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Nickel-based core-shell structured nano catalysis material and preparation method and application thereof

A technology of nano-catalytic materials and core-shell structure, which is applied in the field of catalytic materials and its preparation, can solve the problems of low hydrogenation selectivity, difficulty in popularization and application, and high price, and achieve good dispersion, simple and rapid preparation method, and low manufacturing cost. low effect

Active Publication Date: 2016-05-11
HEBEI UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] One of the purposes of the present invention is to provide a nickel-based core-shell structure nano-catalytic material to solve the problem that the catalytic material in the existing hydrogenation reaction has either poor activity, low selectivity, or high price and is difficult to popularize and apply
[0005] The third object of the present invention is to provide the application of nickel-based core-shell structure nano-catalytic materials to solve the problem of low selectivity of catalytic hydrogenation in the prior art with unsaturated compounds as raw materials

Method used

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  • Nickel-based core-shell structured nano catalysis material and preparation method and application thereof
  • Nickel-based core-shell structured nano catalysis material and preparation method and application thereof
  • Nickel-based core-shell structured nano catalysis material and preparation method and application thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0038] (1) 1.7gNi(CH 3 COO) 2 4H 2 O was dissolved in 200mL of ethylene glycol, 2.24g of polyvinylpyrrolidone (PVP) was added, and stirred until the PVP was completely dissolved; then, under reflux, the solution was heated to 150°C, and 1.9g of NaBH was added at this temperature 4 , then the solution turned black, and continued heating and stirring for 2h, then stopped heating and stirring. After it is cooled, a small amount of acetone is added, centrifuged to obtain a black solid, washed with acetone, and dried at room temperature to obtain Ni nanoparticles;

[0039] (2) Take 0.4g of prepared Ni nanoparticles and add them to the mixed solution of ethanol (320mL) and water (80mL), ultrasonically disperse Ni for 30 minutes, then add 5.0mL ammonia solution (25wt%), and then slowly drop Add 1.0mL tetraethyl orthosilicate (TEOS), stir at room temperature for 5h, then use a magnet to separate, then wash with ethanol and water, and dry in an oven at 60°C for 6h to obtain NiSiO 2...

Embodiment 2

[0047] (1) 1.5gNi(CH 3 COO) 2 4H 2 O was dissolved in 200mL of ethanol, 2g of polyvinylpyrrolidone (PVP) was added, and stirred until the PVP was completely dissolved; then, under reflux, the solution was heated to 145°C, and 1.5g of NaBH was added at this temperature 4 , then the solution turns black, continue heating and stirring for 2h, then stop heating and stirring; after it cools down, add a small amount of acetone, centrifuge to obtain a black solid, wash with acetone, and dry at room temperature to obtain Ni nanoparticles;

[0048] (2) Add 0.4g of the prepared Ni nanoparticles into a mixed solution of ethanol (320mL) and water (80mL), ultrasonically disperse Ni for 30 minutes, then add 4.0mL of ammonia solution (30wt%), and then slowly drop Add 0.5mL tetraethyl orthosilicate (TEOS), stir at room temperature for 4.5h, then use a magnet to separate, then wash with ethanol and water, and dry in an oven at 60°C for 6h to obtain NiSiO 2 ;

[0049] (3) Aluminum isopropox...

Embodiment 3

[0055] (1) 2gNi(CH 3 COO) 2 4H 2 O was dissolved in 200mL of 1,5-pentanediol, 2.5g of polyvinylpyrrolidone (PVP) was added, and stirred until the PVP was completely dissolved; then, under reflux, the solution was heated to 155°C, and 2.5g of NaBH was added at this temperature 4 , then the solution turns black, continue heating and stirring for 2h, then stop heating and stirring; after it cools down, add a small amount of acetone, centrifuge to obtain a black solid, wash with acetone, and dry at room temperature to obtain Ni nanoparticles;

[0056] (2) Add 0.4g of the prepared Ni nanoparticles into a mixed solution of ethanol (320mL) and water (80mL), ultrasonically disperse Ni for 30 minutes, then add 6.0mL of ammonia solution (20wt%), and then slowly drop Add 1.5mL tetraethyl orthosilicate (TEOS), stir at room temperature for 5.5h, then use a magnet to separate, then wash with ethanol and water, and dry in an oven at 60°C for 6h to obtain NiSiO2;

[0057] (3) Dissolve alum...

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Abstract

The invention provides a nickel-based core-shell structured nano catalysis material which has a core-shell structure and material composition of Ni@mSiO2@LDO or Ni@mSiO2@LDH. A preparation method of the nickel-based core-shell structured nano catalysis material comprises the steps of: firstly preparing Ni nano particles, coating the surface of a Ni core with a layer of SiO2, coating the surface of Ni@NiO2 with an LDH shell layer, etching by a NaOH solution, carrying out high-temperature calcination, reducing in H2 atmosphere to obtain the black Ni@mSiO2@LDO core-shell structured catalysis material, and carrying out hydration reaction on the Ni@mSiO2@LDO core-shell structured catalysis material in deionized water under the protection of inert atmosphere to obtain the black Ni@mSiO2@LDH core-shell structured catalysis material. The nickel-based core-shell structured nano catalysis material has good activity and selectivity, and can be used for generating a target compound at high selectivity through catalytic hydrogenation by taking an unsaturated compound as a raw material; and the material is uniform in particle, good in dispersity, good in recycling stability, simple in preparation method, and low in production cost and has broad application prospects in the catalysis field.

Description

technical field [0001] The invention relates to a catalytic material and its preparation method and application, in particular to a nickel-based core-shell structure nano catalytic material, its preparation method and its application in selective hydrogenation reaction. Background technique [0002] Primary amines are widely used in the fields of medicine, pesticides and plastics; imines can be used in the synthesis of dyes, fragrances, fungicides, drugs and pesticides. At present, the methods for synthesizing amines mainly include reductive amination of carbonyl compounds, hydrogenation amination of alkenes or alkynes, and hydrogenation reaction of nitriles; and the oxidation coupling of alcohols and amines. Among them, in the hydrogenation reaction of nitriles, condensation deamination reaction can occur between imine intermediates and primary amines to form imines, and the raw materials of nitrile compounds are cheaper, and the hydrogenation reaction of nitriles is more ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/755C07C209/48C07C211/27
CPCB01J23/002B01J23/78B01J2523/00C07C209/48B01J2523/22B01J2523/31B01J2523/41B01J2523/847C07C211/27
Inventor 白国义曹迎迎牛立博
Owner HEBEI UNIVERSITY
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