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Catalyst for producing melaphenylene from m-dinitrobenze by liquid phase hydrogenation and preparation thereof

A kind of dinitrobenzene liquid, the technology of making m-phenylenediamine, applied in the direction of amino compound preparation, chemical instrument and method, metal/metal oxide/metal hydroxide catalyst, etc., can solve the problem of expensive, unseen patent documents Report, environmental pollution and other issues, to achieve low cost, long life, good selectivity

Inactive Publication Date: 2003-09-03
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Catalytic hydrogenation methods now mostly use framework nickel (Raney Ni) and supported noble metal (such as Pd / C) catalysts, the former will cause environmental pollution during preparation, while the latter is expensive
The supported nickel-based catalyst has the characteristics of low cost, high activity and environmental friendliness, but its application in m-dinitrobenzene hydrogenation has not been reported in patent literature so far.

Method used

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  • Catalyst for producing melaphenylene from m-dinitrobenze by liquid phase hydrogenation and preparation thereof
  • Catalyst for producing melaphenylene from m-dinitrobenze by liquid phase hydrogenation and preparation thereof
  • Catalyst for producing melaphenylene from m-dinitrobenze by liquid phase hydrogenation and preparation thereof

Examples

Experimental program
Comparison scheme
Effect test

example 1

[0014] Example 1: SiO 2 Carrier (specific surface area 432m 2 / g) Roasting at 550°C for 4 hours in advance, measuring its water absorption, using the equal volume impregnation method to impregnate with an aqueous solution of lanthanum nitrate with a content of 5% by weight, immersing at 20°C for 6 hours, and then drying at 110°C, Calcined at 400°C for 5 hours in an air atmosphere, then impregnated with a nickel nitrate aqueous solution with a content of 15% by weight, impregnated at 20°C for 6 hours, then dried at 110°C, and calcined at 400°C for 5 hours in an air atmosphere. Crush the solid particles, and sieve the 80-100 mesh particles. The pre-catalyst was reduced with hydrogen at 400°C for 2 h, and the reduced catalyst was 2 The atmosphere was lowered to room temperature, and protected with nitrogen for later use. The catalyst has excellent m-dinitrobenzene hydrogenation performance, and reacts under the conditions of 100° C., hydrogen pressure of 2.6 Mpa, catalyst dosa...

example 2

[0015] Example 2: Carry out catalyst preparation by the step of example 1, only change the concentration of lanthanum nitrate aqueous solution and be that lanthanum content by weight is 7%, under the constant situation of other conditions, the catalyst prepared is used in m-dinitrobenzene liquid Phase hydrogenation reaction. At the end of the reaction, the conversion rate of dinitrobenzene is higher than 95%, and the yield of m-phenylenediamine is higher than 90%.

example 3

[0016] Example 3: Carry out catalyst preparation by the step of example 1, only change the solution of rare earth element to be cerium nitrate, be 5% by weight, under the situation that other conditions are constant, the catalyst prepared is used in m-dinitrobenzene liquid Phase hydrogenation reaction. At the end of the reaction, the conversion rate of m-dinitrobenzene is higher than 95%, and the yield of m-phenylenediamine is higher than 90%.

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Abstract

A catalyst for preparing metaphenylene diamine by liquid-phase hydrogenation of metadinitrobenzene is composed of the carrier which may be aluminium oxide, SiO2, diatomite, magnesium oxide, TiO2, or activated carbon, and the active component consisting of Ni and the alkali metal, alkali-earth metal, or the compound of RE. Its preparing process includes pretreating carrier, carrying active component and post-treating. Its advantages are high activity and selectivity, and high output rate (more than 93%) of metaphenylene diamine.

Description

technical field [0001] The invention relates to a catalyst and a preparation method for preparing m-phenylenediamine through liquid-phase hydrogenation of m-dinitrobenzene, which belongs to the catalyst preparation technology. Background technique [0002] m-Phenylenediamine is an important organic chemical raw material and intermediate, widely used as an important intermediate in azo dyes, fur dyes, reactive dyes and sulfur dyes in the dye industry; in addition, it is also used in mordants, hair dyes , Color developer, rubber compounding agent, epoxy resin curing agent, petroleum additive, cement coagulant and metal dissolver etc. The industrial production of m-phenylenediamine basically adopts the reduction method of m-dinitrobenzene iron powder. This method has a long history, simple process and mature technology, but the production cost is high, the yield is low, and a large amount of difficult-to-handle aromatic amine-containing Iron sludge and ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/28B01J23/755B01J23/83C07C209/32C07C211/51
Inventor 陈吉祥刘迎新王日杰张继炎
Owner TIANJIN UNIV
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