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A kind of preparation method of nitrogen-sulfur co-doped carbon-coated transition metal nano-sulfide electrochemical oxygen catalyst

A technology of nitrogen-sulfur co-doping and transition metals, applied in nanotechnology, nanotechnology, nanotechnology for materials and surface science, etc., can solve the problems of scarcity and high price that hinder the large-scale practical application of batteries, and achieve Rich reserves, good electrical conductivity, and many surface defects

Active Publication Date: 2022-08-09
GUANGXI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

So far, the noble metal-based catalyst Pt is considered to be the most efficient catalyst for the ORR reaction, and the noble metal IrO 2 and RuO 2 considered to be the most active electrocatalysts for OER [Nat.Commun.2013, 4, 1805], but their scarcity and high price severely hinder the large-scale practical application of batteries

Method used

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  • A kind of preparation method of nitrogen-sulfur co-doped carbon-coated transition metal nano-sulfide electrochemical oxygen catalyst
  • A kind of preparation method of nitrogen-sulfur co-doped carbon-coated transition metal nano-sulfide electrochemical oxygen catalyst
  • A kind of preparation method of nitrogen-sulfur co-doped carbon-coated transition metal nano-sulfide electrochemical oxygen catalyst

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Embodiment 1

[0030] A method for preparing a nitrogen-sulfur co-doped carbon-coated transition metal nano-sulfide electrochemical oxygen catalyst, the specific operation steps are as follows:

[0031] (1) Put 1.3 g of 2,6-diacetylpyridine into a 150ml flat-bottomed flask, measure 50ml of absolute ethanol and add it to the flat-bottomed flask, stir until 2,6-diacetylpyridine is completely dissolved, according to the acetyl group Add 1.99 g of 2,2'-diaminodiphenyl disulfide in a molar ratio of 1:1 to amino group, stir until completely dissolved, add 0.1 g of oxalic acid to the flat-bottomed flask, stir for 30 min, transfer the flask to an oil bath, The temperature was raised to 60°C, and the reaction was carried out under constant temperature stirring for 10 hours;

[0032](2) the obtained solution after the reaction in step (1) was cooled to room temperature, 1.90 g of cobalt chloride hexahydrate was added while stirring, and the room temperature was reacted for 12 hours. After the reaction...

Embodiment 2

[0036] A method for preparing a nitrogen-sulfur co-doped carbon-coated transition metal nano-sulfide electrochemical oxygen catalyst, the specific operation steps are as follows:

[0037] (1) Put 1.3 g of 2,6-diacetylpyridine into a 150ml flat-bottomed flask, measure 50ml of anhydrous ethanol as an organic solvent and add it to the flat-bottomed flask, stir until 2,6-diacetylpyridine is completely dissolved, press The molar ratio of acetyl group and amino group is 1:1, add 1.98g of sulfur-containing amino monomer 4,4-diaminodiphenyl sulfide, stir until completely dissolved, add 0.1g oxalic acid to the flat-bottomed flask, stir for 30min, turn the flask In an oil bath pot, the temperature is raised to 80°C, and the reaction is carried out under constant temperature stirring for 12 hours;

[0038] (2) the obtained solution after the step (1) reaction is cooled to room temperature, 2.16g of transition metal-containing inorganic salt ferric trichloride hexahydrate is added while s...

Embodiment 3

[0043] A method for preparing a nitrogen-sulfur co-doped carbon-coated transition metal nano-sulfide electrochemical oxygen catalyst, the specific operation steps are as follows:

[0044] (1) Put 1.0 g of 2,6-diacetylpyridine into three 150ml flat-bottomed flasks respectively, measure 50ml of organic solvent dehydrated ethanol and add it to the flat-bottomed flask, and stir until 2,6-diacetylpyridine is completely Dissolve, add 1.31g of sulfur-containing amino monomer 2,2'-diaminodiphenyl sulfide according to the molar ratio of acetyl group and amino group 1:1, stir until completely dissolved, add 0.1g oxalic acid to the flat-bottomed flask, stir for 30min , transfer each flask to an oil bath, heat up to 100°C, and react under constant temperature stirring for 8 hours;

[0045] (2) cooling the obtained solution after the step (1) reaction to room temperature, adding 3.6g, 1.2g, 0.4g of transition metal-containing nickel dichloride hexahydrate to the obtained material in the ab...

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Abstract

The invention discloses a preparation method of a nitrogen-sulfur co-doped carbon-coated transition metal nanometer sulfide electrochemical oxygen catalyst: (1) taking a 2,6-diacetylpyridine monomer solution, adding a sulfur-containing amino monomer, Stir and dissolve, add acid, heat up, and react; (2) cooling, adding inorganic salt containing transition metal to react, evaporating, drying and grinding; (3) first thermal cracking, cooling to room temperature, pickling and drying of the obtained material; (4) The second thermal cracking, namely obtaining nitrogen-sulfur co-doped carbon-coated transition metal nano-sulfide electrochemical oxygen catalyst. The nitrogen-sulfur co-doped carbon-coated transition metal nanometer sulfide electrochemical oxygen catalyst prepared by the method is composed of transition metal sulfide, carbon, nitrogen and sulfur, and the material has the structure of highly graphitized carbon layer coating the transition metal sulfide At the same time, it has the characteristics of good electrical conductivity, mesoporous and macroporous structure, many surface defects, and efficient bifunctional oxygen (oxygen reduction and oxygen evolution) catalytic performance.

Description

technical field [0001] The invention relates to the field of electrochemical new energy catalysis materials, in particular to a preparation method of a nitrogen-sulfur co-doped carbon-coated transition metal nanometer sulfide electrochemical oxygen catalyst. Background technique [0002] In the transition from fossil fuels to renewable energy, we must face the growing demands of energy collection, conversion, storage and release. In order to achieve better energy utilization, the development of advanced technologies (water splitting devices, fuel cells to metal-air batteries) is a theme of modern society. In every aspect of our industry and daily life, power plays a vital role in driving a variety of devices, from large grid energy storage systems to automobiles and small electronic devices [J.Mater.Chem.A,2019,7, 18183]. Lithium-ion batteries are by far the most successful power source and have been widely used in various fields. However, the safety and high cost of elec...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M4/88H01M4/90B82Y30/00B82Y40/00
CPCH01M4/8825H01M4/90H01M4/9083B82Y30/00B82Y40/00H01M2004/8689Y02P20/133
Inventor 田植群吕丹丹姚思先沈培康
Owner GUANGXI UNIV
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