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Synthesis process of 2-cyano-4-nitro-6-bromaniline

A synthesis process, nitroaniline technology, applied in the synthesis process of disperse dye intermediates, 2-cyano-4-nitro-6-bromoaniline synthesis process field, can solve the problem of failure to meet quality requirements and environmental protection requirements, Unable to meet the annual output, serious pollution and other problems, to achieve the effect of low cost, reduced energy consumption, and low energy consumption

Active Publication Date: 2015-02-11
SHAOXING JIANG HUA CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, due to the complex steps of the traditional synthesis process of 2-cyano-4-nitro-6-bromoaniline, many by-products, low yield, low purity and serious pollution, it cannot meet the requirements of 2-cyano-4-bromoaniline in the art. The annual output requirements of nitro-6-bromoaniline cannot meet the increasingly stringent quality requirements and environmental protection requirements

Method used

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  • Synthesis process of 2-cyano-4-nitro-6-bromaniline
  • Synthesis process of 2-cyano-4-nitro-6-bromaniline

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Embodiment 1

[0029] The synthetic technique of 2-cyano-4-nitro-6-bromoaniline of the present invention comprises the following steps:

[0030] (1) Synthesis of 2-cyano-4-nitroaniline:

[0031] A1. Put 100g o-chlorobenzonitrile into 333g sulfuric acid medium, then add the mixed acid dropwise, and carry out nitration at 5-10°C to obtain the nitrated compound; the mixed acid is HNO 3 and H 2 SO 4 Mixed with a mass percentage of 0.5:1;

[0032] A2, the nitrated compound in the step A1 is subjected to water analysis, and after the water analysis, it is filtered to obtain the nitrated material;

[0033] A3, the nitrating material in step A2 is dissolved in 400g chlorobenzene, obtains nitric chloride mixed solution;

[0034] A4, carry out ammonolysis reaction with the nitric chloride mixed solution in step A3 and liquefied ammonia, distill and recover solvent at 80 ℃ after reacting to the end point; The ammonolysis reaction temperature is 110 ℃, and the ammonolysis reaction pressure is 2.6MPa...

Embodiment 2

[0045] The synthetic technique of 2-cyano-4-nitro-6-bromoaniline of the present invention comprises the following steps:

[0046] (1) Synthesis of 2-cyano-4-nitroaniline:

[0047] A1. Put 100g o-chlorobenzonitrile into 280g sulfuric acid medium, then add the mixed acid dropwise, and carry out nitration at 5-10°C to obtain the nitrated compound; the mixed acid is HNO 3 and H 2 SO 4 Mixed with a mass percentage of 1:1;

[0048] A2, the nitrated compound in the step A1 is subjected to water analysis, and after the water analysis, it is filtered to obtain the nitrated material;

[0049] A3, the nitrating material in step A2 is dissolved in 360g chlorobenzene, obtains nitric chloride mixed solution;

[0050] A4, carry out ammonolysis reaction with the nitric chloride mixed solution in step A3 and liquefied ammonia, distill and recover solvent at 100 ℃ after reacting to the end point; The ammonolysis reaction temperature is 150 ℃, and the ammonolysis reaction pressure is 4.5MPa;...

Embodiment 3

[0061] The synthetic technique of 2-cyano-4-nitro-6-bromoaniline of the present invention comprises the following steps:

[0062] (1) Synthesis of 2-cyano-4-nitroaniline:

[0063]A1. Put 100g o-chlorobenzonitrile into 300g sulfuric acid medium, then add the mixed acid dropwise, and carry out nitration at 5-10°C to obtain the nitrated compound; the mixed acid is HNO 3 and H 2 SO 4 Mixed with a mass percentage of 0.75:1;

[0064] A2, the nitrated compound in the step A1 is subjected to water analysis, and after the water analysis, it is filtered to obtain the nitrated material;

[0065] A3, the nitrating material in step A2 is dissolved in 375g chlorobenzene, obtains nitric chloride mixed solution;

[0066] A4, carry out ammonolysis reaction with the nitric chloride mixed solution in step A3 and liquefied ammonia, distill and recover solvent at 90 ℃ after reacting to the end point; The ammonolysis reaction temperature is 130 ℃, and the ammonolysis reaction pressure is 3.6MPa...

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Abstract

The invention relates to a synthesis process of 2-cyano-4-nitro-6-bromaniline. The synthesis process comprises the following steps: (1) putting chlorobenzonitrile into a sulfuric acid medium, dropwise adding a mixed acid and carrying out nitration, diluting a nitrified product by adding water and then filtering, dissolving the nitrified material in chlorobenzene, carrying out an ammonolysis reaction on a mixed nitrate-chloride liquid and liquid ammonia and then distilling so as to recycle a solvent, carrying out suction filtration and washing the solvent with water until the solvent is neutral, thereby obtaining a wet product; and (2) putting 2-cyano-4-nitroaniline into the sulfuric acid medium, dropwise adding hydrogen bromide and an oxidizing agent and reacting until the reaction is completely finished, and then filtering so as to obtain a wet 2-cyano-4-nitro-6-bromaniline product. The synthesis process is simple in process procedures and easy to control; and the prepared 2-cyano-4-nitro-6-bromaniline is high in yield and purity, stable in quality, low in cost, less in sewage generation and low in energy consumption, and the environmental index of the prepared 2-cyano-4-nitro-6-bromaniline can meet market demands. Thus, the process provided by the invention is a production process with low energy consumption and pollution.

Description

technical field [0001] The invention relates to a synthesis process of a disperse dye intermediate, in particular to a synthesis process of 2-cyano-4-nitro-6-bromoaniline, belonging to the technical field of fine chemicals. Background technique [0002] As we all know, 2-cyano-4-nitro-6-bromoaniline is a very important intermediate of disperse dyes and an important raw material for the synthesis of disperse dyes such as disperse blue 183. However, due to the complex steps of the traditional synthesis process of 2-cyano-4-nitro-6-bromoaniline, many by-products, low yield, low purity and serious pollution, it cannot meet the requirements of 2-cyano-4-bromoaniline in the art. The requirement of annual output of nitro-6-bromoaniline also can't meet increasingly stringent quality requirement and environmental protection requirement. Therefore, searching for a 2-cyano-4-nitro-6-bromoaniline production process with simple process, high product yield, less sewage and stable product...

Claims

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Application Information

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IPC IPC(8): C07C255/58C07C253/30
Inventor 陈立火李江华李炳潮鲁菊丽
Owner SHAOXING JIANG HUA CHEM
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