N-doped microporous carbon sphere ORR catalytic material and preparation method and application thereof

A catalytic material and microporous carbon technology, applied in the field of electrocatalysis, can solve problems such as unfavorable large-scale commercial preparation and application, high experimental conditions, and inability to meet requirements, etc., to promote the adsorption of oxygen molecules and further catalytic reactions and equipment requirements. Not high, the effect of improving structural stability

Active Publication Date: 2019-07-23
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

These methods are relatively complicated, costly, and require high experimental conditions, which are not conducive to large-scale commercial preparation and application, and still cannot meet the requirements of fuel cells and metal-air batteries for ORR catalysts.

Method used

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  • N-doped microporous carbon sphere ORR catalytic material and preparation method and application thereof
  • N-doped microporous carbon sphere ORR catalytic material and preparation method and application thereof
  • N-doped microporous carbon sphere ORR catalytic material and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0052] First, add 1.36g of zinc chloride into 5mL of formaldehyde (0.03mol) solution, and stir for 0.5h under ice-bath conditions to completely dissolve the zinc salt to form a clear high-salt solution. 1 mL of pyrrole monomer (0.015 mol) was added to the above solution, and after stirring for 0.5 h at 0-5° C., a uniform yellow oily liquid was formed. Transferred to the environment of 30° C. and allowed to stand for reaction for 12 hours, forming a black pyrrole zinc gel solid. Then dry in an oven at 105 °C for 24 h to evaporate water, crush the precursor into powder, place it in a porcelain boat, and then carry out high-temperature pyrolysis in a tube furnace filled with argon atmosphere, with a heating rate of 3 °C / min, controlled The temperature was kept at 900°C for 2h. The sample obtained by the above steps was named N-CS-1. The N doping content is 2.94%; the relative content of pyridine nitrogen is 36.8%

[0053] The micropore porosity is 87.7%, and the specific surfa...

Embodiment 2

[0056] First add 3.4g of zinc chloride into 5mL of formaldehyde (0.03mol) solution, and stir for 0.5h under ice bath conditions to completely dissolve the zinc salt to form a clear high-salt solution. 1 mL of pyrrole monomer (0.015 mol) was added to the above solution, and after stirring for 0.5 h at 0-5° C., a uniform yellow oily liquid was formed. Transferred to the environment of 30° C. and allowed to stand for 6 hours to react, forming a black pyrrole zinc gel solid. Then dry in an oven at 105 °C for 24 h to evaporate water, crush the precursor into powder, place it in a porcelain boat, and then carry out high-temperature pyrolysis in a tube furnace filled with argon atmosphere, with a heating rate of 3 °C / min, controlled The temperature was kept at 900°C for 2h. The sample obtained by the above steps was named N-CS-2. N doping content is 2.19%; relative pyridine nitrogen content is 51.5%

[0057] The micropore porosity is 89.7%, and the specific surface area is 1689m ...

Embodiment 3

[0060] First add 2g of zinc chloride to 10mL of formaldehyde (0.08mol) solution, and stir for 0.5h under ice bath conditions to completely dissolve the zinc salt to form a clear high-salt solution. 1.4 mL of pyrrole monomer (0.02 mol) was added to the above solution, and after stirring for 0.5 h at 0-5° C., a uniform yellow oily liquid was formed. Transferred to the environment of 30° C. and allowed to stand for reaction for 12 hours, forming a black pyrrole zinc gel solid. Then dry in an oven at 105 °C for 24 h to evaporate water, crush the precursor into powder, place it in a porcelain boat, and then perform high-temperature pyrolysis in a tube furnace filled with argon atmosphere, with a heating rate of 2 °C / min, controlled The temperature is kept at 1100°C for 2h. The sample obtained by the above steps is named N-CS-3

[0061] The obtained sample was used as the cathode material of an aluminum-air battery, and the electrochemical performance test was the same as in Examp...

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Abstract

The invention belongs to the field of material preparation and particularly discloses a preparation method of an N-doped microporous carbon sphere ORR catalytic material. The preparation method comprises the following steps: (1) reacting a raw material solution containing pyrrole, formaldehyde and a structure regulator to obtain gel, wherein the structure regulator is water-soluble salt of zinc, and the concentration of Zn<2+> in the raw material solution is 1 to 5 mol/L; and (2), dehydrating the gel and then pyrolyzing the gel at a temperature not lower than 700 DEG C, so as to obtain the N-doped microporous carbon sphere ORR catalytic material. The invention also discloses the material prepared by the preparation method an application of the material in air batteries. The method disclosed by the invention can be used to prepare the ORR catalytic material with uniform spherical morphology, rich microporous structure and rich pyridine nitrogen-doped morphology, and the material has better ORR catalytic performance and anti-catalytic poisoning effect.

Description

technical field [0001] The invention belongs to the technical field of electrocatalysis, and in particular relates to an N-doped microporous carbon sphere (N-CS) ORR catalyst and a preparation method and application thereof. Background technique [0002] With the continuous consumption of fossil energy, the continuous increase of energy demand and the enhancement of environmental protection awareness, all countries in the world have turned their attention to new energy sources, and the development of a low-cost, high-performance energy conversion and storage device has become the key. Rechargeable metal-air batteries have attracted widespread attention due to their simple preparation, low cost, excellent safety performance and environmental friendliness. In the field of metal-air batteries, the biggest bottleneck is the cathode material-oxygen reduction (ORR) catalyst. At present, most of the cathode materials of metal-air batteries use precious metals such as platinum carbo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/24B01J37/08B01J37/06B01J35/10B01J37/03B01J31/02H01M4/88H01M4/90H01M4/96
CPCB01J27/24B01J31/0244B01J35/0033B01J35/1019B01J35/1023B01J35/1028B01J37/036B01J37/06B01J37/082H01M4/8825H01M4/9091H01M4/96Y02E60/50
Inventor 唐有根易诗捷王海燕蔡桂韩
Owner CENT SOUTH UNIV
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