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Catalytic material for oxygen reduction and with gradient pore structure and preparation method thereof

A catalytic material and gradient pore technology, which is applied in the field of oxygen reduction catalytic materials with gradient pore structure and its preparation, can solve the problems of irregular morphology, increase the cost of material preparation, and difficult to control the morphology of intermediate products, etc. Effect of reduction activity, good oxygen reduction performance

Pending Publication Date: 2021-08-27
广东省武理工氢能产业技术研究院
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although this patent application realizes the aqueous phase synthesis of ZIF, the method introduces amines as additives in the preparation process, which increases the preparation cost of the material to a certain extent.
And, when generating solid-state intermediates, a large amount of 2-methylimidazole is added, and the product morphology of the intermediates is difficult to control, and basically there is no regular morphology
[0005] In addition, most metal-organic framework-derived catalytic materials have a high specific surface area, but their pore size distribution is generally concentrated below 5nm, and the lack of large-sized mesopores and macropores will limit the catalytic materials in the process of oxygen reduction reaction. Material transfer efficiency, especially the high mass transfer requirements of batteries at high current densities

Method used

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  • Catalytic material for oxygen reduction and with gradient pore structure and preparation method thereof
  • Catalytic material for oxygen reduction and with gradient pore structure and preparation method thereof
  • Catalytic material for oxygen reduction and with gradient pore structure and preparation method thereof

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Effect test

Embodiment 1

[0029] A method for preparing an oxygen reduction catalytic material with a gradient pore structure mainly includes the following steps.

[0030] 1) Weigh 1.00g of zinc nitrate hexahydrate into a 50mL beaker, add 30mL of deionized water and a magnet, stir and dissolve on a magnetic stirrer to obtain solution A, set aside.

[0031] 2) Dissolve 11.00g of 2-methylimidazole, 0.1g of iron phthalocyanine and 0.5g of silica template in 240mL of deionized water to obtain solution B.

[0032] 3) Quickly add solution B to solution A with continuous magnetic stirring, stir at room temperature for 12 hours, centrifuge the solution 3 times with deionized water, wash 3 times with absolute ethanol, and dry under vacuum at 80°C to obtain a gray precursor material .

[0033] 4) Put the gray precursor obtained in step 3) in a high-temperature tube furnace, use high-purity argon as a protective gas, raise the temperature to 800°C at a rate of 3°C / min, and keep it for 150min. After the heat tre...

Embodiment 2

[0036] A method for preparing an oxygen reduction catalytic material with a gradient pore structure mainly includes the following steps.

[0037] 1) Weigh 1.50g of zinc nitrate hexahydrate into a 50mL beaker, add 30mL of deionized water and a magnet, stir and dissolve on a magnetic stirrer to obtain solution A, and set aside.

[0038] 2) Weigh 10.00g of 2-methylimidazole, 0.05g of iron phthalocyanine and 0.10g of silica template and dissolve in 150mL of deionized water to obtain solution B.

[0039] 3) Quickly add solution B into solution A with continuous magnetic stirring, stir at room temperature for 8 hours, centrifuge the solution 3 times with deionized water, wash 3 times with absolute ethanol, and dry under vacuum at 50°C to obtain a gray precursor material .

[0040]4) Put the gray precursor obtained in step 3) in a high-temperature tube furnace, use high-purity argon as a protective gas, raise the temperature to 1000°C at a rate of 6°C / min, and keep it for 90min. Af...

Embodiment 3

[0043] A method for preparing an oxygen reduction catalytic material with a gradient pore structure mainly includes the following steps.

[0044] 1) Weigh 1.19g of zinc nitrate hexahydrate into a 50mL beaker, add 30mL of deionized water and a magnet, stir and dissolve on a magnetic stirrer to obtain solution A, and set aside.

[0045] 2) Dissolve 11.82g of 2-methylimidazole, 0.08g of iron phthalocyanine and 0.36g of silica template in 180mL of deionized water to obtain solution B.

[0046] 3) Quickly add solution B to solution A with continuous magnetic stirring, stir at room temperature for 24 hours, centrifuge the solution 3 times with deionized water, wash 3 times with absolute ethanol, and dry under vacuum at 60°C to obtain a gray precursor material .

[0047] 4) Put the gray precursor obtained in step 3) in a high-temperature tube furnace, use high-purity argon as a protective gas, raise the temperature to 950°C at a rate of 5°C / min, and keep it for 120min. After the he...

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Abstract

The invention discloses a catalytic material for oxygen reduction and with a gradient pore structure and a preparation method thereof. The preparation method comprises the following steps: dissolving zinc nitrate hexahydrate in deionized water; adding an aqueous zinc nitrate hexahydrate solution into an aqueous solution containing 2-methylimidazole, iron phthalocyanine and a silicon dioxide template, and carrying out stirring; performing centrifuging, washing and drying to prepare a gray precursor sample; and carrying out heat treatment on the precursor in an inert atmosphere and removing a template by using hydrofluoric acid to obtain the catalytic material for oxygen reduction and with the gradient pore structure. According to the catalytic material for oxygen reduction, an iron source and a silicon dioxide template are introduced on the basis of a microporous ZIF-8 derivative material with a high specific surface area; the material has a large number of iron-nitrogen active sites, low-boiling-point zinc volatilizes in a carbonization process to generate a large number of micropores, and the gradient porous structure is constructed by adding mesopores and macropores brought by the silicon dioxide template, so the mass transfer rate of an electrochemical reaction is improved; and the material shows excellent oxygen reduction performance in both alkaline and acidic media, and can be applied to various chemical power supply devices as an oxygen reduction catalyst.

Description

technical field [0001] The invention belongs to the field of new energy materials, and in particular relates to an oxygen reduction catalytic material with a gradient pore structure and a preparation method thereof. Background technique [0002] Green chemical power sources such as high-efficiency fuel cells and metal-air batteries have been developed rapidly in the past decade, and they have achieved commercial applications in some fields, and are getting closer to the goal of large-scale commercialization. In addition to the need to improve the output performance of the battery, the high production cost is also one of the important reasons that limit its commercialization. The oxygen reduction reaction occurs on the cathode side of the above-mentioned green chemical power sources to ensure the operation of the battery, but the oxygen reduction reaction with slow kinetics usually requires the use of noble metal catalytic materials to accelerate the electrochemical reaction....

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/80B01J35/10
CPCB01J23/80B01J35/33B01J35/61
Inventor 张锐明孟子寒吴佳为龚聪文唐浩林
Owner 广东省武理工氢能产业技术研究院
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