Preparation method for palladium/three-dimensional graphene composite microspheres

A graphene composite, graphene technology, applied in chemical instruments and methods, chemical/physical processes, physical/chemical process catalysts, etc., can solve the problem of being unsuitable for industrial large-scale production, complex preparation methods of palladium/three-dimensional graphene catalysts, etc. problem, to achieve the effect of novel and unique method, uniform particle size and simple operation

Inactive Publication Date: 2015-04-22
HEILONGJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The present invention aims to solve the technical problem that the current preparation methods of palladium / three-dimensional graphene catalysts are relatively complicated and not suitable for large-scale industrial production, and provide a preparation method of palladium / three-dimensional graphene composite microbeads

Method used

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  • Preparation method for palladium/three-dimensional graphene composite microspheres
  • Preparation method for palladium/three-dimensional graphene composite microspheres
  • Preparation method for palladium/three-dimensional graphene composite microspheres

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specific Embodiment approach 1

[0020] Specific embodiment one: present embodiment is a kind of preparation method of palladium / three-dimensional graphene composite microbead, is specifically carried out according to the following steps:

[0021] 1. Mix raw materials to form a solution: 5g of graphene oxide solution with a mass fraction of 1% to 1.5%, 0.25g of polyvinylpyrrolidone and 0.0714g of PdCl 2 Mix evenly to obtain a composite dispersed phase solution;

[0022] 2. Curing and molding: Take 10mL of the composite dispersed phase solution obtained in step 1 and pour it into a syringe, push the syringe with a syringe pump to make the composite dispersed phase solution fall into a circular container containing 50mL of simethicone oil, at a temperature of 60°C Insulate for 12h-24h under the conditions of ~70°C and 500rpm rotation speed to obtain composite microbeads; the material of the circular container is polypropylene;

[0023] 3. Calcination: Take the composite microbeads obtained in step 2 out of the...

specific Embodiment approach 2

[0028] Specific embodiment two: the difference between this embodiment and specific embodiment one is: in step one, 5g mass fraction is 1% graphene oxide solution, 0.25g polyvinylpyrrolidone and 0.0714gPdCl 2 Mix evenly to obtain a composite dispersed phase solution. Others are the same as in the first embodiment.

specific Embodiment approach 3

[0029] Specific embodiment three: the difference between this embodiment and one of specific embodiments one to two is: the preparation method of graphene oxide in step one is: take 1.2g of scaly graphite powder and add it into a glass three-necked bottle with a volume of 500mL , then add 50mL of concentrated sulfuric acid, put the glass three-necked bottle into an ice-water bath and stir for 30min at a stirring speed of 250r / min, then slowly add 10g of potassium permanganate and 1.5g of sodium nitrate, and stir at a stirring speed of 250r / min. Stir at 200r / min and ice-water bath for 2h, take the glass three-neck flask out of the ice-water bath and stir for 2h at room temperature and at a stirring speed of 250r / min, then in a water bath at 35°C and at a stirring speed of Stir at 250r / min for 24 hours, then add 10mL to 15mL of hydrogen peroxide solution with a mass fraction of 30% and 10mL of aqueous hydrochloric acid with a mass fraction of 36% to 38% to obtain a viscous soluti...

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Abstract

The invention relates to a preparation method for composite microspheres, in particular to a preparation method for palladium / three-dimensional graphene composite microspheres. The preparation method for the palladium / three-dimensional graphene composite microspheres solves the technical problems that existing preparation methods for the palladium / three-dimensional graphene composite microspheres are complicated and are not suitable for industrial large-scale production. The preparation method comprises the following steps that firstly, raw materials are mixed to prepare a solution; secondly, solidification and forming are conducted; thirdly, calcination is conducted. The preparation method for the palladium / three-dimensional graphene composite microspheres has the advantages that the method is novel and unique, operation is easy, the process is safe, reliable and environmentally friendly, the obtained palladium / three-dimensional graphene composite microspheres are controllable in size and uniform in particle size, the preparation method is one of the ideal preparation methods for the palladium / three-dimensional graphene composite microspheres, and the preparation method is suitable for industrial large-scale production.

Description

technical field [0001] The invention relates to a preparation method of composite microbeads. technical background [0002] Graphene is a two-dimensional structure with a thickness of one atomic layer. Since it was first exfoliated by Geim through mechanical exfoliation, graphene has been widely studied and applied in catalysis, energy conversion, storage and sensors due to its unique characteristics. Graphene has a large theoretical specific surface area, high electronic conductivity, good chemical stability and low production cost, and is used as an auxiliary material in catalytic reactions due to its strong adsorption capacity to the substrate due to its partially conjugated structure. Material. Some studies have shown that metal nanoparticles supported on graphene have superior catalytic activity and broader application prospects than those supported on carbon nanotubes in electrocatalysis and direct fuel cells. In recent years, many studies have pointed out that palla...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/44B01J35/08H01M4/92
CPCY02E60/50
Inventor 孙立国曹晓俭赵冬梅汪成张艳红
Owner HEILONGJIANG UNIV
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