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Pipeline reaction synthesis method of p-nitroaniline

A p-nitroaniline, pipeline reaction technology, applied in the direction of nitro compound preparation, amino compound preparation, chemical instruments and methods, etc., can solve the irritating taste of p-nitroaniline, high pressure of nitroaniline, and lack of high yield Quality and other issues, to achieve the effect of no explosion risk, sufficient response, and increased utilization

Inactive Publication Date: 2020-03-17
乐平市景顺实业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] p-Nitroaniline is an important intermediate of pesticides and dyes, and its consumption is about 40,000 tons a year in China. The reaction synthesis methods of p-Nitroaniline in the prior art all adopt the method of kettle reaction, and the pressure of p-Nitroaniline in this way is Large, low content, large investment in equipment, prone to risk of melting and frying, and the p-nitroaniline produced has a pungent taste, wasting raw materials and not obtaining high-quality p-nitroaniline

Method used

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  • Pipeline reaction synthesis method of p-nitroaniline

Examples

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Embodiment 1

[0023] A kind of synthesis method of p-nitroaniline pipeline reaction, comprises the following steps:

[0024] Step 1: First, carry out nitration reaction of chlorinated benzene and mixed acid to obtain: 63% p-nitrochlorinated benzene, 35% o-nitrochlorinated benzene, 1% p-nitrochlorinated benzene, and dinitrochlorinated benzene 1% mixture;

[0025] Step 2: Put the above mixture into a pulverizer, grind it into a powdered p-nitrochlorobenzene with a particle size of 1000 mesh, put it into the reactor, install a vibration motor at the bottom of the reactor, and vibrate the reactor, while Continuously add cold air into the reaction kettle through the external pipeline of the compressor, control the temperature in the reaction kettle at 5°C, and the pressure at 1MPa for 5 minutes;

[0026] Step 3: Add ammonia water with a concentration of 39% to the powder that has been fully cooled in step 2, and quickly add it to the pipeline reactor with a feed pump, keeping the pressure at 6M...

Embodiment 2

[0035] A kind of synthesis method of p-nitroaniline pipeline reaction, comprises the following steps:

[0036] Step 1: First, carry out nitration reaction of chlorinated benzene and mixed acid to obtain: 63% p-nitrochlorinated benzene, 35% o-nitrochlorinated benzene, 1% p-nitrochlorinated benzene, and dinitrochlorinated benzene 1% mixture;

[0037] Step 2: Put the above mixture into a pulverizer, grind it into a powdered p-nitrochlorobenzene with a particle size of 1000 mesh, put it into the reactor, install a vibration motor at the bottom of the reactor, and vibrate the reactor, while Continuously add cold air into the reactor through the external pipeline of the compressor, control the temperature in the reactor at 10°C, and the pressure at 1MPa for 10 minutes;

[0038] Step 3: Add ammonia water with a concentration of 41% to the powder that has been fully cooled in step 2, and quickly add it to the pipeline reactor with a feed pump, keeping the pressure at 6.9MPa and the t...

Embodiment 3

[0047]A kind of synthesis method of p-nitroaniline pipeline reaction, comprises the following steps:

[0048] Step 1: First, carry out nitration reaction of chlorinated benzene and mixed acid to obtain: 63% p-nitrochlorinated benzene, 35% o-nitrochlorinated benzene, 1% p-nitrochlorinated benzene, and dinitrochlorinated benzene 1% mixture;

[0049] Step 2: Put the above mixture into a pulverizer, grind it into a powdered p-nitrochlorobenzene with a particle size of 1000 mesh, put it into the reactor, install a vibration motor at the bottom of the reactor, and vibrate the reactor, while Continuously add cold air into the reactor through the external pipeline of the compressor, control the temperature in the reactor at 10°C, and the pressure at 1MPa for 10 minutes;

[0050] Step 3: Add ammonia water with a concentration of 41% to the powder that has been fully cooled in step 2, and quickly add it to the pipeline reactor with a feed pump, keeping the pressure at 6.9MPa and the te...

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Abstract

The invention relates to the technical field of chemical engineering, and especially relates to a reaction synthesis method of p-nitroaniline pipeline. The method comprises the following steps: carrying out a nitration reaction on chlorobenzene and a mixed acid to obtain a mixture containing 63% of p-nitrochlorobenzene, 35% of o-nitrochlorobenzene, 1% of m-nitrochlorobenzene and 1% of dinitrochlorobenzene; and putting the mixture into a flour mill, grinding the mixture to form powdery p-nitrochlorobenzene with the particle size of 1000 meshes, putting the ground mixture into a reaction kettle,mounting a vibration motor at the bottom of the reaction kettle, vibrating the reaction kettle, and continuously adding cold air into the reaction kettle through an external pipeline for a compressor. A traditional kettle type reaction is improved, and a tubular reaction is adopted to achieve continuous material use and discharge, so the method has the advantages of stable and easily controlled pressure, no explosion risk, stable pressure, high yield, low tubular reaction cost, stable and safe product quality, and realization of effective recycling of excessive ammonia water and great reduction of the cost by an added subsequent ammonia water recovery process.

Description

technical field [0001] The invention relates to the technical field of chemical industry, in particular to a pipeline reaction synthesis method of p-nitroaniline. Background technique [0002] p-Nitroaniline is an important intermediate of pesticides and dyes, and its consumption is about 40,000 tons a year in China. The reaction synthesis methods of p-Nitroaniline in the prior art all adopt the method of kettle reaction, and the pressure of p-Nitroaniline in this way is Large, low content, large investment in equipment, prone to risk of melting and frying, and the p-nitroaniline produced has a pungent taste, wasting raw materials and not obtaining high-quality p-nitroaniline. In view of this, we propose a pipeline reaction synthesis method for p-nitroaniline. Contents of the invention [0003] The object of the present invention is to provide a kind of synthetic method of p-nitroaniline pipeline reaction, to solve the problem raised in the above-mentioned background tech...

Claims

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Application Information

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IPC IPC(8): C07C209/10C07C211/52
CPCC07C201/08C07C209/10C07C211/52C07C205/12
Inventor 徐德伟
Owner 乐平市景顺实业有限公司
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