Nitrogen-doped mesoporous graphene microspheres, and preparation method and application thereof

A mesoporous graphene, nitrogen-doped technology, applied in electrical components, circuits, battery electrodes, etc., can solve the problems of low stability, low life, high cost, etc., and achieve uniform pore size, low cost, and large pore volume. Effect

Active Publication Date: 2014-06-04
WENZHOU UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to overcome the high cost and low stability of existing fuel cell electrocatalysts, provide a novel nitrogen-doped mesoporous graphene microsphere and its preparation method, and apply it to th

Method used

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  • Nitrogen-doped mesoporous graphene microspheres, and preparation method and application thereof
  • Nitrogen-doped mesoporous graphene microspheres, and preparation method and application thereof
  • Nitrogen-doped mesoporous graphene microspheres, and preparation method and application thereof

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Experimental program
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Effect test

Embodiment 1

[0025] Embodiment 1 mesoporous graphene microsphere

[0026] Accurately weigh 0.2g of metal sodium block with a bright surface, pick it up with tweezers and place it in a 50ml stainless steel high-pressure reaction kettle, use a measuring cylinder to measure 40ml of hexachlorobutadiene, and slowly add it to the stainless steel reaction kettle filled with sodium block , Cover the lid of the reaction kettle, inject argon gas to 5MPa, make sure that it is tightened, and then use an electric heating jacket to raise the temperature to 240°C for 20h. After the reaction, cool down to room temperature naturally, open the reaction kettle, collect the black product in the kettle into an 8ml centrifuge tube with a straw, centrifuge at 8000r / min for 5 minutes, absorb the upper yellow liquid, and add absolute ethanol to the centrifuge tube Centrifuge, repeat 3 times, discard the supernatant and then add 50% ethanol aqueous solution to centrifuge, repeat 3 times, finally discard the superna...

Embodiment 2

[0027] Embodiment 2 mesoporous graphene microspheres

[0028] Accurately weigh 0.2g of metal sodium block with a bright surface, pick it up with tweezers and place it in a 50ml stainless steel high-pressure reaction kettle, measure 12ml of hexachlorobutadiene with a graduated cylinder, and slowly add it to the stainless steel reaction kettle filled with sodium block , Cover the lid of the reaction kettle, inject argon gas to 15MPa, make sure that it is tightened, and then use electric heating to raise the temperature to 200°C for 40 hours. After the reaction, cool down to room temperature naturally, open the reaction kettle, collect the black product in the kettle into an 8ml centrifuge tube with a straw, centrifuge at 8000r / min for 5 minutes, absorb the upper yellow liquid, and add absolute ethanol to the centrifuge tube Centrifuge, repeat 3 times, discard the supernatant and then add 50% ethanol aqueous solution to centrifuge, repeat 3 times, finally discard the supernatant ...

Embodiment 3

[0029] Embodiment 3 mesoporous graphene microspheres

[0030] Accurately weigh 0.1g of metal sodium block with a bright surface, pick it up with tweezers and place it in a 50ml stainless steel autoclave, use a graduated cylinder to measure 30ml of hexachlorobutadiene, and slowly add it to the stainless steel reaction kettle filled with sodium block , cover the lid of the reaction kettle, inject argon gas to 1MPa, make sure that it is tightened, and use electric heating to raise the temperature to 300°C for 10h. After the reaction, cool down to room temperature naturally, open the reaction kettle, collect the black product in the kettle into an 8ml centrifuge tube with a straw, centrifuge at 8000r / min for 5 minutes, absorb the upper yellow liquid, and add absolute ethanol to the centrifuge tube Centrifuge, repeat 3 times, discard the supernatant and then add 50% ethanol aqueous solution to centrifuge, repeat 3 times, finally discard the supernatant and add absolute ethanol to c...

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Abstract

The invention discloses nitrogen-doped mesoporous graphene microspheres, and a preparation method and an application thereof. The method comprises the steps of adding metal sodium into hexachlorobutadiene, carrying out a sealed reaction for 10-40 h at a temperature of 200-300 DEG C and under a pressure of 1-15 MPa, carrying out aftertreatment on a reaction product after the reaction is finished, thus obtaining mesoporous graphene microspheres; mixing the mesoporous graphene microspheres with urea or carrying out ammonia purge on the mesoporous graphene microspheres under the protection of an inert gas, then carrying out a sealed reaction for 0.5-4 h at a temperature of 700-1,200 DEG C; and after the reaction is finished, subjecting a reaction product to centrifugation and washing precipitate with water to obtain the nitrogen-doped mesoporous graphene microspheres. The specific surface area of the nitrogen-doped mesoporous graphene microspheres is 900-1,000 m<2>/g; pore volume is 0.1-1.8 cm<3>/g; and average aperture is 3.5-4.2 nm. The nitrogen-doped mesoporous graphene microspheres can be used as a platinum- and oxygen-free reduction catalyst which has high activity, low cost and long service life, for the field of fuel cells.

Description

(1) Technical field [0001] The invention relates to the preparation of nanomaterials and fuel cell electrode materials, in particular to a preparation method of nitrogen-doped mesoporous graphene microspheres, and the application of nitrogen-doped mesoporous graphene microspheres as cathode catalyst materials in oxygen reduction . (2) Background technology [0002] With the sharp increase in the consumption of fossil fuels (coal, oil, natural gas) and the depletion of energy resource reserves, as well as a series of environmental and pollution problems, it is urgent to find energy technologies that are environmentally friendly and sustainable. As a new type of energy conversion device, the proton exchange membrane fuel cell uses hydrogen and oxygen to react to generate water, and simultaneously releases heat and electricity. hotspot. However, the cathode oxygen reduction reaction of the proton exchange membrane fuel cell is slow and the overpotential is high. Even if plati...

Claims

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Application Information

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IPC IPC(8): B01J27/24B01J35/08H01M4/90
CPCY02E60/50
Inventor 王舜王健金辉乐
Owner WENZHOU UNIVERSITY
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