Graphene loaded high-dispersion nano Ni catalyst as well as preparation method and application thereof

A catalyst and high-dispersion technology, which is applied in the preparation of carbon-based compounds, chemical instruments and methods, and the preparation of organic compounds. It can solve the problems of poor particle dispersion, affecting activity, and reducing the number of active centers, so as to improve structural stability. and chemical stability, good catalytic hydrogenation performance

Inactive Publication Date: 2013-09-18
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, LDHs nanoparticles are easy to agglomerate. During the heating and calcination process, the LDHs laminates gradually collapse and the particles sinter and agglomerate, which will lead to poor dispersion of LDHs or particles after calcination, a decrease in specific surface area, and a decrease in the number of active centers, thereby affecting its activity.

Method used

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  • Graphene loaded high-dispersion nano Ni catalyst as well as preparation method and application thereof
  • Graphene loaded high-dispersion nano Ni catalyst as well as preparation method and application thereof
  • Graphene loaded high-dispersion nano Ni catalyst as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Graphite and concentrated sulfuric acid, sodium nitrate and potassium permanganate are fully mixed in the ratio of 1: 0.5: 23: 3 by mass ratio under ice bath conditions and then warmed up to 35 ° C; by graphite: the mass ratio of deionized water is Add deionized water at a ratio of 1:50, heat up to 98°C and react for 0.5 hours; add deionized water and 30% hydrogen peroxide sequentially at a ratio of graphite: deionized water: 30% hydrogen peroxide mass ratio of 1:100:10; centrifugal separation , followed by dilute hydrochloric acid and deionized water to wash the filter cake to no SO 4 2- And it is neutral, then the product is dried at 70°C to obtain graphite oxide;

[0024] Disperse the above-mentioned graphite oxide in deionized water, prepare a dispersion liquid with a concentration of 3 mg / mL, ultrasonicate for 3 hours, let it stand for 12 hours, and then centrifuge at 3900rmp for 15 minutes, and the obtained supernatant is a graphene oxide solution;

[0025] Prep...

Embodiment 2

[0029] Graphite and concentrated sulfuric acid, sodium nitrate and potassium permanganate are fully mixed in the ratio of 1: 0.5: 30: 5 by mass ratio and then heated up to 40 ° C under ice bath conditions for 1.5 hours; by graphite: deionized water mass ratio is Add deionized water at a ratio of 1:95, heat up to 90°C and react for 6 hours; add deionized water and 30% hydrogen peroxide sequentially at a ratio of graphite: deionized water: 30% hydrogen peroxide mass ratio of 1:130:11; centrifugal separation , followed by dilute hydrochloric acid and deionized water to wash the filter cake to no SO 4 2- And it is neutral, and it is dried at 70°C to obtain graphite oxide;

[0030] Disperse graphite oxide in deionized water, prepare a dispersion with a concentration of 2 mg / mL, ultrasonicate for 2 hours, let it stand for 12 hours, and then centrifuge at 3500rmp for 10 minutes, and the obtained supernatant is graphene oxide solution;

[0031] Prepare the mixed salt solution of nic...

Embodiment 3

[0035] Graphite and concentrated sulfuric acid, sodium nitrate and potassium permanganate are fully mixed in the ratio of 1:1:15:2 by mass ratio and heated up to 25° C. after 0.5 hours under ice-bath conditions; by graphite: the mass ratio of deionized water is Add deionized water at a ratio of 1:40, heat up to 100°C and react for 1.5 hours; add deionized water and 30% hydrogen peroxide sequentially at a ratio of graphite: deionized water: 30% hydrogen peroxide mass ratio of 1:90:5; centrifugal separation , followed by dilute hydrochloric acid and deionized water to wash the filter cake to no SO 4 2- And it is neutral, then the product is dried at 60°C to obtain graphite oxide;

[0036] Disperse graphite oxide in deionized water, prepare a dispersion with a concentration of 5 mg / mL, ultrasonicate for 4 hours, let it stand for 24 hours, and then centrifuge at 3900rmp for 15 minutes, and the obtained supernatant is graphene oxide solution;

[0037] Prepare the mixed salt solut...

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Abstract

The invention provides a graphene loaded high-dispersion nano Ni catalyst as well as a preparation method and application thereof. The catalyst is obtained by loading high-dispersion Ni nano-metal on the surface of graphene, and doping less amorphous Al2O3, wherein the mass percent content of graphene is 40-67%, the mass percent content of Ni is 10-40%, the mass percent content of amorphous Al2O3 is 2-8%, the size distribution of Ni particles is 8-13nm, and the specific area of the catalyst is 155-200 m<2>/g. The preparation method comprises the following steps of: preparing a graphene/lamellar bimetal hydroxide composite material in one step through the hydroxide precipitation and reduction effect, and then preparing the graphene loaded high-dispersion metal Ni nano catalyst through an in-situ self-reduction method by using the reducibility of graphene. The catalyst is used for selectively hydrogenating the cinnamyl aldehyde to synthesize the benzenepropanal, and the conversion rate and the benzenepropanal selectivity are respectively 86-100% and 88-96%.

Description

technical field [0001] The invention relates to the technical field of catalyst preparation, in particular to a preparation method of a highly dispersed and supported nano-Ni catalyst. The catalyst is used for the selective catalytic hydrogenation of cinnamaldehyde. technical background [0002] Phenylpropionaldehyde is widely used in the preparation of various floral flavors, and also has important applications in the pharmaceutical industry. Phenylpropionaldehyde is usually produced by catalytic hydrogenation of cinnamaldehyde. Cinnamaldehyde is a typical α, β-unsaturated aldehyde, and the C=O, C=C and benzene rings in its molecular structure form a large conjugated system, so one or more easily occur during the catalytic hydrogenation of cinnamaldehyde. Catalytic hydrogenation of unsaturated groups. At the same time, due to the steric hindrance of the benzene ring, the C=O bond is easily reduced, so even palladium-based catalysts with excellent hydrogenation activity a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/755C07C47/228C07C45/62
Inventor 李峰马倩范国利
Owner BEIJING UNIV OF CHEM TECH
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