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Preparation method of macroporous carbon oxygen reduction catalyst containing sulfur, nitrogen and transition metal element

A technology of transition metal elements and procatalysts, applied in the direction of physical/chemical process catalysts, chemical instruments and methods, electrical components, etc., to achieve the effect of increasing the concentration of conjugated electrons, uniform distribution, and large specific surface area

Inactive Publication Date: 2015-10-14
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The glucose thiourea resin obtained by the condensation of the aldehyde group of glucose and the amine group of thiourea proposed by the present invention is a carbon source, and the method of synthesizing a sulfur-containing macroporous carbon-based non-noble metal catalyst has not been reported

Method used

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  • Preparation method of macroporous carbon oxygen reduction catalyst containing sulfur, nitrogen and transition metal element
  • Preparation method of macroporous carbon oxygen reduction catalyst containing sulfur, nitrogen and transition metal element
  • Preparation method of macroporous carbon oxygen reduction catalyst containing sulfur, nitrogen and transition metal element

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Embodiment one: preparation of glucose thiourea prepolymer

[0025] Heat 3.96g of glucose to 40°C and dissolve in 3mL of deionized water, heat 1.52g of thiourea to 40°C and dissolve in 4mL of deionized water. Add the thiourea solution into the glucose solution. At this time, the mass ratio of glucose to thiourea is 1:0.38. Place it in a water bath at 85°C, add 0.5 mL of hydrochloric acid dropwise, and stir thoroughly. After reacting for 45 minutes, the viscosity of the liquid increased significantly, and after the color changed from colorless to light yellow to orange red, 40 mL of deionized water was added to terminate the polymerization, and cooled to obtain a glucose thiourea prepolymer solution.

Embodiment 2

[0026] Embodiment two: preparation of catalyst precursor

[0027] Heat 3.96g of glucose to 40°C and dissolve in 3mL of deionized water, heat 3.96g of thiourea to 40°C and dissolve in 8mL of deionized water. Add the thiourea solution into the glucose solution. At this time, the mass ratio of glucose to thiourea is 1:1. Put it in a water bath at 85°C, add 0.5 mL of hydrochloric acid dropwise, and stir well. After reacting for 45 minutes, the viscosity of the liquid increased significantly, and after the color changed from colorless to light yellow to orange red, 40 mL of deionized water was added to terminate the polymerization, and cooled to obtain a glucose thiourea prepolymer solution.

[0028] Take another beaker and put nano-CaCO 3 Disperse 5g of the powder evenly in 30mL of manganese chloride solution (containing 0.1 mmol of manganese chloride) to obtain a suspension, add it to the above glucose thiourea prepolymer solution, heat in a water bath at 85°C, stir for 50 minut...

Embodiment 3

[0029] Example 3: Preparation of nitrogen-containing and sulfur-containing macroporous carbon-supported iron catalyst

[0030] Heat 3.96g of glucose to 40°C and dissolve in 3mL of deionized water, heat 9.12g of thiourea to 40°C and dissolve in 12mL of deionized water. Add the thiourea solution into the glucose solution. At this time, the mass ratio of glucose to thiourea is 1:2.3. Place it in a water bath at 85°C, add 0.5 mL of hydrochloric acid dropwise, and stir thoroughly. After reacting for 45 minutes, the viscosity of the liquid increased significantly, and after the color changed from colorless to light yellow to orange red, 40 mL of deionized water was added to terminate the polymerization, and cooled to obtain a glucose thiourea prepolymer solution.

[0031] Take another beaker and put nano-CaCO 3 5g of the powder is evenly dispersed in 30mL ferric sulfate solution (containing 0.5 mmoles of ferric sulfate) to obtain a suspension, which is added to the above glucose thio...

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Abstract

The invention relates to a preparation method of a oxygen reduction catalyst and aims to provide a preparation method of a macroporous carbon oxygen reduction catalyst containing sulfur, nitrogen and transition metal element. The method comprises the following steps: adding a thiourea solution into a glucose solution, dropwise adding hydrochloric acid in water bath, and reacting to obtain a glucose thiourea prepolymer solution; adding a suspension containing transition metal salt and a nano-CaCO3 powder into the solution, heating to react and spray-drying to obtain a catalyst precursor; heating to carry out deep polymerization and carbonization; and cooling, ball-milling, removing a template by the use of hydrochloric acid, rinsing and drying to obtain a product. The transition metal element is added before the formation of a porous material such that more catalytic centers can be formed and distribution of catalytic centers is more uniform. The catalyst has large specific surface area, good conductivity and high catalytic activity, and is especially suitable for high current working condition. A synthesized non-noble metal catalyst can be applied to various fuel cells and also can be used as a cathode catalyst of an air cell. Costs are low.

Description

technical field [0001] The invention relates to a method for preparing an oxygen reduction catalyst, in particular to using glucose thiourea resin obtained by polymerization of glucose and thiourea as a carbon source, and obtaining a catalyst precursor by calcining a mixture of transition metal salt, glucose thiourea resin and nanometer calcium carbonate , a macroporous carbon oxidation procatalyst containing sulfur, nitrogen and transition metal elements obtained after template removal with acid and a preparation method thereof. Background technique [0002] Fuel cell is a new power generation technology with high efficiency, low pollution and diversified energy sources. The fuel cell power generation system is not only lower in cost than traditional fossil fuels, but also has the advantages of cleanliness and high efficiency. It can also be combined with nuclear energy, biomass energy, solar energy, wind energy and other power generation technologies to make energy use div...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/24H01M4/90H01M8/00H01M12/00
Inventor 刘宾虹周恒李洲鹏
Owner ZHEJIANG UNIV
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