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Preparation method of high-dispersibility m-dinitrobenzene hydrogenation structuring catalyst

A structured catalyst, m-dinitrobenzene technology, applied in the chemical industry, can solve the problems of low specific surface area, low dispersion, large metal particles, etc., achieve simple process, reduce production cost, and reduce environmental pollution.

Inactive Publication Date: 2013-08-28
WUHAN INSTITUTE OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the cordierite honeycomb ceramic structured matrix cannot meet the needs of structured catalysts due to its low specific surface area. gamma -Al 2 o 3 to coat
Nevertheless, the specific surface area of ​​the coated structured catalyst is still low, generally no more than 40m 2 / g, when the impregnation method is used to load the active components, the main problem is that the dispersion of the active components is low when the active components are loaded, and the metal particles are large, which affects the catalyst activity.
[0004] In the invention patent CN200510083037.6, a vacuum impregnation method is disclosed to prepare a powder catalyst with high dispersion, amorphous state and high desulfurization activity, and the modified γ-Al 2 o 3 As a carrier, the molybdenum salt solution added with surfactant was slowly added to the vacuumed carrier, dried on a water bath shaker after full contact, and finally calcined step by step in a muffle furnace to prepare a granular catalyst with good performance , but this method is not suitable for the preparation of structured catalysts
[0005] In the invention patent CN200710011729.9, a palladium-ruthenium bimetallic powder catalyst prepared by the traditional impregnation method is disclosed in the production of m-phenylenediamine, and a higher yield is obtained, but there is a shortcoming that the product and the catalyst are not easy to separate
[0006] The impregnation method is used to load the active components. Although the operation is simple, the active components are not easy to disperse uniformly. The structured catalyst is prepared by loading the active components by excessive impregnation and vacuum suction, and is used for the catalytic hydrogenation of m-dinitrobenzene to prepare m-dinitrobenzene. Among phenylenediamines, there has been no report so far

Method used

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  • Preparation method of high-dispersibility m-dinitrobenzene hydrogenation structuring catalyst

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Effect test

Embodiment 1

[0035] A kind of preparation method of highly dispersed m-dinitrobenzene hydrogenation structured catalyst, comprises the following steps:

[0036](1) Excessive impregnation: The cordierite honeycomb ceramic substrate coated with γ-Al2O3, as a structured substrate, is immersed in a nickel nitrate impregnation solution with a concentration of 0.5mol / L, and the impregnation time is 1h;

[0037] (2) Drying and roasting: The structured substrate treated by vacuum suction was first rotated and dried at room temperature for 24 hours, then dried at a constant temperature of 120°C for 2 hours, and finally roasted at a constant temperature of 400°C for 3 hours to obtain Ni / γ-Al 2 o 3 / cordierite structured catalyst precursor;

[0038] (3) Repeated load: according to the obtained Ni / γ-Al 2 o 3 / The quality difference between the cordierite structured catalyst precursor and the cordierite honeycomb ceramic matrix coated with γ-Al2O3, calculate the loading amount of the active compone...

Embodiment 2

[0043] A kind of preparation method of highly dispersed m-dinitrobenzene hydrogenation structured catalyst, comprises the following steps:

[0044] (1) Excessive impregnation: The cordierite honeycomb ceramic substrate coated with γ-Al2O3, as a structured substrate, is immersed in a nickel nitrate impregnation solution with a concentration of 0.5mol / L, and the impregnation time is 1h;

[0045] (2) Vacuum suction: Take out the impregnated structured matrix, put it into the vacuum suction system, adjust the vacuum degree to 0.05MPa, and the vacuum time to 2min;

[0046] (3) Drying and roasting: The structured substrate treated by vacuum suction was first rotated and dried at room temperature for 24 hours, then dried at a constant temperature of 120°C for 2 hours, and finally roasted at a constant temperature of 400°C for 3 hours to obtain Ni / γ-Al 2 o 3 / cordierite structured catalyst precursor;

[0047] (4) Repeated load: according to the obtained Ni / γ-Al 2 o 3 / The quality ...

Embodiment 3

[0051] A kind of preparation method of highly dispersed m-dinitrobenzene hydrogenation structured catalyst, comprises the following steps:

[0052] (1) Excessive impregnation: The cordierite honeycomb ceramic substrate coated with γ-Al2O3, as a structured substrate, is immersed in a nickel nitrate impregnation solution with a concentration of 0.2mol / L, and the impregnation time is 2h;

[0053] (2) Vacuum suction: Take out the impregnated structured matrix, put it into the vacuum suction system, adjust the vacuum degree to 0.095MPa, and the vacuum time to 1min;

[0054] (3) Drying and roasting: The structured substrate treated by vacuum suction was first rotated and dried at room temperature for 24 hours, then dried at a constant temperature of 120°C for 2 hours, and finally roasted at a constant temperature of 400°C for 3 hours to obtain Ni / γ-Al 2 o 3 / cordierite structured catalyst precursor;

[0055] (5) Repeated load: according to the obtained Ni / γ-Al 2 o 3 / The quality...

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Abstract

The invention discloses a preparation method of a high-dispersibility m-dinitrobenzene hydrogenation structuring catalyst, which comprises the following steps: (1) impregnating a cordierite honeycomb ceramic matrix coated with gamma-Al2O3 in a nickel nitrate impregnation liquid; (2) performing vacuum suction; (3) drying, and performing constant-temperature roasting to obtain a Ni / gamma-Al2O3 / cordierite structuring catalyst precursor; (4) repeatedly loading until the load mass percent of the active component Ni is 12-14%; and (5) reducing the catalyst precursor with H2 to obtain the high-dispersibility m-dinitrobenzene hydrogenation structuring catalyst. By changing the concentration of the impregnation liquid, controlling the impregnation time and introducing the vacuum suction action, the metal dispersion degree is increased from 9.3% (in the traditional method) to 38.4%; and a nickel-based structuring catalyst having excellent dispersibility, namely the high-dispersibility m-dinitrobenzene hydrogenation structuring catalyst, can be prepared.

Description

technical field [0001] The invention belongs to the field of chemical industry, and in particular relates to a preparation method of a highly dispersed m-dinitrobenzene hydrogenation structured catalyst. Background technique [0002] Structured catalysts are increasingly used in petrochemical processes. In terms of catalytic hydrogenation, the production of hydrogen peroxide from anthraquinone is the earliest application of structured catalysts to achieve industrialized heterogeneous reactions. The monolithic structure of structured catalysts makes the operation simple Easy to implement and realize large-scale production. Nijhuis et al. Ni / Al 2 o 3 / cordierite structured catalysts are applied to the hydrogenation reaction of α-methylstyrene and benzyl alcohol, and the reactivity in the structured reactor and the traditional trickle bed reactor are compared respectively, and the results show that the former has a higher selectivity and yield. Grezee et al. preliminarily d...

Claims

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Application Information

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IPC IPC(8): B01J23/755B01J37/02C07C211/51C07C209/36
Inventor 刘少文管卓龙程娟
Owner WUHAN INSTITUTE OF TECHNOLOGY
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