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Preparation method of nitrogen-carbon doping modified nickel-based catalyst and application thereof for catalyzing nitrocyclohexane hydrogenation reaction

A nickel-based catalyst and nitrocyclohexane technology, applied in chemical instruments and methods, physical/chemical process catalysts, oxime preparation, etc., can solve problems such as uneven dispersion of active metals, low catalyst activity, and small metal surface area. Achieve the effects of improving production conditions, increasing metal specific surface area, and not corroding equipment

Active Publication Date: 2016-07-20
XIANGTAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This method has the problems of high catalyst cost when supporting noble metals and low catalyst activity when supporting non-noble metals.
[0005] In summary, loading active metals on molecular sieves or activated carbon can significantly improve catalytic activity. However, when noble metals are used, the catalytic effect is better, but the cost is high. When non-noble metals are used, the effect is not ideal and the yield is low. There are also problems such as uneven dispersion of active metals, large particle size, and small metal surface area when loading.

Method used

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  • Preparation method of nitrogen-carbon doping modified nickel-based catalyst and application thereof for catalyzing nitrocyclohexane hydrogenation reaction

Examples

Experimental program
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Effect test

Embodiment 1

[0030] (1) Mix carbon and melamine at a mass ratio of 1:1.1, then add deionized water, then add formaldehyde at a mass ratio of formaldehyde to melamine of 2:1, and then soak for 12 hours;

[0031] (2) Add 1mol / L sodium hydroxide to the solution obtained in step (1) to adjust the pH to 11, then raise the temperature to 75°C for 30 minutes;

[0032] (3) After the reaction solution obtained in step (2) was cooled to room temperature, acetic acid was added to adjust the pH to 2.5, and then stirred for 12 hours;

[0033] (4) centrifuging the reaction solution obtained in step (3), drying at 100°C for 24 hours, and roasting at 450°C for 4 hours to obtain nitrogen-doped carbon;

[0034] (5) The above-mentioned nitrogen-doped carbon is loaded with nickel by impregnation method to obtain a nickel-based catalyst modified by nitrogen-doped carbon, and the loading of nickel is controlled at 20% of the total mass of the catalyst;

[0035] (6) Activate the obtained catalyst with hydrogen,...

Embodiment 2

[0039] (1) Mix carbon and melamine at a mass ratio of 1:1.2, then add deionized water, then add formaldehyde at a mass ratio of formaldehyde to melamine of 2:1, and then impregnate for 15 hours;

[0040] (2) Add 0.5mol / L sodium hydroxide to the solution obtained in step (1) to adjust the pH to 10, and then raise the temperature to 80°C for 40 minutes;

[0041] (3) After the reaction solution obtained in step (2) is cooled to room temperature, add acetic acid to adjust the pH to 3, and then stir for 10 hours;

[0042] (4) centrifuging the reaction solution obtained in step (3), drying at 100°C for 24 hours, and roasting at 450°C for 4 hours to obtain nitrogen-doped carbon;

[0043] (5) The above-mentioned nitrogen-doped carbon is loaded with nickel by impregnation method to obtain a nickel-based catalyst modified by nitrogen-doped carbon, and the loading of nickel is controlled at 20% of the total mass of the catalyst;

[0044] (6) Activate the obtained catalyst with hydrogen,...

Embodiment 3

[0048] (1) Mix carbon and melamine at a mass ratio of 1:1.1, then add deionized water, then add formaldehyde at a mass ratio of formaldehyde to melamine of 3:1, and then impregnate for 20 hours;

[0049] (2) Add 2mol / L potassium hydroxide to the solution obtained in step (1) to adjust the pH to 12, then raise the temperature to 70°C for 60 minutes;

[0050] (3) After the reaction solution obtained in step (2) is cooled to room temperature, add acetic acid to adjust the pH to 2, and then stir for 20 hours;

[0051] (4) centrifuging the reaction solution obtained in step (3), drying at 100°C for 24 hours, and roasting at 450°C for 4 hours to obtain nitrogen-doped carbon;

[0052] (5) The above-mentioned nitrogen-doped carbon is loaded with nickel by impregnation method to obtain a nickel-based catalyst modified by nitrogen-doped carbon, and the loading of nickel is controlled at 20% of the total mass of the catalyst;

[0053] (6) Activate the obtained catalyst with hydrogen, an...

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Abstract

The invention discloses a preparation method of a nitrogen-carbon doping modified nickel-based catalyst and application thereof for catalyzing nitrocyclohexane hydrogenation reaction. According to the invention, a catalyst is firstly subjected to nitrogen doping modification, and then is loaded with nickel, and the obtained catalyst is applied to the nitrocyclohexane hydrogenation reaction. An N doped carbon support is capable of improving the dispersibility of reactive metal remarkably, the particle size of metal is reduced and the specific surface of metal is increased, so that cheap metal Ni is used to replace noble metal as reactive metal, high selectivity of cyclohexanone-oxime can be ensured and the cost is remarkably reduced. The application process is environmentally friendly and simple and has mild conditions, and the yield of cyclohexanone-oxime is obviously improved by improvement of the reaction conditions and the catalyst.

Description

technical field [0001] The invention relates to the fields of material preparation and chemical engineering, in particular to a preparation method of a nitrogen-doped carbon modified nickel-based catalyst and its application in catalyzing the hydrogenation reaction of nitrocyclohexane. Background technique [0002] The hydrogenation of nitrocyclohexane mainly produces cyclohexanone oxime, and cyclohexanone oxime synthesizes caprolactam. Caprolactam is one of the important organic chemical raw materials, and is mainly used to synthesize nylon-6 fiber and nylon-6 engineering plastics. Due to its excellent thermal stability, high mechanical strength, chemical corrosion resistance and processability, caprolactam has a wide range of applications, mainly in the fields of automobiles, medical equipment, ships, electronic appliances, and daily necessities. From a global perspective, the consumption fields of caprolactam mainly include three categories: fibers (civilian silk, industr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/24C07C249/10C07C251/44
CPCB01J27/24C07C249/10C07C251/44
Inventor 刘平乐唐珊珊郝芳熊伟熊绍锋罗和安
Owner XIANGTAN UNIV
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