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Nitrogen-doped carbon fiber loaded zirconium induced transition metal phosphide and preparation method thereof

A nitrogen-doped carbon fiber, transition metal technology, applied in the electrolysis process, electrodes, electrolysis components, etc., can solve problems such as unfavorable commercial application of catalysts

Active Publication Date: 2021-04-06
SHAANXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The supported catalysts reported at this stage often use relatively expensive carbon materials such as graphene oxide and carbon nanotubes, which is not conducive to the commercial application of catalysts.

Method used

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  • Nitrogen-doped carbon fiber loaded zirconium induced transition metal phosphide and preparation method thereof
  • Nitrogen-doped carbon fiber loaded zirconium induced transition metal phosphide and preparation method thereof
  • Nitrogen-doped carbon fiber loaded zirconium induced transition metal phosphide and preparation method thereof

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preparation example Construction

[0029] The present invention is a preparation method of transition metal phosphide oxygen evolution electrocatalyst induced by nitrogen-doped biomass carbon fiber loaded with zirconium, which specifically comprises the following steps:

[0030] Step 1: Add 0.5mL of pyrrole monomer to 100mL of 1mg / mL bacterial cellulose suspension, add 1330mg of p-toluenesulfonic acid as a dopant, transfer the above mixed liquid to an ice-water bath at 1-4°C, 1946mg Ferric chloride was dissolved in 60mL of deionized water, and slowly added to the reaction system, and reacted for 4 to 8 hours. The membrane product was obtained by suction filtration, washed and dried.

[0031] Ferric chloride was used as an initiator to induce the in-situ polymerization of pyrrole monomers on the surface of bacterial cellulose to form Ppy (polypyrrole) / BC (bacterial cellulose) materials.

[0032] Step 2: Put the dried material in step 1 in a tube furnace, raise the temperature to 250-300°C at 1-3°C / min, and keep...

Embodiment 1

[0037]Step 1) Add 0.5mL of pyrrole monomer to 100mL of 1mg / mL bacterial cellulose suspension, add 1330mg of p-toluenesulfonic acid as a dopant, transfer the above mixed liquid to an ice-water bath at 1°C, and dissolve 1946mg of ferric chloride in 60mL deionized water, and slowly added to the reaction system, reacted for 6h. Suction filter to form a film, wash and dry.

[0038] Step 2) Put the dried material in step 1) in a tube furnace, raise the temperature to 300°C at 2°C / min, keep it for 1h, then raise the temperature to 800°C at 5°C / min, and keep it for 2h. The obtained carbon fibers were ground into powders, ultrasonically cleaned with 10% hydrochloric acid, washed and dried.

[0039] Step 3) Take 40 mg of the obtained nitrogen-doped carbon fiber and ultrasonically disperse it in 45 ml of ethanol, add 0.6 mmol of cobalt chloride, 0.3 mmol of ferric chloride and 0.1 mmol of zirconium chloride into the carbon fiber dispersion, stir for 30 minutes, and slowly add 2.5 mL of ...

Embodiment 2

[0046] Step 1) Add 0.5 mL of pyrrole monomer to 100 mL of 1 mg / mL bacterial cellulose suspension, add 1330 mg of p-toluenesulfonic acid as a dopant, transfer the above mixed liquid to 2 °C ice water bath, and dissolve 1946 mg of ferric chloride in 60mL deionized water, and slowly added to the reaction system, reacted for 4h. Suction filter to form a film, wash and dry.

[0047] Step 2) Place the dried material in step 1) in a tube furnace, raise the temperature to 250°C at 3°C / min, keep it for 1h, then raise the temperature to 600°C at 5°C / min, and keep it for 3h. The obtained carbon fibers were ground into powders, ultrasonically cleaned with 12% hydrochloric acid, washed and dried.

[0048] Step 3) Take 40 mg of the obtained nitrogen-doped carbon fiber and ultrasonically disperse it in 45 ml of ethanol, add 0.63 mmol of cobalt chloride, 0.32 mmol of ferric chloride and 0.05 mmol of zirconium chloride into the carbon fiber dispersion, stir for 30 minutes, and slowly add 2.5 ...

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Abstract

The invention relates to a nitrogen-doped carbon fiber-loaded zirconium-induced transition metal phosphide and a preparation method, the method comprises the following steps: carbonizing polypyrrole polymerized in situ on the surface of bacterial cellulose, washing the obtained product with hydrochloric acid and distilled water in sequence, and drying; dispersing the nitrogen-doped carbon fiber into ethanol, adding cobalt chloride, ferric chloride, zirconium chloride and monobutylamine into the dispersion liquid, and uniformly mixing; and then carrying out hydrothermal treatment on the precursor solution at 140-180 DEG C, centrifuging the obtained reaction solution, sequentially washing and drying, carrying out pre-oxidation treatment on the obtained compound, and carrying out phosphating treatment on the pre-oxidized compound and sodium hypophosphite at 300-400 DEG C to obtain the nitrogen-doped carbon fiber loaded zirconium induced transition metal phosphide. The obtained transition metal phosphide oxygen evolution electrocatalyst is good in catalytic activity and low in price, can be used for water electrolysis anode reaction, and has the advantages of being good in electrical conductivity, high in electrochemical specific surface area and multiple in exposed active sites.

Description

technical field [0001] The invention belongs to the field of energy materials, in particular to a nitrogen-doped carbon fiber supported zirconium-induced transition metal phosphide and a preparation method thereof. Background technique [0002] As a new type of clean energy, hydrogen is expected to achieve clean production and sustainable supply, which can be used to replace traditional fossil energy and solve energy crisis and environmental problems. Among the many ways to produce hydrogen, electrolysis of water is the most promising one. Water electrolysis involves oxygen evolution at the anode and hydrogen evolution at the cathode. Among them, the oxygen evolution reaction involves a four-electron transfer process, which has serious kinetic retardation and often requires a large potential to drive. Therefore, it is necessary to prepare efficient catalysts to reduce the overpotential required for the reaction. [0003] At present, the commonly used electrocatalysts for ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C25B11/04C25B1/04
CPCC25B1/04C25B11/04Y02E60/36
Inventor 张素风魏宁姚雪姚紫洁呼旭旭周秋生
Owner SHAANXI UNIV OF SCI & TECH