyst

A technology of solid acid catalyst and dichloronitrobenzene, which is applied in the preparation of nitro compounds, organic chemistry, etc., can solve the problems of low purity of finished products, long reaction time, incomplete reaction, etc., and achieve simplified reaction steps and complete reaction , the effect of high utilization rate

Inactive Publication Date: 2012-09-19
JIANGSU LONGCHANG CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the traditional reaction system uses a stirred tank to stir the reaction for a long time, the reaction is incomplete, the yield is low, and the purity of the finished product is not high

Method used

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Examples

Experimental program
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Effect test

Embodiment 1

[0014] Select materials and mix them with p-toluenesulfonic acid, concentrated nitric acid and o-dichlorobenzene in a molar ratio of 1:1.3:1.25.

[0015] Use p-toluenesulfonic acid as a catalyst, fully mix it with o-dichlorobenzene solution in the kettle, add dropwise concentrated nitric acid with a mass concentration of 98%, and carry out nitration reaction at 48°C for 6 hours, and keep warm for 2.5 hours after the reaction is completed. hour, and then stand for half an hour; then carry out solid-liquid separation to obtain the crude product of 3,4-dichloronitrobenzene; neutralize the obtained crude product with NaOH, wash and separate it with water, and obtain the pure product 3,4-dichloronitrobenzene Nitrobenzene.

[0016] In order to obtain this product, the present invention adopts the patent No. ZL2011203282529, and the patent name is a forced internal cooling circulation system of a nitration reactor to realize the external circulation nitration reaction.

[0017...

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PUM

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Abstract

The invention discloses a preparation method of 3, 4-dichloronitrobenzene by a solid acid catalyst, comprising the following steps of: taking p-toluenesulfonic acid as a catalyst; after fully mixing with o-dichlorobenzene solution in a kettle, dropping nitric acid with 98% of concentration, and performing nitration reaction at a certain temperature; after reaction, maintaining the temperature, and standing; performing solid and liquid separation to obtain crude 3, 4-dichloronitrobenzene; and after using NaOH to neutralize the crude product, using water to wash and separate so as to obtain pure 3, 4-dichloronitrobenzene. The product obtained by the method has 98% of yield and more than 99.8% of content.

Description

technical field [0001] The invention relates to an application method of a solid acid catalyst, in particular to a solid acid catalyst applied to the preparation of 3,4-dichloronitrobenzene. Background technique [0002] 3,4-Dichloronitrobenzene is an important intermediate of organic chemical products such as fluorochloroaniline, fluorochloronitrobenzene, and 3,4-dichloroaniline. [0003] There are currently two main production methods. One is nitration by o-dichlorobenzene, and the nitration temperature can be controlled at about 0°C, or it can be carried out at a temperature slightly higher than room temperature; the other production method is chlorination of p-nitrochlorobenzene. However, the traditional reaction system uses a stirred tank to stir for a long time, the reaction is incomplete, the yield is low, and the purity of the finished product is not high. Contents of the invention [0004] The main task of the present invention is to provide an external circulat...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C205/12C07C201/08
Inventor 郑兰荪王兆昌张剑宇王为
Owner JIANGSU LONGCHANG CHEM
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