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A kind of synthesis technique of 2-cyano-4-nitro-6-bromoaniline

A synthesis process, the technology of nitroaniline, which is applied in the synthesis process of 2-cyano-4-nitro-6-bromoaniline and the synthesis process of disperse dye intermediates, can solve the problem that the quality requirements and environmental protection requirements cannot be met, Unable to meet the annual output, complex steps and other issues, to achieve the effect of low cost, reduced energy consumption and stable quality

Active Publication Date: 2016-09-28
SHAOXING JIANG HUA CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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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  • A kind of synthesis technique of 2-cyano-4-nitro-6-bromoaniline
  • A kind of synthesis technique of 2-cyano-4-nitro-6-bromoaniline
  • A kind of synthesis technique of 2-cyano-4-nitro-6-bromoaniline

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Experimental program
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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, after reacting to the end point, distill and recover the solvent at 90°C; the ammonolysis reaction temperature is 130°C, and the ammonolysis reaction pressure is 3...

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Abstract

The invention relates to a synthesis process of 2-cyano-4-nitro-6-bromoaniline, comprising the following steps (1) putting o-chlorobenzonitrile into a sulfuric acid medium, adding mixed acid dropwise for nitration, and adding water to the nitrated compound Filter after water analysis, dissolve the nitrating material in chlorobenzene, carry out ammonolysis reaction between the nitric chloride mixture and liquid ammonia, distill and recover the solvent, carry out suction filtration and wash to neutrality, and obtain the wet product; (2) 2-cyano ‑4‑nitroaniline is put into a sulfuric acid medium, and hydrogen bromide and an oxidant are added dropwise to react, and after reaching the end point, filter to obtain the wet material of 2‑cyano‑4‑nitro‑6‑bromoaniline; the process of the present invention The steps are simple and easy to control, and the obtained product has high yield, high purity, and stable quality, and the environmental protection index can meet market needs, low cost, less sewage, and reduced energy consumption. It is a production process with low energy consumption and low 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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Patent Type & Authority Patents(China)
IPC IPC(8): C07C255/58C07C253/30
Inventor 陈立火李江华李炳潮鲁菊丽
Owner SHAOXING JIANG HUA CHEM