Method for preparing diaminonaphthalene by catalytic hydrogenation of dinitronaphthalene

A technology of dinitronaphthalene catalysis and diaminonaphthalene, which is applied in the preparation of amino compounds, chemical instruments and methods, and the preparation of organic compounds, can solve the problems of large catalyst consumption and low product yield, and reduce catalyst consumption, The effect of increasing the conversion rate and improving the activity of the catalyst

Inactive Publication Date: 2009-11-11
JIANGSU POLYTECHNIC UNIVERSITY +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The deficiency of preparing diaminonaphthalene according to the method of above-

Method used

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  • Method for preparing diaminonaphthalene by catalytic hydrogenation of dinitronaphthalene

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Effect test

Embodiment 1

[0020] In a stirred stainless steel autoclave, add 0.5% Pd / activated carbon catalyst 0.02g (carrier activated carbon without pretreatment), 1,8-dinitronaphthalene 2g, isopropanol 40ml, close the autoclave, and replace with nitrogen Air in the reactor for three times, then replace the nitrogen in the reactor with hydrogen for three times and keep the pressure in the reactor, raise the temperature to 90°C, fill in hydrogen to make the reaction pressure to 4MPa, start stirring, keep the temperature until the pressure no longer drops , the reaction solution was taken out, the catalyst was removed by filtration, and the filtrate was analyzed by liquid chromatography.

Embodiment 2

[0022] In a stirred stainless steel autoclave, add 5% Pd / activated carbon catalyst 0.02g (carrier activated carbon without pretreatment), 1,5-dinitronaphthalene 2g, isopropanol 40ml, close the autoclave, and replace with nitrogen Air in the reactor for three times, then replace the nitrogen in the reactor with hydrogen for three times and keep the pressure in the reactor, raise the temperature to 90°C, fill in hydrogen to make the reaction pressure to 4MPa, start stirring, keep the temperature until the pressure no longer drops , the reaction solution was taken out, the catalyst was removed by filtration, and the filtrate was analyzed by liquid chromatography.

Embodiment 3

[0024]In a stirred stainless steel autoclave, add 0.02g of 5% Pd / mesoporous carbon catalyst (the carrier mesoporous carbon is not pretreated), 2g of 1,8-dinitronaphthalene, 40ml of isopropanol, and close the reactor , Replace the air in the reactor with nitrogen three times, then replace the nitrogen in the reactor with hydrogen three times and keep the pressure in the reactor, raise the temperature to 90°C, fill in hydrogen to make the reaction pressure to 4MPa, start stirring, and keep the temperature until the pressure Take out the reaction liquid until it no longer drops, remove the catalyst by filtration, and analyze the filtrate by liquid chromatography.

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Abstract

A method for preparing diaminonaphthalene by catalytic hydrogenation of dinitronaphthalene relates to a preparation technology of the diaminonaphthalene, which comprises the following steps: adding a palladium catalyst comprising active components and a carrier and adding the dinitronaphthalene and solvent to a stainless steel high-pressure reactor with an agitator, closing the reactor, replacing air in the reactor with nitrogen for at least three times and then replacing the nitrogen in the reactor with hydrogen for at least three times, and then filling the hydrogen in the reactor so that the reaction pressure in the reactor reaches 0.4-4.0MPa, heating the reactor so that the reaction temperature reaches 30-150 DEG C so as to carry out catalytic hydrogenation to prepare the diaminonaphthalene. The method adopts the hydrogenation reaction technology in the stainless steel high-pressure reactor with the agitator; a catalyst carrier is pretreated to improve the activity of the catalyst and reduce the consumption of the catalyst. By optimizing the technological conditions, the rate of conversion from the dinitronaphthalene to the diaminonaphthalene is effectively improved and high selectivity of the product diaminonaphthalene is maintained.

Description

technical field [0001] The invention relates to a preparation process of diaminonaphthalene, in particular to a method for preparing diaminonaphthalene by catalytic hydrogenation of dinitronaphthalene. Background technique [0002] The reduction of dinitronaphthalene to diaminonaphthalene is an important organic synthesis unit reaction and an important way to prepare diaminonaphthalene, and the product diaminonaphthalene is an important pigment intermediate. Diaminonaphthalene mainly includes 1,5-diaminonaphthalene and 1,8-diaminonaphthalene. [0003] 1,5- and 1,8-diaminonaphthalene are two important compounds among the isomers of diaminonaphthalene. They are mainly used as intermediates of dyes (pigments) and also as raw materials for resins and pesticides. Among them, in addition to being used to prepare azo dyes, 1,5-diaminonaphthalene is also an important polyurethane material intermediate. 1,5-naphthalene diisocyanate is prepared from 1,5-diaminonaphthalene, and then p...

Claims

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Application Information

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IPC IPC(8): C07C209/36C07C211/58B01J23/44
Inventor 张伟孙建芝李明时鲁墨弘单玉华朱建军倪海平陈玉忠张东宝
Owner JIANGSU POLYTECHNIC UNIVERSITY
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