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Heteroatom doped hollow carbon sphere material loaded precious metal nano particle and preparation thereof

A nanoparticle and heteroatom technology, applied in the field of fuel cell anode catalyst materials, can solve the problems of high price, limited reserves of precious metals, poisoning of intermediate products, etc., and achieve the effect of simple and clear preparation process and high practical value

Active Publication Date: 2016-10-12
SHANGHAI UNIVERSITY OF ELECTRIC POWER
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The electrocatalysts of direct alcohol fuel cells are mainly noble metals, but the reserves of noble metals in nature are limited and expensive, and they are easily poisoned by intermediate products.

Method used

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  • Heteroatom doped hollow carbon sphere material loaded precious metal nano particle and preparation thereof
  • Heteroatom doped hollow carbon sphere material loaded precious metal nano particle and preparation thereof
  • Heteroatom doped hollow carbon sphere material loaded precious metal nano particle and preparation thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] (1) Preparation of heteroatom-doped hollow carbon spheres

[0041] ① SiO 2 Preparation: Mix 12ml of ethanol, 5ml of water and 2ml of ammonia water at room temperature and stir evenly, add 1ml of ethyl orthosilicate, stir for 3-5h, centrifuge and clean with ethanol and deionized water, and dry overnight at 50-70°C.

[0042] ② SiO2 2 @Preparation of polyphosphazene: 0.2g SiO 2 Disperse in 200ml acetonitrile, add 0.4g hexachlorocyclotriphosphazene, ultrasonic 10min, add 0.4g 4,4-dihydroxydiphenol, ultrasonic 10min, add 4ml triethylamine, ultrasonic 2-6h, centrifuge, 50-70 °C dried overnight.

[0043] ③ SiO2 2 Preparation of @doped carbon: SiO 2 @Polyphosphazene at 800-1000°C N 2 Calcined under atmosphere for 2-5h.

[0044] ④ Preparation of doped hollow carbon: Etching 50-100mg of SiO with 5% HF 30ml 2 @Doped carbon spheres, ultrasonically etched for 8 hours, washed by centrifugation, and vacuum dried overnight at 50-70°C.

[0045] (2) Preparation of noble metal na...

Embodiment 2

[0054] A preparation method of a heteroatom-doped hollow carbon supported palladium nanoparticle material, specifically comprising the following steps:

[0055] (1) Preparation of heteroatom-doped hollow carbon spheres

[0056] ① SiO 2 Preparation: Mix 12ml of ethanol, 5ml of water and 2ml of ammonia water at room temperature and stir evenly, add 1ml of ethyl orthosilicate, stir for 3-5h, centrifuge and clean with ethanol and deionized water, and dry overnight at 50-70°C.

[0057] ② SiO2 2 @Preparation of polyphosphazene: 0.2g SiO 2 Disperse in 100ml ethanol and 100ml tetrahydrofuran solution, add 0.2g hexachlorocyclotriphosphazene, sonicate for 10min, add 0.4g 4,4-dihydroxydiphenol, sonicate for 10min, add 4ml triethylamine, sonicate for 4-6h, centrifuge , 50-70 ℃ dry overnight.

[0058] ③ SiO2 2 Preparation of @doped carbon: SiO 2 @Polyphosphazene at 800-1000°C N 2 Calcined under atmosphere for 2-5h.

[0059] ④ Preparation of doped hollow carbon: Etching 50-100mg of ...

Embodiment 3

[0063] A method for preparing heteroatom-doped hollow carbon sphere material loaded noble metal nanoparticles, comprising the following steps:

[0064] (1) Preparation of heteroatom-doped hollow carbon spheres

[0065] (1-1) SiO 2 @Preparation of polyphosphazene: Weigh 0.2g of silicon dioxide and disperse it in 200ml of acetonitrile, add 0.2g of hexachlorocyclotriphosphazene, ultrasonic for 10min, then add 0.16g of 4,4-dihydroxydiphenol, ultrasonic for 10min, add 4ml triethylamine, sonicate for 2h, centrifuge, and dry overnight at 50-70°C;

[0066] (1-2)SiO2 2 @Preparation of heteroatom-doped carbon: the prepared SiO 2 @polyphosphazene at 800°C N 2 Under the atmosphere, calcined for 5h;

[0067] (1-3) Preparation of heteroatom-doped hollow carbon spheres: etching SiO with 20wt% HF 2 @Heteroatom-doped carbon, ultrasonically etched for 3 hours, washed by centrifugation, and dried overnight at 50-70°C.

[0068] (2) Preparation of noble metal nanoparticles supported by hete...

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Abstract

The invention relates to a heteroatom doped hollow carbon sphere material loaded precious metal nano particle and preparation thereof. The preparation comprises the following steps that firstly, heteroatom doped hollow carbon spheres are prepared, wherein 1-1, silicon dioxide serves as a template, comonomer phosphonitrilic chloride trimer and 4,4-dyhydroxyl bi-phenol are added, a polymerization reaction is carried out, and polyphosphazene wrapping silicon dioxide is generated; 1-2, the polyphosphazene wrapping silicon dioxide is calcined, and heteroatom doped carbon spheres with silicon dioxide as cores are obtained; 1-3, ultrasonic etching continues to be carried out, and after washing and drying, the heteroatom doped hollow carbon spheres are obtained; secondly, the prepared heteroatom doped hollow carbon spheres are dispersed into water, a precious metal precursor and a complexing agent are added, pH is adjusted to be 8-14, a reducing agent is added, stirring is carried out for a reaction, and after drying, the target product is obtained. Compared with the prior art, the catalyst has good electrocatalytic activity and electrochemical stability, and the preparation process is simple.

Description

technical field [0001] The invention relates to the field of fuel cell anode catalyst materials, in particular to a heteroatom-doped hollow carbon sphere material loaded with noble metal nanoparticles and a preparation method thereof. Background technique [0002] Due to the depletion of global fossil energy resources and the aggravation of environmental pollution, it is urgent for people to find clean and efficient new environmentally friendly energy sources. Among them, fuel cells are used in various fields due to their high energy density and wide range of fuel sources. The key to the energy conversion efficiency of fuel cells is the catalyst. The electrocatalysts of direct alcohol fuel cells are dominated by noble metals, but the reserves of noble metals in nature are limited and expensive, and they are easily poisoned by intermediate products. Therefore, noble metals need to be compounded with carbon materials. Among them, hollow carbon materials have large specific su...

Claims

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Application Information

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IPC IPC(8): B82Y30/00H01M4/88H01M4/92
CPCB82Y30/00H01M4/88H01M4/926Y02E60/50
Inventor 徐群杰林艳吴桐刘其范金辰
Owner SHANGHAI UNIVERSITY OF ELECTRIC POWER
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