Preparation method of fluffy porous nitrogen-doped oxygen reduction catalyst

A nitrogen-doped carbon and catalyst technology, applied in chemical instruments and methods, physical/chemical process catalysts, chemical/physical processes, etc., can solve the problems of general performance of oxygen reduction catalysts, various raw materials, and inability to meet the requirements of oxygen reduction catalysts, etc. , to achieve excellent resistance to methanol and carbon monoxide poisoning, increase specific surface area and pore volume, and excellent oxygen reduction catalytic performance

Inactive Publication Date: 2017-10-24
HENAN NORMAL UNIV
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  • Summary
  • Abstract
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  • Claims
  • Application Information

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Problems solved by technology

[0003] At present, the patent whose publication number is CN104258892A discloses a kind of SiO synthesized by sol-gel hydrothermal method 2 As a hard template, a hierarchical porous carbon block material is prepared by nano-casting method, and then a nitrogen source (urea, etc.) is added to prepare a nitrogen-doped mesoporous/macroporous hierarchical carbon-oxygen reduction catalyst. Although the specific surface area of ​​the nitrogen-doped carbon-oxygen reduction catalyst is as high as 1570-2480m 2 g -1 , with large pores connected in three dimensions, but this method is complicated and difficult to operate
The patent with the publication number CN105186010A discloses a method for preparing a solid-phase polymer using a eutectic salt as a template, and the

Method used

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  • Preparation method of fluffy porous nitrogen-doped oxygen reduction catalyst
  • Preparation method of fluffy porous nitrogen-doped oxygen reduction catalyst
  • Preparation method of fluffy porous nitrogen-doped oxygen reduction catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] (1) Put 1.1g of glucose, 3.3g of zinc chloride, 1.1g of basic magnesium carbonate pentahydrate and 0.297g of urea in a glass mortar and grind for 10 minutes to mix them well to obtain material A1;

[0027] (2) Transfer material A1 to a porcelain boat and place it in a tube furnace. Under the protection of nitrogen gas with a flow rate of 100mL / min, the temperature was raised from room temperature to 300°C for 60 minutes, kept at 300°C for 120 minutes, and then heated at 10°C / min. The heating rate of min was raised to 900°C for 120 minutes, and then the temperature was naturally lowered to room temperature to obtain material B1;

[0028] (3) Transfer material B1 to a 100mL beaker and add 80mL of hydrochloric acid solution with a molar concentration of 2mol / L to soak for 18h, then wash with high-purity water until the filtrate is neutral, and then dry in a blast drying oven at 40°C for 12h to obtain fluffy and porous Nitrogen-doped carbon-oxygen reduction catalyst C1.

Embodiment 2

[0030] (1) Put 1.1g of glucose, 3.3g of zinc chloride, 1.1g of basic magnesium carbonate pentahydrate and 0.594g of urea in a glass mortar and grind for 10 minutes to mix them well to obtain material A2;

[0031] (2) Transfer material A2 to a porcelain boat and place it in a tube furnace. Under the protection of nitrogen gas with a flow rate of 100mL / min, the temperature was raised from room temperature to 300°C for 60 minutes, kept at 300°C for 120 minutes, and then heated at 10°C / min. The heating rate of min was raised to 900°C for 120 minutes, and then the temperature was naturally lowered to room temperature to obtain material B2;

[0032] (3) Transfer material B2 to a 100mL beaker and add 80mL of hydrochloric acid solution with a molar concentration of 2mol / L to soak for 18h, then wash with high-purity water until the filtrate is neutral, and then dry in a blast drying oven at 40°C for 12h to obtain fluffy and porous Nitrogen-doped carbon-oxygen reduction catalyst C2.

Embodiment 3

[0034] (1) Put 1.1g of glucose, 3.3g of zinc chloride, 1.1g of basic magnesium carbonate pentahydrate and 1.16g of urea in a glass mortar and grind for 10 minutes to mix them well to obtain material A3;

[0035] (2) Transfer material A3 to a porcelain boat and place it in a tube furnace. Under the protection of nitrogen gas with a flow rate of 100mL / min, the temperature was raised from room temperature to 300°C for 60 minutes, kept at 300°C for 120 minutes, and then heated at 10°C / min. The heating rate of min was raised to 900°C for 120 minutes, and then the temperature was naturally lowered to room temperature to obtain material B3;

[0036] (3) Transfer material B3 to a 100mL beaker and add 80mL of hydrochloric acid solution with a molar concentration of 2mol / L to soak for 18h, then wash with high-purity water until the filtrate is neutral, and then dry in a blast drying oven at 40°C for 24h to obtain fluffy and porous Nitrogen-doped carbon-oxygen reduction catalyst C3.

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Abstract

The invention discloses a preparation method of a fluffy porous nitrogen-doped oxygen reduction catalyst, belonging to the technical field of synthesis of porous carbon materials. According to the key point of the technical scheme of the invention, the preparation method comprises the following steps: putting a carbon source, a nitrogen source, zinc chloride and a pentahydrate basic magnesium carbonate into a glass mortar, grinding for 10-20 minutes until the materials are uniformly stirred so as to obtain a material A, transferring the material A into a ceramic boat, putting the ceramic boat into a tubular furnace, heating to 800-1000 DEG C under the protection of inert gas, standing for 120 minutes, and naturally cooling to the room temperature, so as to obtain a material B; and transferring the material B into a container, adding an acidic solution, soaking for 18 hours, washing with high-purity water until filtrate is neutral, and drying at 40-60 DEG C for 12-24 hours, so as to obtain the fluffy porous nitrogen-doped oxygen reduction catalyst. The specific surface area of the prepared fluffy porous nitrogen-doped oxygen reduction catalyst is 1346m<2>/g-1976m<2>/g, the hole diameter is about 3.8nm, and the fluffy porous nitrogen-doped oxygen reduction catalyst has excellent oxygen reduction catalytic performance and is capable of resisting methanol and carbon monoxide poisoning.

Description

technical field [0001] The invention belongs to the technical field of synthesis of porous carbon materials, and in particular relates to a preparation method of a fluffy porous nitrogen-doped carbon-oxygen reduction catalyst. Background technique [0002] Porous carbon material has become a typical fuel cell cathode oxygen reduction reaction catalyst due to its high specific surface area, rich pore structure and good electrical conductivity. Doping heteroatoms into carbon materials can effectively improve the surface structure of carbon materials, improve the surface wettability of carbon materials, and enhance the capacitance and catalytic properties of carbon materials (Peng, H.; Ma, G.; Sun, K.; et al. Electrochim. Acta 2016, 190, 862-871.). Nitrogen atoms doped into carbon materials exist in the following ways: pyridinic nitrogen, pyrrole nitrogen, graphite nitrogen and oxide nitrogen. The nature of the active sites for nitrogen-doped carbon materials to catalyze the ...

Claims

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Application Information

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IPC IPC(8): B01J27/24H01M4/90
CPCB01J27/24B01J35/0033B01J35/1028B01J35/1061H01M4/9083Y02E60/50
Inventor 高书燕李小阁魏献军
Owner HENAN NORMAL UNIV
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