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Preparation method for metal single atom/phosphor doping carbon nitride photocatalyst

A carbon nitride light and phosphorus doping technology, applied in the direction of physical/chemical process catalysts, chemical instruments and methods, non-metallic elements, etc., can solve the problem of narrow forbidden energy band, achieve low preparation cost, and improve visible light absorption Utilization, the effect of excellent photolysis water hydrogen production activity

Inactive Publication Date: 2018-11-30
XIANGTAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, at present, the preparation of cheap metal single atom / carbon nitride photocatalyst materials with high loading and better activity than Pt cocatalyst, especially the high loading of cheap metal single atom / nitrogen with narrow forbidden energy band and wide visible light absorption range Carbonized photocatalytic materials remain a major challenge

Method used

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  • Preparation method for metal single atom/phosphor doping carbon nitride photocatalyst
  • Preparation method for metal single atom/phosphor doping carbon nitride photocatalyst
  • Preparation method for metal single atom/phosphor doping carbon nitride photocatalyst

Examples

Experimental program
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Effect test

Embodiment 1

[0027] Mix 10 g of urea and 0.2 g of cobalt chloride in ethanol uniformly, reflux at 45° C. for 3 h, and then evaporate the solvent to dryness to obtain urea-cobalt complex. Mix 5g of urea-cobalt complex and 4g of melamine evenly, place in a tube furnace, raise the temperature to 580°C under an argon atmosphere, keep the temperature at a constant temperature for 3 hours, and after natural cooling, monoatomic cobalt / carbon nitride is obtained. After the monoatomic cobalt / carbon nitride and sodium hypophosphite are mixed uniformly at a mass ratio of 1:2, they are placed in a tube furnace and heated to 300°C under an argon atmosphere, and the temperature is kept constant for 2 hours. After natural cooling, the obtained solid was washed several times and dried to obtain monoatomic cobalt / phosphorus doped carbon nitride.

Embodiment 2

[0029] Mix 20g of urea with 40mg of silver nitrate, 40mg of ferric nitrate and 40mg of copper acetate in water, reflux at 60°C for 2 hours, and then evaporate the solvent to dryness to obtain a urea silver+iron+copper complex. Mix 10g of urea silver+iron+copper complex with 4g of dicyandiamide evenly, put it in a tube furnace, raise the temperature to 500°C under an argon atmosphere, keep the temperature at a constant temperature for 10h, and after natural cooling, monoatomic silver+iron is obtained + Copper / Carbon Nitride. Monoatomic silver+iron+copper / carbon nitride and magnesium hypophosphite are mixed evenly at a mass ratio of 1:0.5, and placed in a tube furnace under an argon atmosphere to raise the temperature to 400°C and keep the temperature constant for 1h. After natural cooling, the obtained solid was washed several times and dried to obtain monoatomic silver+iron+copper / phosphorus doped carbon nitride.

Embodiment 3

[0031] Mix 15g of urea with 0.4g of ferric chloride and 0.4g of nickel nitrate in methanol, reflux at 25°C for 24h, and then evaporate the solvent to dryness to obtain urea iron+nickel complex. Put 10g of urea-iron+nickel complex in a tube furnace, raise the temperature to 650°C under a mixed gas atmosphere of nitrogen and argon, and keep the temperature for 1h to obtain monatomic iron+nickel / carbon nitride. The mixture of monoatomic iron+nickel / carbon nitride and potassium hypophosphite, magnesium hypophosphite and ammonium hypophosphite is mixed uniformly at a mass ratio of 1:5, and placed in a tube furnace in an argon atmosphere Lower the temperature to 250°C and keep the temperature constant for 4h. After natural cooling, the obtained solid was washed several times and dried to obtain monoatomic iron+nickel / phosphorous doped carbon nitride.

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Abstract

The invention discloses a preparation method for metal single atom / phosphor doping carbon nitride photocatalyst. The preparation process of the preparation method comprises the following steps: a) preparing urea metal complex: enabling metal salt and urea to react in a solvent to obtain urea metal complex; b: carrying out heat polycondensation: under the protection of inert atmosphere, evenly mixing the urea metal complex and carbon nitride precursor, and carrying out the heat polycondensation to obtain a heat polycondensation product; c) carrying out phosphorization: after the heat polycondensation product and hypophosphorous acid salt are evenly mixed, carrying out heat treatment under the inert atmosphere to obtain the metal single atom / phosphor doping carbon nitride photocatalyst. By use of the method disclosed by the invention, the carbon nitride photocatalyst of which the metal single atom capacity is 20wt% is prepared, and the hydrogen evolution rate is 2 times of that of phosphor doping carbon nitride which takes noble metal platinum as a hydrogen evolution cocatalyst. The preparation method has the advantages of rich raw material, low price, simple preparation method, lowpreparation cost and the like.

Description

technical field [0001] The invention relates to a method for preparing a metal single atom / phosphorous doped carbon nitride photocatalyst, belonging to the field of photocatalytic material preparation. Background technique [0002] Photocatalytic water splitting technology is one of the ideal methods to realize solar energy conversion and obtain clean energy-hydrogen energy. Carbon nitride is a non-metal semiconductor photocatalytic material, which has the advantages of wide source of raw materials, simple preparation, low price, narrow band gap (about 2.7eV), and good visible light response. However, the slow transfer rate of photogenerated charges and the low utilization rate of solar energy lead to the low efficiency of solar-driven carbon nitride photolysis of water for hydrogen production. [0003] In order to increase the hydrogen production rate of carbon nitride by photolysis of water, the current research mainly focuses on the following two aspects: 1) broaden the ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/24C01B3/04
CPCC01B3/042B01J27/24B01J35/391B01J35/39Y02E60/36
Inventor 赵才贤陈烽焦培鑫兰富军詹夏罗和安
Owner XIANGTAN UNIV
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