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Method and product for preparing oxygen reduction catalyst from biomass

A biomass and catalyst technology, applied in the field of biomass-based carbon material preparation, can solve the problems of poor conductivity, difficult graphitization, and low carbonization degree, and achieve the effect of optimizing the degree of graphitization

Active Publication Date: 2021-05-07
HUAZHONG UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This method has several disadvantages: 1) the raw material applicability is narrow, only suitable for a small amount of nitrogen-rich biomass (nitrogen N>3wt.%); 2) the precipitation of nitrogen during high-temperature carbonization leads to the reduction of active sites, while Low-temperature carbonization, the degree of carbonization is too low, and the conductivity is too poor, so the contradiction between conductivity and active sites brings technical difficulties; 3) It is difficult to quantitatively control the nitrogen content on the surface of carbon products, and more importantly, the form of nitrogen (Pyridine, pyrrole, G nitrogen, nitrogen oxide) are even more unpredictable, unable to be prepared in a directional manner, resulting in unstable catalytic activity; 4) The inherent structure of biomass macromolecules is difficult to graphitize. Amorphous carbon often has the disadvantage of poor cycle stability in terms of catalytic performance

Method used

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  • Method and product for preparing oxygen reduction catalyst from biomass
  • Method and product for preparing oxygen reduction catalyst from biomass
  • Method and product for preparing oxygen reduction catalyst from biomass

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0054] (1) Wash and crush the collected chestnut shells to 80 mesh, dry in an oven at 80 degrees for 24 hours, take 10 g of dried samples, add 10 ml of 0.1 mol / l ferric nitrate solution (that is, 1 g of chestnut shells corresponds to 0.01 mol of nitric acid iron), stirred at room temperature for 24 hours, and vacuum freeze-dried at minus 30°C;

[0055] (2) Use a fixed-bed reactor with a diameter of 45 mm and a length of 60 mm to pyrolyze the impregnated sample. After the reactor is heated to 700 ° C, the sample is quickly placed in the middle of the reactor (the heating rate is 20 ° C / min ), the reaction time is 30min, the mixture is fully pyrolyzed, the argon gas flow rate is 50min / min, and the pyrolytic carbon is obtained by cooling under an inert atmosphere, which is recorded as composite material-1;

[0056] (3) Take 1g of composite material-1, disperse it into 50ml of ethanol solution, soak and stir for 12h, add 10g of melamine into the solution soaked in composite mate...

Embodiment 2

[0061] (1) Wash and crush the collected bamboo chips to 120 mesh, dry in an oven at 80 degrees for 24 hours, take 10 g of the dried sample, add 500 ml of 0.2 mol / l cobalt oxalate solution, stir at room temperature for 24 hours, minus 40 ℃ vacuum freeze-drying;

[0062] (2) Use a fixed-bed reactor with a diameter of 45mm and a length of 60mm to pyrolyze the impregnated sample. After heating the reactor to 900°C, put the sample into the middle of the reactor quickly, and the reaction time is 300min. Fully pyrolyze, the helium flow rate is 50min / min, and cool in an inert atmosphere to obtain pyrolytic carbon, which is recorded as composite material-1;

[0063](3) Take 1g of composite material-1, disperse it into 200ml of isopropanol solution, soak and stir for 24 hours, add 20g of melamine into the solution soaked in composite material-1, and add 200ml of 0.2mol / l manganese acetate solution at the same time, shake, Stir for 5 hours, dry in an oven at 80°C for 36 hours to obtain ...

Embodiment 3

[0068] (1) Wash and crush the collected bamboo chips to 120 mesh, dry in an oven at 80 degrees for 24 hours, take 10 g of the dried sample, add 200 ml of 0.1 mol / l nickel nitrate solution, stir at room temperature for 24 hours, minus 50 ℃ vacuum freeze-drying to obtain the impregnated sample;

[0069] (2) Use a fixed-bed reactor with a diameter of 45 mm and a length of 60 mm to pyrolyze the impregnated sample. After heating the reactor to 1000 ° C, the sample is quickly placed in the middle of the reactor, and the reaction time is 300 min. Fully pyrolyze, the argon flow rate is 50min / min, and cool in an inert atmosphere to obtain pyrolytic carbon, which is recorded as composite material-1;

[0070] (3) Take 1g of composite material-1, disperse it into 100ml of ethanol solution, soak and stir for 12h, add 5g of melamine into the solution soaked in composite material-1, and add 500ml of manganese sulfate solution of 0.05mol / l at the same time, oscillate, and stir for 24h , drie...

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Abstract

The invention discloses a method and a product for preparing an oxygen reduction catalyst from biomass, which comprises the following steps: S1 mixing and freeze-drying the biomass and a transition metal salt solution to obtain a mixture; S2 pyrolyzing the mixture under an inert atmosphere Obtain a core-shell structure material with graphite carbon layer wrapped transition metal nanoparticles; S3 disperse the core-shell structure material in a volatile organic solvent, add nitrogen-containing organic matter and transition metal salt solution 2, mix and dry to obtain mixture 2 ; S4 Pyrolyzing the mixture two under an inert atmosphere to grow nitrogen-containing carbon nanofibers on the surface of the core-shell structure material, and obtain the required oxygen reduction catalyst after washing, filtering and drying. The invention can prepare the sea urchin-shaped oxygen reduction catalyst, has developed porosity, high nitrogen content, stable metal active sites, and has good activity and durability in oxygen reduction catalysis.

Description

technical field [0001] The invention belongs to the field of preparation of biomass-based carbon materials, and more specifically relates to a method and product for preparing an oxygen reduction catalyst from biomass, in particular to a method for preparing a nitrogen-rich carbon catalyst coated with metal alloy nanoparticles by utilizing biomass. Background technique [0002] Metal-air battery is a device that can continuously convert chemical energy into electrical energy. Metal-air battery has the advantages of high conversion efficiency and convenient use. Especially in recent years, the research and development and commercialization of hydrogen energy vehicles have attracted extensive attention. , while noble metal (including platinum, palladium, ruthenium, etc.) catalysts are usually used in the cathode oxygen reduction process in batteries, and their high cost, limited resources and poor durability restrict the further development of batteries. Therefore, there is an...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M4/88H01M4/90H01M4/96H01M12/06
CPCH01M4/8825H01M4/90H01M4/9041H01M4/96H01M12/06
Inventor 陈汉平夏孙文杨海平陈应泉陈伟陈旭邵敬爱张雄王贤华张世红
Owner HUAZHONG UNIV OF SCI & TECH
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