Method for producing 5-chloro-2-nitroaniline

The technology of a kind of nitroaniline and production method is applied in the production field of 5-chloro-2-nitroaniline, which can solve the problems of complex production method, low content of finished product, low yield of product, etc., and achieve easy operation and simple method Effect

Inactive Publication Date: 2012-07-04
江苏优普生物化学科技股份有限公司
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  • Application Information

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Problems solved by technology

[0002] The existing 5-chloro-2-nitroaniline production method is compli

Method used

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Embodiment Construction

[0014] A production method of 5-chloro-2-nitroaniline, comprising the following steps:

[0015] (1) Nitration: Nitrate m-dichlorobenzene with a mixed acid made of sulfuric acid and nitric acid at 45~55°C for 4~5 hours. After the nitrification is completed, the layers are separated, and the upper oil phase is washed with water until neutral, and then 4% hydrogen The sodium oxide solution was boiled with alkali and allowed to stand for stratification, and the oil phase in the lower layer was washed with water until neutral to obtain 2,4-dichloronitrobenzene;

[0016] (2) Amination: Add 2,4-dichloronitrobenzene into the high-pressure amination kettle, feed liquid ammonia, keep warm at 140~150℃, 7.0~8.5MPa for 5~6 hours, release the pressure to 0.5MPa, and put Press the material into the water washing kettle, wash away the ammonium chloride, and filter with suction to obtain a filter cake containing the product 5-chloro-2-nitroaniline, and the obtained filter cake is also refined ...

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Abstract

The invention discloses a method for producing 5-chloro-2-nitroaniline. The method comprises the following steps of: performing nitration on m-dichlorobenzene by using mixed acid of sulfuric acid and nitric acid at the temperature of between 45 and 55 DEG C for 4 to 5 hours, then layering after the nitration is finished, washing an oil phase of the upper layer until the oil phase of the upper layer is neutral, performing soda boiling by using a 4 percent sodium hydroxide solution, standing and layering, washing an oil phase of a lower layer until the oil phase of the lower layer is neutral to obtain 2,4-dichloronitrobenzene; and adding 2,4-dichloronitrobenzene into a high-pressure amination kettle, introducing liquid ammonia, preserving heat at the temperature of between 140 and 150 DEG C under the pressure of 7.0 to 8.5MPa for 5 to 6 hours, relieving pressure until the pressure is 0.5MPa, pressing materials into a washing kettle, washing off ammonium chloride, and suction-filtering to obtain a filter cake containing a product 5-chloro-2-nitroaniline. The method is simple and convenient, and is easy to operate, and the content of a finished product reaches over 98 percent.

Description

technical field [0001] The invention relates to a production method of 5-chloro-2-nitroaniline. Background technique [0002] The existing 5-chloro-2-nitroaniline production method is complicated, the product yield is low, and the finished product content is low. Contents of the invention [0003] The purpose of the present invention is to provide a kind of easy operation, the production method of the 5-chloro-2-nitroaniline that finished product content is high. [0004] Technical solution of the present invention is: [0005] A kind of production method of 5-chloro-2-nitroaniline is characterized in that: comprise the following steps: [0006] (1) Nitration: Nitrate m-dichlorobenzene with a mixed acid made of sulfuric acid and nitric acid at 45~55°C for 4~5 hours. After the nitrification is completed, the layers are separated, and the upper oil phase is washed with water until neutral, and then 4% hydrogen The sodium oxide solution was boiled with alkali and allowed t...

Claims

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Application Information

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IPC IPC(8): C07C211/52C07C209/10
Inventor 陶坤山徐国军张建华张继钱于海军
Owner 江苏优普生物化学科技股份有限公司
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