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A kind of preparation method of nickel-based catalyst and its application to the method for preparing imine compounds from nitriles and amine compounds

An amine compound and catalyst catalyzing nitrile technology, which is applied in the preparation of imino compounds, chemical instruments and methods, catalysts for physical/chemical processes, etc. Good performance, good industrial application prospects, high conversion rate

Active Publication Date: 2022-03-29
SOUTH CENTRAL UNIVERSITY FOR NATIONALITIES
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, azo compounds themselves are expensive, unstable and difficult to preserve. In the prior art, there is no better way to solve such problems. Therefore, to develop a method for hydrogenation of nitrile compounds and amine compounds under mild conditions An efficient method for the selective synthesis of unsymmetrical imines by cross-coupling is particularly challenging and practical

Method used

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  • A kind of preparation method of nickel-based catalyst and its application to the method for preparing imine compounds from nitriles and amine compounds
  • A kind of preparation method of nickel-based catalyst and its application to the method for preparing imine compounds from nitriles and amine compounds
  • A kind of preparation method of nickel-based catalyst and its application to the method for preparing imine compounds from nitriles and amine compounds

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] A kind of mesoporous aluminum oxide supported nickel (Ni / Meso-Al 2 o 3 -450) the preparation method of catalyst, its step is as follows:

[0049] (1) Dissolve Pluronic P123 (2.1g) in ethanol (20mL), and dissolve it by magnetic stirring at room temperature to obtain solution A; 67wt.% concentrated HNO 3 (3.2 mL) and aluminum isopropoxide (4.08 g) were dissolved in ethanol (20 mL) to prepare solution B; solution B was then slowly added to solution A under vigorous stirring to obtain a mixture solution.

[0050] (2) Nickel nitrate hexahydrate {Ni(NO 3 ) 2 ·6H 2 After O} (0.4g) was dissolved in ethanol (5mL), it was added dropwise to the above mixture solution under stirring, and continued to stir at room temperature for 24h after the drop; then the mixture was dried in an oven at 70°C to obtain green gel;

[0051] (3) Grind the green gel obtained in step (2) into powder, then put the powder into a muffle furnace, heat up to 500°C at a rate of 5°C / min in air, and then...

Embodiment 2-4

[0055] A kind of mesoporous aluminum oxide supported nickel (Ni / Meso-Al 2 o 3 -550, 600, 650) the preparation method of catalyst, its step is as follows:

[0056] On the basis of Example 1, only the target hydrogen calcination temperature in step (4) was changed to 550°C, 600°C, and 650°C respectively, and the rest of the steps and operations were the same as in Example 1. The prepared catalysts were labeled as Ni / Meso-Al 2 o 3 -550, Ni / Meso-Al 2 o 3 -600, Ni / Meso-Al 2 o 3 -650.

Embodiment 5

[0058] The preparation method of a kind of mesoporous aluminum oxide supported nickel oxide catalyst used as contrast, its steps are as follows:

[0059] On the basis of embodiment 1, only carry out step (1)-(3), do not carry out step (4), thereby obtain: Catalyst NiO / Meso-Al 2 o 3 .

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Abstract

The invention belongs to the technical field of catalyst preparation and application, and specifically discloses a method for preparing a nickel-based catalyst and a method for applying it to nitrile and amine compounds to prepare imine compounds. The nickel-based catalyst is prepared by co-precipitation The nickel-aluminum double hydroxide precursor is calcined at high temperature in the air, and further prepared by reduction under high-temperature hydrogen. The catalyst uses nickel as the active site and mesoporous aluminum oxide as the carrier. The catalyst can be used for catalysis under mild conditions. After reduction, nitrile compounds are cross-coupled with amine compounds to synthesize important organic synthesis intermediates—imine compounds. The preparation method of the catalyst in the invention is simple, has good catalytic effect in the cross-coupling reaction with amine compounds after catalyzing the reduction of nitrile compounds, the catalyst can be recycled more than 10 times, has good stability, and has excellent industrial application prospects.

Description

technical field [0001] The invention relates to the technical field of catalyst preparation and application, in particular to a mesoporous aluminum oxide-supported nickel (Ni / Meso-Al 2 o 3 ) catalyst preparation method and its application in the selective cross-coupling of nitriles and amines to prepare imines. Background technique [0002] Imine compounds are a class of organic compounds with carbon-nitrogen double bonds in the molecule, and the general formula is R 2 C=NR', where R and R' can be hydrocarbon groups or hydrogen; imine compounds widely exist in natural products, and can be used as intermediates to participate in rearrangement reactions in sugar chemistry, such as: Amadori rearrangement reactions, and are widely used In agrochemicals, pharmaceuticals, dyes, pigments and polymers. The conventional preparation method of imine compounds is the catalytic condensation of amines and aldehydes in the presence of acid catalysts, but since aldehydes are prone to sel...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/755C07C249/02C07C251/24C07D213/53
CPCB01J23/755C07C249/02C07D213/53C07C251/24
Inventor 张泽会袁紫亮周鹏刘冰
Owner SOUTH CENTRAL UNIVERSITY FOR NATIONALITIES
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