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Preparation method of porous nitrogen and phosphorus dual-doped carbon oxygen reduction catalyst

A dual-doping and catalyst technology, applied in chemical instruments and methods, physical/chemical process catalysts, chemical/physical processes, etc., can solve the problems of lengthy implementation procedures and insufficient catalytic activity of oxygen reduction, and achieve excellent resistance to methanol interference and carbon monoxide poisoning performance, excellent oxygen reduction catalytic performance, and enhanced electrochemical performance

Inactive Publication Date: 2018-02-02
HENAN NORMAL UNIV
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  • Abstract
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  • Claims
  • Application Information

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Problems solved by technology

The patent with the publication number CN106807427A discloses a metal-embedded composite material prepared with agar as the carbon source, ethylenediaminetetramethylphosphoric acid (EDTMPA) as the nitrogen source and phosphorus source, and transition metal salt as the precursor and pore-forming agent. Nitrogen-phosphorous double-doped carbon material method, however, the implementation procedure of this method is quite lengthy, and the catalytic activity of oxygen reduction is not outstanding enough

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  • Preparation method of porous nitrogen and phosphorus dual-doped carbon oxygen reduction catalyst
  • Preparation method of porous nitrogen and phosphorus dual-doped carbon oxygen reduction catalyst
  • Preparation method of porous nitrogen and phosphorus dual-doped carbon oxygen reduction catalyst

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Embodiment 1

[0027] (1) Put 3g of dry and clean biomass precursor white jade mushroom and 30mL of ultrapure water in an autoclave for hydrothermal reaction at 180°C for 24 hours. Dry at 80°C for 10 hours in a blast drying oven to obtain material A;

[0028] (2) Aqueous ammonia solution (0.011mol NH 3 ·H 2 O) Add dropwise to zinc chloride aqueous solution (0.022mol ZnCl 2 ) to obtain a mixed double activator solution B1 containing both zinc hydroxide and zinc chloride, immerse 1g of material A in the mixed double activator solution B1 and mix evenly, then place it in a blast drying oven at 105°C Drying for 10 hours to obtain material C1, that is, to complete the carbonization pretreatment process;

[0029] (3) Transfer the material C1 to a porcelain boat and place it in a tube furnace. Under the protection of nitrogen gas with a flow rate of 100mL / min, raise the temperature from room temperature to 300°C for 2h after 60min, and then increase the temperature at a rate of 10°C / min. Raise ...

Embodiment 2

[0032] (1) Ammonia solution (0.022mol NH 3 ·H 2 O) Add dropwise to zinc chloride aqueous solution (0.022mol ZnCl 2 ) to obtain a mixed double activator solution B2 containing both zinc hydroxide and zinc chloride, immerse 1g of material A in the mixed double activator solution B2 and mix evenly, then place it in a blast drying oven at 105°C Drying for 10 hours to obtain material C2, that is, the carbonization pretreatment process is completed;

[0033] (2) Transfer the material C2 to a porcelain boat and place it in a tube furnace. Under the protection of nitrogen gas with a flow rate of 100mL / min, raise the temperature from room temperature to 300°C for 2h after 60min, and then increase the temperature at a rate of 10°C / min. Raise the temperature to 900°C for 2 hours, then naturally cool down to room temperature to obtain material D2;

[0034] (3) Transfer the material D2 to a reaction vessel and add 100mL of hydrochloric acid solution with a molar concentration of 2mol / L ...

Embodiment 3

[0036] (1) Ammonia solution (0.033mol NH 3 ·H 2 O) Add dropwise to zinc chloride aqueous solution (0.022mol ZnCl 2 ) to obtain a mixed double activator solution B3 containing both zinc hydroxide and zinc chloride, immerse 1g of material A in the mixed double activator solution B3 and mix evenly, then place it in a blast drying oven at 105°C Drying for 10 hours to obtain material C3, that is, the carbonization pretreatment process is completed;

[0037] (2) Transfer the material C3 to a porcelain boat and place it in a tube furnace. Under the protection of nitrogen gas with a flow rate of 100mL / min, raise the temperature from room temperature to 300°C for 2h after 60min, and then increase the temperature at a rate of 10°C / min. Raise the temperature to 900°C for 2 hours, then naturally cool down to room temperature to obtain material D3;

[0038] (3) Transfer the material D3 to a reaction vessel and add 100mL of hydrochloric acid solution with a molar concentration of 2mol / L ...

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Abstract

The invention discloses a preparation method of porous nitrogen and phosphorus dual-doped carbon oxygen reduction catalyst, which includes steps of performing hydrothermal reaction on white beech mushroom and ultrapure water for 24 hours at 180 DEG C; cooling to room temperature and then drying product slurry to obtain a material A; dropwise adding ammonium hydroxide solution in zinc chloride solution to obtain mixed dual-activator solution B; immersing the material A in the mixed dual-activator solution B and mixing evenly; drying to obtain a material C; heating the material C from the room temperature to 300 DEG C for 60 min and keeping the material for 2 hours; then raising temperature to 700-1000 DEG C at the heating rate of 10 DEG C / min and keeping for 2 hours; cooling to room temperature to obtain a material D; adding the material D in acid solution and immersing for 12 hours; washing the material D by high purity water until the filter fluid is neutral; drying the material for 6hours at 105 DEG C to obtain the porous nitrogen and phosphorus dual-doped carbon oxygen reduction catalyst. the specific area of the porous nitrogen and phosphorus dual-doped carbon oxygen reductioncatalyst prepared by the invention is 1075.311 m2 / g; the average porous diameter is 2.587 nm; the porous nitrogen and phosphorus dual-doped carbon oxygen reduction catalyst has excellent oxygen reduction catalytic performance, methyl alcohol disturbance resistance and carbon monoxide poisoning resistance.

Description

technical field [0001] The invention belongs to the technical field of synthesis of porous heteroatom-doped carbon materials, and in particular relates to a preparation method of a porous nitrogen-phosphorus double-doped carbon-oxygen reduction catalyst. Background technique [0002] Heteroatom-doped carbon materials are favored by many researchers because of their low cost, high catalytic activity for oxygen reduction, strong resistance to methanol interference, and good long-term stability. Single heteroatom metal-free carbon-based catalysts were the first to attract people's attention. Since Dai Liming et al. reported that nitrogen-doped carbon nanotubes have excellent oxygen reduction catalytic activity in 2009, nitrogen-doped carbon materials have become the most studied single-atom-doped carbon so far. In addition, other single heteroatom (B, S, P, and F) doped carbon materials have also been gradually prepared and studied. In recent years, after single-atom doping h...

Claims

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Application Information

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IPC IPC(8): B01J27/24B01J35/10
CPCB01J27/24B01J35/33B01J35/617B01J35/647
Inventor 高书燕赵亚岭魏献军
Owner HENAN NORMAL UNIV
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