Preparation method of nitrogen-doped graphene aerogel supported non-precious metal oxygen reduction catalyst

A technology of nitrogen-doped graphene and non-precious metals, applied in the direction of physical/chemical process catalysts, chemical instruments and methods, chemical/physical processes, etc., can solve the low utilization rate of oxygen reduction active sites, unfavorable industrial production, and equipment requirements Advanced problems, easy to expand production, low production cost, simple preparation method

Inactive Publication Date: 2014-12-03
CENT SOUTH UNIV
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  • Abstract
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Problems solved by technology

[0004] Nitrogen-doped graphene-supported non-precious metal materials are used as oxygen reduction catalysts, which have good oxygen reduction catalytic performance. Chinese patents CN103599805A and CN103611555A mix graphene oxide solution, non-noble metal salt solution and nitrogen-containing organic small molecules, evaporate to dryness, and then The non-noble metal oxygen reduction catalyst supported by nitrogen-doped graphene was obtained by high-temperature heat treatment, which showed good oxygen reduction catalytic activity. However, the graphene layer has π-π interaction, which is easy to reunite during use. And positively charged non-noble metal ions can further promote the agglomeration of negatively charged graphene sheets, making the specific surface area of ​​the composite much smaller than the theoretical specific surface area of ​​graphene, resulting in low utilization of oxygen reduction active sites.
At present, the method to solve graphene aggregation is mainly to...

Method used

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  • Preparation method of nitrogen-doped graphene aerogel supported non-precious metal oxygen reduction catalyst
  • Preparation method of nitrogen-doped graphene aerogel supported non-precious metal oxygen reduction catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Weigh 0.62g melamine and disperse it in 20ml deionized water, add 1.2ml formaldehyde solution with a mass fraction of 37wt%, stir at 70°C for 0.5h to obtain a prepolymer, then add graphene oxide solution (100ml 1.0 mg / ml) and an aqueous solution containing 0.1g of ferrous sulfate, continuously stirred at 98°C for 3h to obtain a hydrogel, freeze-dried to obtain a nitrogen-doped graphene airgel loaded non-noble metal oxygen reduction catalyst precursor, and the above-mentioned nitrogen-doped graphene The airgel-loaded non-noble metal oxygen reduction catalyst precursor was placed in a porcelain boat, and under the protection of an inert gas, the temperature was raised to 800°C at a heating rate of 5°C / min and kept for 2 hours, and then naturally cooled to room temperature to obtain nitrogen-doped graphene gas condensation Gum-supported non-noble metal oxygen reduction catalysts.

[0027] Weigh 2.0 mg of the nitrogen-doped graphene airgel-supported non-noble metal oxygen r...

Embodiment 2

[0031] Weigh 0.4g of melamine and 0.4g of urea and disperse them in 20ml of deionized water, add 1.0ml of a glyoxal solution with a mass fraction of 40wt%, stir at 55°C for 2h to obtain a prepolymer, and then add a graphene oxide solution (50ml 1.0 mg / ml) and an aqueous solution containing 0.05 g cobalt sulfate, continuously stirred at 65 ° C for 24 h to obtain a hydrogel, freeze-dried to obtain a nitrogen-doped graphene airgel-loaded non-noble metal oxygen reduction catalyst precursor, the above nitrogen Doped graphene airgel loaded non-precious metal oxygen reduction catalyst precursor was placed in a ceramic boat, and under the protection of inert gas, the temperature was raised to 700°C at a heating rate of 1°C / min and kept for 1h, and then naturally cooled to room temperature to obtain nitrogen-doped Graphene airgel supported non-noble metal oxygen reduction catalyst.

Embodiment 3

[0033] Weigh 0.9g of dicyandiamide and disperse it in 20ml of deionized water, add 0.8ml of a glyoxal solution with a mass fraction of 40wt%, stir at 80°C for 0.5h to obtain a prepolymer, and then add a graphene oxide solution (200ml 1.0 mg / ml) and an aqueous solution containing 0.2g nickel nitrate, and continuously stirred at 85°C for 12h to obtain a hydrogel, which was supercritically dried with carbon dioxide to obtain a nitrogen-doped graphene airgel-loaded non-noble metal oxygen reduction catalyst precursor, which The above nitrogen-doped graphene airgel-loaded non-noble metal oxygen reduction catalyst precursor was placed in a porcelain boat, and under the protection of an inert gas, the temperature was raised to 1000°C at a heating rate of 10°C / min and kept for 4 hours, and naturally cooled to room temperature to obtain nitrogen Doped graphene airgel supported non-noble metal oxygen reduction catalyst.

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Abstract

The invention provides a preparation method of a nitrogen-doped graphene aerogel supported non-precious metal oxygen reduction catalyst. The method comprises the following steps: stirring a mixed solution of organic amine and aldehyde for 0.5-2 hours at the temperature of 50-90 DEG C, adding graphene oxide and a non-precious salt solution, stirring for 1-24 hours at the temperature of 60-99 DEG C to obtain organogel, performing freezing or supercritical drying, heating to 500-1000 DEG C under protection of inert gas, preserving heat for 1-6 hours, and naturally cooling to room temperature, thereby obtaining the nitrogen-doped graphene aerogel supported non-precious metal oxygen reduction catalyst. The preparation method of the nitrogen-doped graphene aerogel supported non-precious metal oxygen reduction catalyst is simple, the production can be easily expanded, the cost is low, the oxygen reduction catalysis activity is high, and the commercial popularization is facilitated.

Description

technical field [0001] The invention belongs to the field of graphene catalytic materials, in particular to the preparation and application of a nitrogen-doped graphene airgel-loaded non-noble metal oxygen reduction catalyst. Background technique [0002] Oxygen reduction reaction, as the positive electrode reaction of fuel cells and metal-air batteries, has always been a hot spot in electrochemical research. Oxygen has a slow reaction rate, so catalysts are needed. Traditional catalysts are mainly Pt-based noble metals, which have poor stability and high production costs, and are not suitable for commercial promotion. Therefore, it is particularly important to develop a cheap, efficient, stable, and large-scale production of non-noble metal catalysts to replace Pt-based noble metal catalysts. [0003] Graphene is a two-dimensional honeycomb carbon material with a thickness of one atomic layer. It has the characteristics of high specific surface area and high conductivity. ...

Claims

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Application Information

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IPC IPC(8): B01J27/24
Inventor 刘洪涛雷刚黄燕平
Owner CENT SOUTH UNIV
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