Application of metal-free hydrogenation catalyst in catalyzing hydrogenation reaction of nitrobenzene and derivatives thereof

A technology of nitrobenzene derivatives and hydrogenation catalysts, which is applied in the preparation of organic compounds, catalysts for physical/chemical processes, preparation of amino compounds, etc., can solve the problems of high catalyst cost, metal loss, metal dissolution loss, etc. The method is simple, the production cost is low, and the reaction is easy to control

Active Publication Date: 2016-06-15
XIANGTAN UNIV
View PDF4 Cites 16 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although this method can reduce the loss of the catalyst to a certain extent, its active components are still noble metals, and the cost of the catalyst is very high. The invention also uses base metal nickel as the catalytically active metal, but the loss of the active metal is unavoidable in the reaction. polluted the environment
[0006] In summary, the preparation cost of noble metal catalysts is high, and metal dissolution and loss are

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Application of metal-free hydrogenation catalyst in catalyzing hydrogenation reaction of nitrobenzene and derivatives thereof
  • Application of metal-free hydrogenation catalyst in catalyzing hydrogenation reaction of nitrobenzene and derivatives thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] 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:

[0042] (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.

[0043] (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;

[0044] (3) Add 1mol / L NaOH dropwise to the above solution to adjust the pH to about 10;

[0045] (4) Raise the temperature to 75°C for 30 minutes;

[0046] (5) A...

Embodiment 2

[0050] 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:

[0051] (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.

[0052] (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;

[0053] (3) Add 0.5mol / L KOH dropwise to the above solution to adjust the pH to about 11;

[0054] (4) Raise the temperature to 70°C for 60 minutes;

[0055] (5) After co...

Embodiment 3

[0059] 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:

[0060] (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 acidification for 8 hours, centrifuged and washed, and dried at 80°C for 12 hours Obtain carbon nanotubes.

[0061] (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;

[0062] (3) Add 2mol / L NaCO dropwise to the above solution 3 , adjust the pH to about 12;

[0063] (4) Raise the temperature to 80°C for 30 minutes;

[0064] (5)...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

PUM

No PUM Login to view more

Abstract

The invention discloses application of a metal-free hydrogenation catalyst in catalyzing hydrogenation reaction of nitrobenzene and derivatives thereof. The metal-free hydrogenation catalyst is nitrogen-doped carbon nanotubes prepared by an impregnation process by using melamine as a nitrogen source, or nitrogen-doped carbon nanotubes prepared by an in-situ synthesis process by using ammonia gas as a nitrogen source; and the catalyst is applied to hydrogenation reaction of nitrobenzene and derivatives thereof. The nitrogen-doped carbon nanotubes used as the nitrobenzene hydrogenation catalyst do not support any metal active component, and can achieve the goal of hydrogenation catalysis only by using the nitrogen doping modification process. The whole reaction process avoids the use of noble metals, thereby saving the cost and avoiding environment pollution; and meanwhile, the catalyst can be recycled. The catalyst has the advantages of simple preparation method, low production cost, favorable hydrogenation effect, controllable reaction and environment friendliness, can not cause secondary pollution to the environment, and can be widely used in 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 nitrobenzene and its derivatives. Background technique [0002] Aniline is an important organic chemical intermediate and solvent, which is widely used and has a large market demand. At present, the production process of aniline mainly adopts nitrobenzene iron powder reduction method, phenol ammoniation method and nitrobenzene catalytic hydrogenation method. Among them, the catalytic hydrogenation method of nitrobenzene has the characteristics of low reaction temperature and few by-products, accounting for about 85% of the total production capacity of aniline. [0003] At present, most of the liquid-phase hydrogenation reactions of nitrobenzene use noble metal catalysts. Although the noble metal catalysts have high activity, the cost is also high and it...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

Application Information

Patent Timeline
no application Login to view more
IPC IPC(8): C07C209/36C07C211/46C07C215/76C07C213/02C07C211/52C07C255/58C07C253/30B01J27/24B01J21/18
CPCY02P20/584C07C209/36B01J21/185B01J27/24C07C213/02C07C253/30C07C211/46C07C215/76C07C211/52C07C255/58
Inventor 郝芳张文斌刘平乐熊伟熊绍锋罗和安
Owner XIANGTAN UNIV
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products