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Preparation method of m-nitroaniline

A technology for nitroaniline and m-dinitrobenzene, which is applied in the field of preparation of m-nitroaniline, can solve problems such as difficult separation of solvent and reaction solution, and achieve the effects of high selectivity, high conversion rate and simple processing operation

Inactive Publication Date: 2018-06-29
NANJING POLYTECHNIC INSITUTE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the process uses a toxic solvent tetrahydrofuran, and it is difficult to separate the solvent from the reaction solution.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Add m-dinitrobenzene 20.0g in autoclave, [Bmim]BF 4 100.0g, water 2.4g, Pd-Fe / TiO 2 Catalyst 2.0g, replaced by CO after purging with nitrogen, the temperature was raised to 130°C, CO gas was introduced, the reaction pressure was controlled at 2.0MPa, and the reaction was continued for 4h. Cooling crystallization separation, HPLC analysis. The yield of m-nitroaniline is 96.8%, the conversion rate of m-dinitrobenzene is 98.7%, and the selectivity of m-nitroaniline is 98.1%.

Embodiment 2

[0020] Add m-dinitrobenzene 20.0g in autoclave, [Bmim]BF 4 200.0g, water 2.4g, Pd-Fe / TiO 2 Catalyst 3.0g, replaced by CO after purging with nitrogen, the temperature was raised to 180°C, CO gas was introduced, the reaction pressure was controlled at 0.2MPa, and the reaction was continued for 2h. Cooling crystallization separation, HPLC analysis. The yield of m-nitroaniline is 95.0%, the conversion rate of m-dinitrobenzene is 99.0%, and the selectivity of m-nitroaniline is 96.0%.

Embodiment 3

[0022] Add m-dinitrobenzene 20.0g in autoclave, [Bmim]BF 4 100.0g, water 2.4g, Pd-Fe / TiO 2 Catalyst 2.5g, replaced by CO after purging with nitrogen, the temperature was raised to 160°C, CO gas was introduced, the reaction pressure was controlled at 1.0MPa, and the reaction was continued for 4h. Cooling crystallization separation, HPLC analysis. The yield of m-nitroaniline is 97.4%, the conversion rate of m-dinitrobenzene is 98.9%, and the selectivity of m-nitroaniline is 98.5%.

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PUM

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Abstract

The invention relates to a preparation method of m-nitroaniline. The m-nitroaniline is prepared from m-dinitrobenzene serving as a raw material, ionic liquid [Bmim]BF4 serving as a reaction medium, Pd-Fe / TiO2 serving as a catalyst and CO / H2O serving as a reducing agent under certain reaction pressure and at certain reaction temperature. The method is simple in treatment operation, high in conversion rate and high in selectivity. Through test, the conversion rate of the m-dinitrobenzene is more than or equal to 98.0 percent and the selectivity of the m-nitroaniline is more than or equal to 96.0percent.

Description

technical field [0001] The invention relates to the technical field of fine organic chemistry, in particular to a preparation method of m-nitroaniline. Background technique [0002] m-Nitrophenylamine (m-Nitrophenylamine) is an important fine chemical intermediate, which is widely used in dyestuff, medicine, rubber and other industries. Raw materials for agents, etc. As a kind of important chemical intermediate material, m-nitroaniline has been paid attention to by people. The preparation of m-nitroaniline mainly includes m-nitrochloroaniline ammonolysis method and m-dinitrobenzene reduction method. [0003] The m-nitrochloroaniline ammonolysis method uses m-nitrochlorobenzene as a raw material to directly prepare m-nitroaniline through ammonolysis under high pressure. This process has high selectivity and can prepare high-purity m-nitroaniline, but it will produce a large amount of Chlorine-containing wastewater is not environmentally friendly. The raw material of m-din...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C209/36C07C211/52
CPCC07C209/36C07C211/52
Inventor 张金龙王明权任春梅陈学梅
Owner NANJING POLYTECHNIC INSITUTE