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Nonmetal oxygen reduction catalyst and preparation method thereof

A catalyst, non-metal technology, applied in the field of oxygen reduction catalyst without metal element and its preparation, can solve the problems of complicated process conditions, carbon monoxide poisoning, catalyst oxidation and the like, achieve simple and safe preparation process, improve catalytic activity and low cost Effect

Inactive Publication Date: 2013-12-04
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

For example, element-doped graphene or carbon nanotubes have high catalytic activity (Angew.Chem.Int.Ed.2012, 51, 4209; Angew.Chem.Int.Ed.2011, 50, 11756.), but this In order to obtain a better doping effect, the process conditions of the catalyst are cumbersome and the cost is high
In addition, high-performance oxygen reduction catalysts can also be obtained by pyrolyzing suitable carbon sources, nitrogen sources, and transition metals (Co, Fe) (Adv. Funct. Mater. 2012, 22, 3500.), however, due to the Existence, easy to cause problems such as catalyst oxidation and carbon monoxide poisoning

Method used

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  • Nonmetal oxygen reduction catalyst and preparation method thereof
  • Nonmetal oxygen reduction catalyst and preparation method thereof
  • Nonmetal oxygen reduction catalyst and preparation method thereof

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specific Embodiment approach

[0020] The following are examples of the present invention, providing detailed implementation and specific operation process, the purpose of which is only to better understand the content of the present invention. The scope of protection of the invention is therefore not restricted by the examples given.

[0021] The test method of the catalyst performance that the present invention uses is as follows:

[0022] Mix 2 mg of the prepared nitrogen-phosphorous co-doped porous carbon material with 1 mL of 5wt% Nafion emulsion and ethanol (volume ratio 1:9) and sonicate for 30 minutes to obtain a dispersion; take 10 μL of the dispersion and apply it on a rotating circle After drying on the disc electrode at room temperature, a thin film electrode was obtained. Using a three-electrode system with Ag / AgCl electrode as the reference electrode and Pt wire as the counter electrode, in oxygen-saturated 0.1mol / L KOH, 0.1mol / L PBS, 0.5mol / L H 2 SO 4 Cyclic voltammetry and linear sweep vo...

Embodiment 1

[0024] The aqueous solution of polystyrene microspheres with a mass fraction of 10% and a particle size of 160 nm and dimethyl sulfoxide solution with 10% polyvinyl alcohol were uniformly mixed at a volume ratio of 1:1 at 70°C, and then the obtained The precursor solution was frozen at -20°C for 4 hours and thawed at 25°C for 1 hour to obtain a composite hydrogel of polyvinyl alcohol and polystyrene. 10 g of composite hydrogels were chemically cross-linked with 50 mL of 0.75% glutaraldehyde aqueous solution for 6 hours. The chemically crosslinked composite hydrogel was immersed in 10 mL of aqueous solution of cyanamide and phosphoric acid (the mass ratio of phosphoric acid to cyanamide was 0.2:1) for 12 hours to reach adsorption swelling equilibrium. Then dry at 80°C for 24 hours. The soaked and dried solid was pyrolyzed at 900° C. in an inert atmosphere and kept for 3 hours. Then naturally cooled to room temperature to obtain a hierarchically porous nitrogen-phosphorus co-d...

Embodiment 2

[0027] The aqueous solution of polystyrene microspheres with a mass fraction of 10% and a particle size of 160nm and the dimethyl sulfoxide solution of 10% polyvinyl alcohol were uniformly mixed at a volume ratio of 1:1 at 70°C, and then the obtained The precursor solution was frozen at -20°C for 4 hours and thawed at 25°C for 1 hour to obtain a composite hydrogel of polyvinyl alcohol and polystyrene. 10 g of composite hydrogels were chemically cross-linked with 50 mL of 0.75% glutaraldehyde aqueous solution for 6 hours. The chemically crosslinked composite hydrogel was soaked in 10 mL of 50% cyanamide aqueous solution for 12 hours to reach adsorption swelling equilibrium. Then dry at 80°C for 24 hours. The soaked and dried solid was pyrolyzed at 900° C. in an inert atmosphere and kept for 3 hours. Then cooled naturally to room temperature to obtain hierarchically porous nitrogen-doped carbon materials.

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Abstract

The invention discloses a nonmetal oxygen reduction catalyst and a preparation method thereof. The nonmetal oxygen reduction catalyst is of a three-dimensional grading porous structure. Main components of the nonmetal oxygen reduction catalyst are carbon, nitrogen and phosphorus. Nitrogen and phosphorus are dopped in carbon. The comparison content of nitrogen and phosphorus is 0-10 at%. The comparison content of phosphorus and carbon is 0-8 at%. The content of nitrogen and the content of phosphorus can not be zero at the same time. Solution of polystyrene microspheres and polyvinyl alcohol is frozen in low temperature, and then is unfrozen at room temperature, so that composite hydrogel of polyvinyl alcohol and polystyrene is prepared. The composite hydrogel is used as a template. Front drive body solution with mixed elements is filled into clearance of the hydrogel, and three-dimensional grading porous element-dopped carbon materials are manufactured through high-temperature calcining. According to the preparation method, raw materials are common and can be obtained easily, cost is low, and the preparation process is simple and safe. Obtained materials have good oxygen reduction catalytic activity in acid, neutralized and alkaline electrolyte and is approximate to the reaction process of four electrons.

Description

technical field [0001] The invention relates to the technical field of fuel cells, in particular to a metal element-free oxygen reduction catalyst for fuel cells and a preparation method thereof. Background technique [0002] A fuel cell is an energy conversion device that can convert chemical energy into electrical energy through redox reactions at the anode and cathode. It has the characteristics of low operating temperature, high energy efficiency, and no electrolyte corrosion. a research hotspot. However, so far, fuel cells have not been widely commercially produced, and one of the important constraints is the problem of its cathode catalyst. Platinum-based noble metals are currently mainly used as this type of catalyst, but the cost of this type of catalyst is too high, the source is limited, and there are shortcomings such as intolerance to carbon monoxide and methanol poisoning (Nature2001,414,345; Science2007,315,493; J.Am.Chem.Soc .2009, 131, 15330.). Therefore, ...

Claims

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Application Information

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IPC IPC(8): B01J27/24B01J35/10H01M4/90
CPCY02E60/50
Inventor 朱以华江宏亮杨晓玲赵鹏冯茜
Owner EAST CHINA UNIV OF SCI & TECH
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