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Preparation and application for non-noble metal electro-catalyst with core-shell structure

A non-precious metal, electrocatalyst technology, applied in structural parts, circuits, electrical components, etc., can solve the problems of high oxygen reduction activity of non-precious metal electrocatalysts, poor oxygen reduction activity of electrocatalysts, complicated preparation methods, etc. The effect of stable structure and simple preparation method

Inactive Publication Date: 2016-03-30
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In 2007, the Dodelet research group used the impregnation method to load iron porphyrin on the surface of the carbon support, and then used NH 3 The sample was processed, and the obtained sample had higher oxygen reduction activity, but its durability was poor (Charreteur, F., Jaouen, F. & Dodelet, J.‐P, Electrochim.Acta, 2009, 54, 6622‐6630 )
Patent CN200810040926 uses ultrasonic method to synthesize metalloporphyrins in situ, then loads them on carbon supports, and heats them to obtain non-precious metal electrocatalysts, which have poor oxygen reduction activity
[0004] The above preparation methods all use metalloporphyrins as precursors to prepare non-precious metal electrocatalysts. The preparation methods are relatively complicated, or reagents that are harmful to the environment are used in the preparation process, and the obtained non-precious metal electrocatalysts only have high oxygen reduction activity

Method used

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  • Preparation and application for non-noble metal electro-catalyst with core-shell structure
  • Preparation and application for non-noble metal electro-catalyst with core-shell structure
  • Preparation and application for non-noble metal electro-catalyst with core-shell structure

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Weigh 6g commercial carbon black (Ketjen EC-600, 20-30nm, 1400m 2 / g) dispersed in 600mL3mol / LHNO 3 In the solution, reflux in a water bath at 80° C. for 1 hour, filter with suction, wash with deionized water until neutral, and dry to obtain pretreated carbon black. Add 50 mg of meso‐tetrakis (4‐methoxyphenyl) porphyrin iron and 70 mL of chloroform into a 250 mL round bottom flask, ultrasonically dissolve the porphyrin, then add 100 mg of pretreated carbon black, ultrasonic for 30 min, 65 °C, The solvent was removed by rotary evaporation under the condition of 100 rpm, and the obtained solid was heated to 800° C. under the protection of an argon atmosphere, and was stabilized for 2 hours and then naturally cooled to room temperature. After 0.5MH 2 SO 4 The solution was stirred in a water bath at 80° C. for 6 h, then suction-filtered, washed with water until neutral, and dried in vacuum at 65° C. to finally obtain a black powdery solid.

[0032] As shown in Figure 1,...

Embodiment 2

[0037] Weigh 6g commercial carbon black (Ketjen EC-600, 20-30nm, 1400m 2 / g) dispersed in 600mL3mol / LHNO 3 In the solution, reflux in a water bath at 80° C. for 1 hour, filter with suction, wash with deionized water until neutral, and dry to obtain pretreated carbon black. Add 100mg meso‐tetrakis(4‐methoxyphenyl)porphyrin iron and 70mL chloroform into a 250mL round bottom flask, ultrasonically dissolve the porphyrin, then add 100mg pretreated carbon black, ultrasonicate for 30min, 65°C, The solvent was removed by rotary evaporation under the condition of 100 rpm, and the obtained solid was heated to 800° C. under the protection of an argon atmosphere, and was stabilized for 2 hours and then naturally cooled to room temperature. After 0.5MH 2 SO 4 The solution was stirred in a water bath at 80° C. for 6 h, then suction-filtered, washed with water until neutral, and dried in vacuum at 65° C. to finally obtain a black powdery solid.

[0038] Such as Figure 5 , the obtained ...

Embodiment 3

[0043] Weigh 6g commercial carbon black (Ketjen EC-600, 20-30nm, 1400m 2 / g) dispersed in 600mL3mol / LHNO 3 In the solution, reflux in a water bath at 80° C. for 1 hour, filter with suction, wash with deionized water until neutral, and dry to obtain pretreated carbon black. Add 1000mg meso‐tetrakis(4‐methoxyphenyl)porphyrin iron and 70mL chloroform into a 250mL round bottom flask, ultrasonically dissolve the porphyrin, then add 100mg pretreated carbon black, ultrasonicate for 30min, 65°C, The solvent was removed by rotary evaporation under the condition of 100 rpm, and the obtained solid was heated to 800° C. under the protection of an argon atmosphere, and was stabilized for 2 hours and then naturally cooled to room temperature. After 0.5MH 2 SO 4 The solution was stirred in a water bath at 80° C. for 6 h, then suction-filtered, washed with water until neutral, and dried in vacuum at 65° C. to finally obtain a black powdery solid.

[0044] The morphology and performance of...

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Abstract

The invention provides preparation and application for a non-noble metal electro-catalyst with a core-shell structure, and belongs to the field of fuel cells and metal / air cell catalysts. The preparation for the non-noble metal electro-catalyst comprises the steps of dispersing carbon black into an HNO3 solution, performing back flow at a temperature of 20-90 DEG C for 0.5-10h, performing suction filtration, washing until the solution is neutral, and drying; dissolving porphyry into organic solvent, adding pre-processed carbon black, performing ultrasonic dispersion for more than 20 min, and drying the solvent by evaporation; roasting the rest materials in carrier gas at a temperature of 400-1,200 DEG C for 0.5-4h, cooling to room temperature, and adding an acidic water solution, and performing back flow in a water bath at a temperature of 30-90 DEG C for 1-24h, and then performing suction filtration, washing by deionized water until the solution is neutral, and drying to obtain the non-noble metal electro-catalyst with the core-shell structure. The preparation is simple in operation, easy to control, mild in conditions and environment-friendly; and the prepared non-noble metal electro-catalyst with the core-shell structure is quite high in oxygen reduction activity, and can be used for the fuel cells and the metal / air cells.

Description

technical field [0001] The invention belongs to the field of catalysts for fuel cells and metal / air batteries, and relates to the preparation and application of a core-shell structure non-noble metal electrocatalyst. Background technique [0002] Due to the advantages of high energy density, high efficiency, and environmental friendliness, fuel cells have attracted extensive attention. The cathodes of fuel cells mainly use noble metal platinum and its alloys as oxygen reduction catalysts. However, due to the shortcomings of platinum, such as high price, scarce resources, poor durability, and easy to be poisoned, the commercialization of fuel cells is seriously hindered. Therefore, it is of great importance to develop non-noble metal electrocatalysts with higher oxygen reduction activity, better durability, and lower cost. [0003] Since Jasinski discovered that cobalt phthalocyanine has oxygen reduction activity in alkaline system in 1964 (R. Jasinski, Nature, 1964, 201, 12...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/90
CPCH01M4/9008H01M4/9083Y02E60/50
Inventor 宋玉江李佳
Owner DALIAN UNIV OF TECH
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