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Ball-milling assisted method for preparing carbon nitrogen based monatomic iron catalyst

An iron catalyst, carbon-nitrogen-based single technology, applied in electrical components, grain processing, battery electrodes, etc., can solve the problems of easy agglomeration of metal active sites, cumbersome catalyst preparation process, unfavorable sustainable development, etc., and achieve low cost. , short response time, environmental friendly effect

Active Publication Date: 2018-11-27
CAPITAL NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the metal active sites of these catalysts are prone to agglomeration during the synthesis process, resulting in low atom utilization, and the synthesis process generally involves the use of a large amount of organic solvents and pickling process, resulting in a cumbersome catalyst preparation process, which is not conducive to sustainable development.

Method used

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  • Ball-milling assisted method for preparing carbon nitrogen based monatomic iron catalyst
  • Ball-milling assisted method for preparing carbon nitrogen based monatomic iron catalyst
  • Ball-milling assisted method for preparing carbon nitrogen based monatomic iron catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment １

[0030] Add 81 milligrams (mg) of zinc oxide, 289 mg of 2-ethylimidazole, 10 mg of ammonium sulfate, and 16 mg of iron porphyrin into an 80 mL ball mill jar, mix well, then add 200 μL of N,N-diethylformamide, and mix 20 Put the zirconia balls with a diameter of 10mm into the ball milling pot, install the ball milling pot on the ball mill, adjust the ball milling condition to 50 Hz, and ball mill twice, each time for 30 minutes, with a stop of 5 minutes in between. After the ball milling, wash the samples in the ball mill tank with water, centrifuge and wash twice with ethanol, dry in a vacuum oven at 80°C for 12 hours, and put the powder into a magnetic boat after simple grinding, and heat it in a tube furnace. Nitrogen or argon protection is required, the heating temperature is 950°C, the heating rate is 5°C / min, the pyrolysis is 3h, and the black Fe-N-C single-atom catalyst is obtained.

[0031] The Fe-N-C single-atom catalyst, high-angle annular dark field image-scanning tra...

Embodiment 2

[0036] Add 81 milligrams (mg) of zinc oxide, 289 mg of 2-ethylimidazole, 10 mg of ammonium sulfate, and 21 mg of iron porphyrin into an 80 mL ball mill jar, mix well, then add 200 μL of N,N-diethylformamide, and mix 20 Put the zirconia balls with a diameter of 10mm into the ball milling pot, install the ball milling pot on the ball mill, adjust the ball milling condition to 50 Hz, and ball mill twice, each time for 30 minutes, with a stop of 5 minutes in between. After the ball milling, wash the samples in the ball mill tank with water, centrifuge and wash twice with ethanol, dry in a vacuum oven at 80°C for 12 hours, and put the powder into a magnetic boat after simple grinding, and heat it in a tube furnace. Nitrogen or argon protection is required, the heating temperature is 950°C, the heating rate is 5°C / min, the pyrolysis is 3h, and the black Fe-N-C single-atom catalyst is obtained.

Embodiment 3

[0038] Add 81 milligrams (mg) of zinc oxide, 289 mg of 2-ethylimidazole, 10 mg of ammonium sulfate, and 31 mg of iron porphyrin into an 80 mL ball mill jar, mix well, then add 200 μL of N,N-diethylformamide, and mix 20 Put the zirconia balls with a diameter of 10mm into the ball milling pot, install the ball milling pot on the ball mill, adjust the ball milling condition to 50 Hz, and ball mill twice, each time for 30 minutes, with a stop of 5 minutes in between. After the ball milling, wash the samples in the ball mill tank with water, centrifuge and wash twice with ethanol, dry in a vacuum oven at 80°C for 12 hours, and put the powder into a magnetic boat after simple grinding, and heat it in a tube furnace. Nitrogen or argon protection is required, the heating temperature is 950°C, the heating rate is 5°C / min, the pyrolysis is 3h, and the black Fe-N-C single-atom catalyst is obtained.

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Abstract

The invention provides a ball-milling assisted method for preparing a carbon nitrogen based monatomic iron catalyst. The method comprises the following steps: adopting a one-pot process for wrapping ferriporphyrin in a metallic organic frame hole in a monomolecular form through mechanical ball milling, thereby forming a subject-object structure; forming a nitrogen-doped porous carbon carrier by ametallic organic frame object and keeping an original porous structure, through the high-temperature pyrolytic reaction under the inert gas atmosphere; and forming a monatomic Fe-Nx structure by the ferriporphyrin molecules and fixing in the hole structure. The invention adopts a mechanical ball-milling assisted method for compounding a nanometer compound precursor; only an infinitesimal organic solvent participates in the process; the method is simple and convenient, safe, green and environment-friendly, and suitable for large-scale production; the acquired carbon nitrogen based monatomic iron catalyst has ultrahigh electrocatalytic activity and stability for the oxygen reduction reaction under an alkaline condition, and has a bright market prospect.

Description

technical field [0001] The invention relates to a preparation method of a carbon-nitrogen-based metal single-atom catalyst, in particular to a method for preparing a single-atom iron catalyst with the aid of ball milling without solvent participation, and belongs to the technical field of single-atom catalysts. Background technique [0002] The electrochemical oxygen reduction reaction plays an important role in the storage and conversion of renewable energy sources such as fuel cells and zinc-air batteries. Slow kinetics of oxygen reduction reactions require catalysts. Platinum and its alloy catalysts have high catalytic activity and energy efficiency, and are considered to be the best oxygen reduction catalysts. However, platinum is expensive, sensitive to methanol and CO, and has poor stability, which limits its application. Therefore, the development of non-precious metal catalysts with high activity, low cost and good stability is the key to solve the problem. Transi...

Claims

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Application Information

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IPC IPC(8): H01M4/88H01M4/90B02C17/10
CPCB02C17/10H01M4/8825H01M4/9041H01M4/9083Y02E60/50
Inventor 魏玮石晓蒙
Owner CAPITAL NORMAL UNIVERSITY
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