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Nitrogen-doped carbon material composite magnesium oxide loaded nickel catalyst and preparation method and application thereof

A nitrogen-doped carbon and catalyst technology, applied in physical/chemical process catalysts, organic chemical methods, chemical instruments and methods, etc., can solve problems such as high consumption, difficult separation of primary amine and imine products, unfavorable production, etc., to achieve High conversion rate and selectivity, good industrial application prospects, and easy operation

Pending Publication Date: 2022-03-01
SOUTH CENTRAL UNIVERSITY FOR NATIONALITIES
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The oxidative synthesis of imines using nitro compounds as starting materials requires two steps, that is, the hydrogenation of nitro compounds into primary amines in the first step, and the oxidation of primary amines into imines in the second step. However, the catalysts disclosed in the prior art Most of the methods for reducing nitro compounds use molecular oxygen, the selectivity is not high, and there is the problem of difficult separation of primary amines and imine products, and usually requires high pressure and temperature, high requirements for reaction equipment, and potential safety hazards Larger, not conducive to actual production
[0003] Therefore, the development of a method to obtain the above-mentioned imines by catalyzing the reduction of nitro compounds and the coupling of carbonyl compounds can fundamentally solve the problem of high pollution and high consumption in previous chemical synthesis processes, and provide important technical support for chemical production

Method used

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  • Nitrogen-doped carbon material composite magnesium oxide loaded nickel catalyst and preparation method and application thereof
  • Nitrogen-doped carbon material composite magnesium oxide loaded nickel catalyst and preparation method and application thereof
  • Nitrogen-doped carbon material composite magnesium oxide loaded nickel catalyst and preparation method and application thereof

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Effect test

Embodiment 1

[0038] A kind of preparation method of nitrogen-doped carbon material composite magnesia supported nickel (Ni / CN-MgO) catalyst, its steps are as follows:

[0039] Add nickel nitrate, magnesium nitrate, chitosan and dicyandiamide with a mass ratio of 0.2:0.6:0.2:0.6 into 10mL of water and stir to dissolve fully, wherein the mass of nickel nitrate is 0.2g, and then add 0.3mL of glacial acetic acid to it , and stirred for 20 minutes. After thorough stirring, the resulting material was dried at 100 °C to obtain a pale green precursor. The obtained precursor was pyrolyzed in nitrogen at 500 °C for 2 hours to obtain a Ni / CN-MgO catalyst. Abbreviated as Ni / CN-MgO-500. The pyrolysis process is as follows: heating to 500°C at 2°C / min in a nitrogen-filled tube furnace, and then holding the temperature for 120min.

Embodiment 2

[0041] A kind of preparation method of nitrogen-doped carbon material composite magnesia supported nickel (Ni / CN-MgO) catalyst, its steps are as follows:

[0042] Add nickel nitrate, magnesium nitrate, chitosan and dicyandiamide with a mass ratio of 0.2:0.6:0.2:0.6 into 10mL of water and stir to dissolve fully, wherein the mass of nickel nitrate is 0.2g, and then add 0.3mL of glacial acetic acid to it , and stirred for 20 minutes. After thorough stirring, the resulting material was dried at 100 °C to obtain a pale green precursor. The obtained precursor was pyrolyzed in nitrogen at 600 °C for 2 hours to obtain a Ni / CN-MgO catalyst. Abbreviated as Ni / CN-MgO-600. The pyrolysis process is as follows: heating to 600°C at 2°C / min in a nitrogen-filled tube furnace, and holding for 120min. The X-ray diffraction pattern of the catalyst is shown in figure 1 , it can be seen that the characteristic peaks of magnesium oxide appear at 2θ=36.8°, 42.8°, 62.2°, 74.5° and 78.4°, and the c...

Embodiment 3

[0044] A kind of preparation method of nitrogen-doped carbon material composite magnesia supported nickel (Ni / CN-MgO) catalyst, its steps are as follows:

[0045]Add nickel nitrate, magnesium nitrate, chitosan and dicyandiamide with a mass ratio of 0.2:0.6:0.2:0.6 into 10mL of water and stir to dissolve fully, wherein the mass of nickel nitrate is 0.2g, and then add 0.3mL of glacial acetic acid to it , and stirred for 20 minutes. After thorough stirring, the resulting material was dried at 100 °C to obtain a pale green precursor. The obtained precursor was pyrolyzed in nitrogen at 700 °C for 2 hours to obtain a Ni / CN-MgO-700 catalyst. Abbreviated as Ni / CN-MgO-700. The pyrolysis process is as follows: heating at 2°C / min to 700°C in a tube furnace with nitrogen gas, and holding for 120min.

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Abstract

The invention belongs to the technical field of catalysts, and particularly relates to a nitrogen-doped carbon material composite magnesium oxide loaded nickel catalyst, a preparation method of the nitrogen-doped carbon material composite magnesium oxide loaded nickel catalyst and application of the nitrogen-doped carbon material composite magnesium oxide loaded nickel catalyst to preparation of an imine compound by catalyzing reduction of a nitro compound and coupling of a carbonyl compound. The catalyst is obtained by performing high-temperature pyrolysis on a precursor prepared by a one-pot method in nitrogen, and can be used for catalyzing nitro compound reduction and carbonyl compound coupling to prepare an imine compound under mild conditions. The catalyst disclosed by the invention is very simple in preparation method and relatively good in stability, can be recycled for more than 10 times, and has a good industrial application prospect in preparation of an imine compound by catalyzing reduction of a nitro compound and coupling of a carbonyl compound.

Description

technical field [0001] The invention belongs to the technical field of catalysts, and in particular relates to a nitrogen-doped carbon material composite magnesium oxide-supported nickel catalyst and a preparation method thereof, as well as an application in catalyzing reduction of nitro compounds and coupling of carbonyl compounds to prepare imine compounds. Background technique [0002] The reductive coupling of nitro species is of great significance to many fields of chemical industry, such as chemical industry and pharmaceuticals. Imine derivatives are widely used in the production of heterocyclic compounds and pharmaceutical compounds. In recent decades, several new catalytic methods have been established for the synthesis of imines, such as amination of carbonyl compounds and dehydrogenation of amines. Currently, the oxidation of primary amines has become a research hotspot for the synthesis of imines, and it can even be achieved by using metal-free nitrogen-doped car...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/24C07C249/02C07C251/24C07C253/30C07C255/61C07B43/00
CPCB01J27/24C07C249/02C07C253/30C07B43/00C07C251/24C07C255/61
Inventor 张泽会王岩鑫刘冰李波
Owner SOUTH CENTRAL UNIVERSITY FOR NATIONALITIES