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A kind of green synthetic method of reducing o-nitroaniline to prepare o-phenylenediamine

A technology of o-nitroaniline and o-phenylenediamine, which is applied in the field of synthesis of o-phenylenediamine, can solve the problems of difficulty in large-scale production, short catalyst deactivation time, and difficult catalyst recovery, and achieve green production and Emissions, suitable for large-scale production and promotion, and environmentally friendly effects

Active Publication Date: 2017-05-31
江阴市华亚化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0009] The process route is relatively mature, but the disadvantages are: the reaction time of the kettle-type ammonium solution is long, the high temperature and high pressure, and the by-product ammonium chloride cause serious corrosion to the equipment, increase equipment investment, and have potential safety hazards
The above-mentioned methods are beneficial to reduce production costs to a certain extent, but there are also defects such as large amount of catalyst used, short catalyst deactivation time, difficult recovery and easy contamination of products by catalysts, making it difficult to achieve large-scale production

Method used

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  • A kind of green synthetic method of reducing o-nitroaniline to prepare o-phenylenediamine
  • A kind of green synthetic method of reducing o-nitroaniline to prepare o-phenylenediamine

Examples

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Effect test

Embodiment 1

[0029] Add 1mol o-nitroaniline, 3g of the above-mentioned supported catalyst (Ni, Se, Fe / C catalyst), 500mL of water and 100mL of ethanol into a stainless steel autoclave with a capacity of 1000mL, set the temperature in the autoclave to 30°C, and then After the air in the autoclave was replaced, 0.5 MPa carbon monoxide was introduced, and the reaction was stirred for 10 hours. The conversion rate of o-phenylenediamine was 99.8% as detected by gas chromatography.

[0030] In this example, o-phenylenediamine is prepared by reduction, with mild reaction conditions, high product yield, long-lasting catalyst activity, high reaction selectivity, less catalyst consumption, easy separation of product and catalyst, and convenient recycling.

Embodiment 2

[0032] Add 1mol o-nitroaniline, 2.5g supported catalyst (Pt, Se, Fe / C catalyst), 500mL water into a stainless steel autoclave with a capacity of 1000mL, set the temperature inside the autoclave to 50°C, and then replace the autoclave with carbon monoxide After neutralizing the air, 0.7MPa carbon monoxide was introduced, and the reaction was stirred for 10 hours. The conversion rate of o-phenylenediamine was 98% as detected by gas chromatography.

[0033] In this example, the preparation of o-phenylenediamine by reduction has mild reaction conditions, high product yield, no pollution, long-lasting catalyst activity, less catalyst consumption, easy separation of product and catalyst, easy recovery and recycling, light treatment of three wastes, and can meet the requirements of cleaning production requirements.

Embodiment 3

[0035] Add 1mol of o-nitroaniline, 3g of supported catalyst (Pt, Se, Ni / C catalyst), 500mL of water and 80mL of acetone into a stainless steel autoclave with a capacity of 1000mL, set the temperature in the autoclave to 100°C, and then replace it with carbon monoxide After the air in the autoclave, 0.5MPa carbon monoxide was introduced, and the reaction was stirred for 10 hours. The conversion rate of o-phenylenediamine was 99.5% as detected by gas chromatography.

[0036] In this example, the preparation of o-phenylenediamine by reduction has mild reaction conditions, high product yield, no pollution, long-lasting catalyst activity, less catalyst consumption, easy separation of product and catalyst, easy recovery and recycling, light treatment of three wastes, and can meet the requirements of cleaning production requirements.

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Abstract

The invention relates to a green synthetic method of preparing o-phenylenediamine by reducing o-nitroaniline, wherein the method includes following steps: with o-nitroaniline as a substrate, dissolving the o-nitroaniline in water or in a mixed liquid composed of water and a co-solvent, and adding a supported catalyst under a carbon monoxide atmosphere, wherein the supported catalyst includes a supporter and a catalyst body supported thereon, and performing a reaction to prepare the o-phenylenediamine at 30-150 DEG C. In the method, the supported catalyst is used for preparing the o-phenylenediamine through reduction. The catalyst is high in selectivity and reaction yield and is mild in reaction condition. The method is environment-friendly in production system and less in treatment load of waste water, waste gas and solid waste, achieves green and clean production of the o-phenylenediamine, and is suitable for large-scale popularization.

Description

technical field [0001] The invention relates to a synthesis method of o-phenylenediamine, in particular to a synthesis method for preparing o-phenylenediamine by reduction of o-nitroaniline. Background technique [0002] O-phenylenediamine is an important organic chemical intermediate. In addition to being used in the production of dyes, it is also the main raw material for systemic fungicides such as pesticides carbendazim, benomyl, and (methyl) thiophanate. It is also a developer , Leveling agent and surfactant, etc. are important raw materials. [0003] At present, there are several routes for the synthesis of o-phenylenediamine, and two of the more important routes are as follows: [0004] First, the patent CN 102633653 reports a method for preparing o-phenylenediamine by catalytic hydrogenation of o-nitroaniline, using o-nitroaniline as a raw material, alcohol as a solvent, and nickel as a catalyst, at a hydrogen pressure of 1 to 6 MPa, At a temperature of 40-80°C, th...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C209/36C07C211/51B01J23/89B01J27/057B01J23/889
Inventor 谭建新马牧
Owner 江阴市华亚化工有限公司
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