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Preparation of iron-nitrogen co-doped porous carbon sphere electrocatalyst

An electrocatalyst and co-doping technology, applied in the fields of carbon materials and energy, can solve the problems of complex process and increased risk, and achieve the effect of wide application prospect, good sphericity and complete structure

Inactive Publication Date: 2021-02-09
TIANJIN POLYTECHNIC UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The Chinese invention patent application document with the application number 201510033461.3 discloses a method for preparing iron-nitrogen co-doped porous carbon sphere catalysts by template method using 2-aminopyridine as a monomer, ammonium persulfate and ferric chloride as oxidants, although The prepared material has a high specific surface area and excellent electrocatalytic performance for oxygen reduction. However, this preparation method uses porous silica as a template. After carbonization, it is necessary to remove the silica template with highly corrosive hydrofluoric acid. Complicates the process and increases the risk

Method used

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  • Preparation of iron-nitrogen co-doped porous carbon sphere electrocatalyst
  • Preparation of iron-nitrogen co-doped porous carbon sphere electrocatalyst
  • Preparation of iron-nitrogen co-doped porous carbon sphere electrocatalyst

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Preparation of iron-nitrogen co-doped spherical porous carbon materials:

[0029] Step 1) 1.07 g of 3,3'-diaminobenzidine was dissolved in 80 mL of ethanol, and the mixture was heated to 70°C.

[0030] Step 2) Add 10mL F127 ethanol solution (concentration is 10g / L), 10mL Fe(NO 3 ) 3 9H 2 O ethanol solution (0.025mol / L concentration) and 1.63g p-benzoquinone were stirred and refluxed at 70°C for 2 hours.

[0031] Step 3) After the reaction, the obtained brown product was filtered and washed with ethanol and water respectively until the solution was colorless, and dried at 120° C. to remove moisture to obtain polymer nanospheres.

[0032] Step 4) put the product of step 3) into the carbonization furnace, -1 The heating rate was increased to 900 °C. The atmosphere is a mixed gas of argon and ammonia, the flow rate ratio of which is 1:2 and kept for 2 hours, and the black powder target material is obtained after cooling down.

[0033] Electrocatalytic oxygen reduction...

Embodiment 2

[0039] Preparation of iron-nitrogen co-doped spherical porous carbon materials:

[0040] Step 1) 0.16 g of 3,3'-diaminobenzidine was dissolved in 60 mL of ethanol, and the mixture was heated to 90°C.

[0041] Step 2) Add 10mL F127 ethanol solution (concentration is 5g / L), 30mLFe(NO 3 ) 3 9H 2 O ethanol solution (0.0125 mol / L concentration) and 0.41 g p-benzoquinone were stirred and refluxed at 90° C. for 4 hours.

[0042] Step 3) After the reaction, the obtained brown product was filtered and washed with ethanol and water respectively until the solution was colorless, and dried at 80° C. to remove moisture to obtain polymer nanospheres.

[0043] Step 4) putting the product of step 3) into a carbonization furnace. at 2°C·min -1 The heating rate was increased to 800 °C. The atmosphere is a mixed gas of ammonia and argon with a flow rate ratio of 1:3 and kept for 3h. Obtain black powder target material after cooling down.

[0044] The electrocatalytic oxygen reduction tes...

Embodiment 3

[0046] Preparation of iron-nitrogen co-doped spherical porous carbon materials:

[0047] Step 1) 0.94 g of 3,3'-diaminobenzidine was dissolved in 70 mL of ethanol, and the mixture was heated to 80°C.

[0048] Step 2) Add 20mL F127 ethanol solution (concentration is 10g / L), 10mL Fe(NO 3 ) 3 9H 2 O ethanol solution (concentration: 0.0125mol / L) and 1.89g p-benzoquinone were stirred and refluxed for 3 hours at 80°C.

[0049] Step 3) After the reaction, the obtained brown product was filtered and washed with ethanol and water respectively until the solution was colorless, and dried at 100° C. to remove moisture to obtain polymer nanospheres.

[0050] Step 4) putting the product of step 3) into a carbonization furnace. at 3°C·min -1 The heating rate was increased to 1000 °C. The atmosphere is a mixed gas of ammonia and argon with a flow rate ratio of 1:1 and kept for 2h. Obtain black powder target material after cooling down.

[0051] The electrocatalytic oxygen reduction te...

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Abstract

The preparation method comprises the following steps: by taking 3, 3'-diaminobenzidine, p-benzoquinone, F127 and a metal iron salt as raw materials, synthesizing iron-nitrogen co-doped nanospheres through a simple quinone amine polymerization process, and pyrolyzing the iron-nitrogen co-doped nanospheres in an ammonia gas and argon mixed atmosphere to obtain an iron-nitrogen co-doped porous carbonsphere material, namely the iron-nitrogen co-doped porous carbon sphere material, wherein the material has excellent electrocatalytic oxygen reduction performance. The preparation method has the advantages that the preparation method is simple, low in cost and suitable for engineering amplification and large-scale preparation; the porous carbon spheres are good in sphericity degree, complete in structure, uniform in particle size, large in specific surface area and rich in pore structure, and exposure of catalytic active sites and adsorption of oxygen are facilitated; through co-doping of heteroatom nitrogen and transition metal iron, the electrocatalytic activity of the material can be effectively improved, and the material has important significance and value in the field of preparationof porous carbon electrocatalysts.

Description

technical field [0001] The invention belongs to the technical fields of carbon materials and energy, and in particular relates to the preparation of an iron-nitrogen co-doped porous carbon sphere electrocatalyst. Background technique [0002] The depletion of fossil energy is accelerating, and environmental problems are becoming more and more serious. The development of new clean energy has become an inevitable choice. New electrochemical energy storage and conversion devices such as fuel cells and metal-air batteries are considered to be one of the most promising technologies to solve the human energy crisis due to their high energy density, high energy efficiency, and environmental friendliness. However, there are still many problems in fuel cells and metal-air batteries, among which the slow oxygen reduction reaction (ORR) at the cathode is the main reason restricting their development. [0003] At present, the most common catalyst for catalyzing the oxygen reduction pro...

Claims

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Application Information

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IPC IPC(8): H01M4/96H01M4/90H01M4/88H01M12/06
CPCH01M4/96H01M4/90H01M4/8825H01M4/8892H01M12/06
Inventor 马昌王亚丽甘瑞辉史景利
Owner TIANJIN POLYTECHNIC UNIV
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