Method for preparing o-phenylenediamine by utilizing catalytic reduction of ortho-nitroaniline

A technology of o-nitroaniline and o-phenylenediamine, which is applied in the preparation of o-phenylenediamine and in the field of organic synthesis, can solve the problems of inability to be recycled for a long time, high initial activity, loss, etc., and achieves difficult deactivation and good maintenance , The effect of catalyst stabilization

Active Publication Date: 2019-01-18
ANHUI DONGZHI GUANGXIN AGROCHEMICAL CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0009] The present invention aims at the deficiencies of the prior art, such as high initial activity, but can not be recycled for a long time, the problem of loss, the problem of inactivation, etc., and proposes a new method for preparing o-phenylenediamine by catalytic reduction of o-nitroaniline

Method used

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  • Method for preparing o-phenylenediamine by utilizing catalytic reduction of ortho-nitroaniline
  • Method for preparing o-phenylenediamine by utilizing catalytic reduction of ortho-nitroaniline

Examples

Experimental program
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Effect test

Embodiment 1

[0019] The preparation of embodiment 1 Pd-Ni bimetallic catalyst (Pd-Ni / GO)

[0020] 50ml of deionized water, 0.5ml of 0.02mol / L PdCl 2 , 0.5ml of 0.02mol / L NiCl 2 , 0.8g graphene oxide, after ultrasonication at 160W for 30min at room temperature, 2ml hydrazine hydrate was added dropwise, continued ultrasonication at 160W, 60°C for 1h, centrifugation, washing with deionized water 3 times, centrifugation, and vacuum drying to obtain Pd-Ni / GO.

Embodiment 2

[0021] The preparation of embodiment 2 other catalysts

[0022] According to the method of Example 1, adjust different metal salts, such as using ferric chloride instead of nickel chloride to obtain Pd-Fe / GO, copper chloride instead of nickel chloride to obtain Pd-Cu / GO, and cobalt chloride instead of chloride Nickel can obtain Pd-Co / GO, chloroplatinic acid can replace palladium chloride to obtain Pt-Ni / GO, chloroauric acid can obtain Au-Ni / GO, and sequentially prepare Pt-Fe / GO, Pt-Cu / GO, Pt-Co / GO, Au-Cu / GO, Au-Co / GO. Wherein it involves the catalyst preparation of iron, the reducing agent adopts ascorbic acid, and the dosage is 0.4g.

Embodiment 3

[0023] Embodiment 3 contrast catalyst and blank catalyst

[0024] At the same time, only a single metal salt can be used to obtain Pd / GO, Pt / GO, Au / GO, Cu / GO, Co / GO, Ni / GO, and without using any metal, a blank catalyst, that is, a reduced GO catalyst support can be obtained . The dosage of a single salt is 1ml.

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Abstract

The invention provides a method for preparing o-phenylenediamine by utilizing catalytic reduction of ortho-nitroaniline. A bimetal loaded graphene oxide is taken as a catalyst for taking part in hydrogenation reduction in a reaction kettle with a polytetrafluoroethylene liner. According to the scheme, the problems of difficulty in realizing industrial production, difficulty in keeping long-term stable activity of catalyst and the like of the prior art can be solved. The method has a broad industrial application prospect.

Description

technical field [0001] The invention belongs to the field of organic synthesis and relates to the preparation of organic chemical intermediates, in particular to the field of preparation of o-phenylenediamine. Background technique [0002] O-phenylenediamine, also known as 1,2-phenylenediamine (1,2-diaminobenzene), is an intermediate of dyes, pesticides, auxiliaries, photosensitive materials, etc. It is a dye fur yellow brown M, mainly used in pesticides and medicines , Rubber, dyes and other industries are used to manufacture polyamide, polyurethane, carbendazim and thiophanate, vat red GG, leveling agent, anti-aging agent MB, and also used to prepare developer and surfactant. [0003] O-phenylenediamine is widely used in the production of benzimidazole fungicides, such as carbendazim, thiophanate, mebendazole, etc., and those containing benzimidazole ring structure have become a direction for the research and development of new fungicides. The representative product is br...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C209/36C07C211/51B01J23/89
CPCB01J23/8906B01J23/8913B01J23/892B01J23/8926C07C209/36C07C211/51
Inventor 陈永贵黄中桂蔡小林袁晓林杨镭王先武罗立忠袁树林章子虎张俊丁锐
Owner ANHUI DONGZHI GUANGXIN AGROCHEMICAL CO LTD
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