Nickel-based structured catalyst for synthesizing m-phenylenediamine through hydrogenation of m-dinitrobenzene and its preparation method

A m-phenylenediamine nickel-based, structured catalyst technology, applied in the field of catalysis, can solve the problems of low product m-phenylenediamine selectivity, high bed pressure drop, etc., to improve heat transfer and mass transfer efficiency, and airflow resistance Low, easy industrial production effect

Inactive Publication Date: 2012-02-15
WUHAN INSTITUTE OF TECHNOLOGY +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The purpose of the present invention is to overcome the shortcomings of the high pressure drop of the traditional granular catalyst bed, which leads to the low selectivity of the product m-phenylenediamine, and provide a structured catalyst

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] a. First take 43.27ml of concentrated nitric acid (68.01wt%) in a 250ml volumetric flask to prepare 2.5mol / L of HNO 3 Solution, diameter 10mm, length 30mm, hole density 400cells / in 2 (62cells / cm 2 ), a cordierite ceramic substrate with a mass of 1.58g was immersed in HNO 3 Treat in the solution for 30 minutes, take it out and wash it with deionized water, and then dry it in an oven for 2 hours for later use; weigh 13.33g of activated alumina powder (particle size 4.81μm) and 40ml of distilled water as raw materials, and use mechanical stirring method to configure γ-Al 2 o 3 coating suspension; the treated cordierite honeycomb ceramic matrix in the above-mentioned γ-Al 2 o 3 Immerse in the coating suspension for 2 minutes, repeat the immersion 3 times, take it out and spin dry it at room temperature for 24 hours, then dry it in an oven at 120°C for 2 hours, and then bake it in a muffle furnace at 400°C for 4 hours. The coating load is 13.55wt%. That is, the catalyst...

Embodiment 2

[0021] a. preparation of catalyst support is the same as in Example 1

[0022] b. Weigh 12.7gNi(NO 3 ) 2 .6H 2 O, 3.91g La(NO 3 ) 2 .6H 2 O was dissolved in 50ml deionized water, and the prepared catalyst carrier was impregnated in the above NiNO 3 -LaNO 3 Take out the aqueous solution, take it out and spin dry it at room temperature for 12 hours, dry it in an oven at 120°C for 2 hours, and bake it in a muffle furnace at 400°C for 4 hours to obtain a Ni / γ-Al with a Ni content of 15wt% and an additive La content of 3wt%. 2 o 3 / cordierite structured catalyst.

[0023] c. The reduction and evaluation of the catalyst was carried out according to the method of Example 1, the conversion rate of m-dinitrobenzene was 88%, and the selectivity was 85%.

Embodiment 3

[0025] a. preparation of catalyst support is the same as in Example 1

[0026] b. Weigh 4.38g Ni(NO 3 ) 2 .6H 2 O was dissolved in 50ml deionized water, and the prepared catalyst carrier was impregnated in the above NiNO 3Take it out from the aqueous solution, take it out and spin dry it at room temperature for 12 hours, dry it in an oven at 120°C for 2 hours, and bake it in a muffle furnace at 400°C for 4 hours to obtain Ni / γ-Al with a Ni content of 5wt%. 2 o 3 / cordierite structured catalyst.

[0027] c. The reduction and evaluation of the catalyst was carried out according to the method of Example 1, the conversion rate of m-dinitrobenzene was 78%, and the selectivity was 80%.

[0028] Compared with Catalyst 1, the introduction of promoters improved the catalytic activity. Characterized by TPR, the results show that the introduction of additive La inhibits the NiAl 2 o 4 Formation changes the performance of the catalyst by changing the structure of the catalyst.

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Abstract

The invention relates to a nickel-based structured catalyst for synthesizing m-phenylenediamine through hydrogenation of m-dinitrobenzene, which takes cordierite honeycomb ceramic as a matrix, gamma-Al2O3 as a composite carrier of a coating and La modified Ni as an active component. The preparation method comprises the following steps: taking cordierite as a substrate and active alumina as a coating, preparing the gamma-Al2O3 / cordierite composite carrier by using an immersion method; selecting appropriate nickel salt and lanthanum salt, immersing, drying and calcining to obtain a catalyst precursor, reducing through hydrogen to obtain the structured catalyst. The cordierite structured catalyst is capable of keeping the characteristics of an original particles supported Ni catalyst and preparing a structured reactor, so that hydrogenation reaction is carried out under continuous state. Simultaneously, an auxiliary agent La is introduced in the catalyst for inhibiting the interacting effect of the active component and the carrier, and weakening the formation of NiAl2O4 which is not beneficial to the hydrogenation reaction activity. So that the conversion rate and selectivity of m-dinitrobenzene hydrogenation reaction can be enhanced further.

Description

technical field [0001] The invention belongs to the technical field of catalysis, and specifically relates to a loaded nickel-based structured catalyst used in the hydrogenation process of various organic compounds in petrochemical, pharmaceutical, dye and other industries, as well as its preparation method and application, and is especially suitable for nitro Selective hydrogenation of benzene. Background technique [0002] In the dye industry, m-phenylenediamine is widely used as an intermediate of azo dyes, fur dyes, reactive dyes and sulfur dyes, and has a good application prospect. Among the methods for synthesizing m-phenylenediamine, the catalytic hydrogenation method has attracted more and more attention as an environmentally friendly process route with simple process and good product quality. The core of catalytic hydrogenation technology is the catalyst, therefore, the development of catalysts with excellent performance has become the key to the development of thi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/83C07C211/51C07C209/36
Inventor 刘少文尹玲玲包传平李萍赵慧平王文灿
Owner WUHAN INSTITUTE OF TECHNOLOGY
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