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Application of metal-free hydrogenation catalyst in catalytic nitrocyclohexane hydrogenation reaction

A hydrogenation catalyst, nitrocyclohexane technology, applied in physical/chemical process catalysts, organic chemistry, chemical instruments and methods, etc., can solve the problems of high catalyst cost, metal loss, complicated catalyst processes and steps, etc. The preparation method is simple, the production cost is low, and the hydrogenation effect is good.

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

AI Technical Summary

Problems solved by technology

Its active components are still precious metals, and the cost of the catalyst is very high. This invention also uses base metal nickel as the catalytic active metal, but the loss of active metals is inevitable during the reaction, which pollutes the environment.
[0007] In summary, the preparation cost of noble metal catalysts is high, and metal dissolution and loss are prone to occur during the reaction, which not only leads to a continuous decline in activity, but also causes environmental pollution.
Although non-precious metals greatly reduce the cost of catalyst preparation, the catalyst process and steps are complicated, which is not conducive to engineering operations, and the amount of metal used is large. At the same time, the phenomenon of metal loss is inevitable, causing environmental pollution.

Method used

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  • Application of metal-free hydrogenation catalyst in catalytic nitrocyclohexane hydrogenation reaction
  • Application of metal-free hydrogenation catalyst in catalytic nitrocyclohexane hydrogenation reaction

Examples

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Effect test

Embodiment 1

[0042] A method for preparing a metal-free hydrogenation catalyst, using melamine as a nitrogen source to prepare nitrogen-doped carbon nanotubes by means of an impregnation method, specifically comprising the following steps:

[0043] (1) Oxidation treatment of carbon nanotubes: carbon nanotubes are acidified by adding a mixed acid of concentrated sulfuric acid and concentrated nitric acid with a volume ratio of 3:1 at a solid-to-liquid ratio of 1:80 for acidification for 12 hours, centrifuged and washed, and dried at 80°C for 12 hours Obtain carbon nanotubes.

[0044] (2) Take an appropriate amount of the above-mentioned oxidized carbon nanotubes, mix them with melamine at a mass ratio of 1:1, add deionized water, and add an appropriate amount of formaldehyde twice the mass of melamine, and immerse for 12 hours;

[0045] (3) Add 1mol / L NaOH dropwise to the above solution to adjust the pH to about 10;

[0046] (4) Raise the temperature to 75°C for 30 minutes;

[0047] (5) A...

Embodiment 2

[0051] A method for preparing a metal-free hydrogenation catalyst, using melamine as a nitrogen source to prepare nitrogen-doped carbon nanotubes by means of an impregnation method, specifically comprising the following steps:

[0052] (1) Oxidation treatment of carbon nanotubes: carbon nanotubes were acidified by adding a mixed acid of concentrated sulfuric acid and concentrated nitric acid with a volume ratio of 3:1 at a solid-to-liquid ratio of 1:60 for 15 hours, centrifuged and washed, and dried at 100°C for 12 hours Obtain carbon nanotubes.

[0053] (2) Take an appropriate amount of the above-mentioned oxidized carbon nanotubes, mix them with melamine at a mass ratio of 1:1.1, add deionized water, and add an appropriate amount of formaldehyde three times the mass of melamine, and immerse for 10 hours;

[0054] (3) Add 0.5mol / L KOH dropwise to the above solution to adjust the pH to about 11;

[0055] (4) Raise the temperature to 70°C for 60 minutes;

[0056] (5) After co...

Embodiment 3

[0060] A method for preparing a metal-free hydrogenation catalyst, using melamine as a nitrogen source to prepare nitrogen-doped carbon nanotubes by means of an impregnation method, specifically comprising the following steps:

[0061] (1) Oxidation treatment of carbon nanotubes: carbon nanotubes are acidified by adding a mixed acid of concentrated sulfuric acid and concentrated nitric acid with a volume ratio of 3:1 at a solid-to-liquid ratio of 1:120 for 8 hours, centrifuged and washed, and dried at 80°C for 12 hours Obtain carbon nanotubes.

[0062] (2) Take an appropriate amount of the above-mentioned oxidized carbon nanotubes, mix them with melamine at a mass ratio of 1:1.2, add deionized water, and add an appropriate amount of formaldehyde twice the mass of melamine, and immerse for 20 hours;

[0063] (3) Add 2mol / L NaCO dropwise to the above solution 3 , adjust the pH to about 12;

[0064] (4) Raise the temperature to 80°C for 30 minutes;

[0065] (5) After cooling t...

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Abstract

The invention discloses an application of a metal-free hydrogenation catalyst in catalytic nitrocyclohexane hydrogenation reaction, wherein the metal-free hydrogenation catalyst adopted by the application is a nitrogen doped carbon nanotube prepared by taking melamine as a nitrogen source through an impregnation method or a nitrogen doped carbon nanotube prepared by taking ammonia gas a nitrogen source through an in-situ synthesis process; and the obtained catalyst is applied to nitrocyclohexane hydrogenation reaction. According to the application, the nitrogen doped carbon nanotube is used as a nitrocyclohexane hydrogenation catalyst, and any metal active ingredient is not loaded, so that the purpose of hydrogenation catalysis is achieved by only utilizing a nitrogen doped modifying method. The whole reaction process avoids use of noble metals, so that the cost is reduced, the environment is not polluted, and the catalyst can be repeatedly used. The catalyst disclosed by the invention is simple in preparation method, is low in production cost, is good in hydrogenation effect, and is easy to control in reaction; and the catalyst is environment-friendly, does not cause secondary pollution to the environment, and can be widely applied to various hydrogenation reactions.

Description

technical field [0001] The invention relates to the fields of material preparation and chemical engineering, in particular to the application of a metal-free hydrogenation catalyst 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, industrial silk, carpet silk), engineering plastics...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C249/10C07C251/44B01J27/24B01J21/18
CPCB01J21/185B01J27/24C07C249/10C07C251/44
Inventor 刘平乐熊伟郝芳熊绍锋罗和安
Owner XIANGTAN UNIV
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