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Iron-tin alloy-supported sulfur-nitrogen co-doped carbon electrocatalyst and preparation method

A technology of iron-tin alloy and electrocatalyst, which is applied in fuel cell-type half-cells and secondary battery-type half-cells, circuits, electrical components, etc., to achieve improved stability, high open circuit potential, and uniform distribution of active sites Effect

Active Publication Date: 2022-02-11
EAST CHINA NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Despite great efforts, reducing the noble metal content to enhance the electrocatalytic activity remains a major challenge due to the limitations of noble metals.

Method used

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  • Iron-tin alloy-supported sulfur-nitrogen co-doped carbon electrocatalyst and preparation method
  • Iron-tin alloy-supported sulfur-nitrogen co-doped carbon electrocatalyst and preparation method
  • Iron-tin alloy-supported sulfur-nitrogen co-doped carbon electrocatalyst and preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] a. Preparation of 5,10,15,20-tetra(nitro)phenylporphyrin

[0032] Add 0.1 mole of p-nitrobenzaldehyde to 100 mL of boiling propionic acid (analytically pure) and stir for 30 min, add dropwise 10 mL of propionic acid containing 0.2 mole of pyrrole, reflux for 1 h at a temperature of 130 ° C, and use the filtered product after the reaction Wash thoroughly with deionized water and dry under vacuum. Afterwards, reflux washing with pyridine, cooling overnight, suction filtration, washing with acetone (analytical pure) until the filtrate is colorless, and after vacuum drying, it is 5,10,15,20-tetrakis(nitro)phenylporphyrin (TNPP).

[0033] b. Preparation of doped Sn(OH) x 5,10,15,20-tetra(amino)phenylporphyrin

[0034] Under the protection of nitrogen, take 0.1 mole of 5,10,15,20-tetra(nitro)phenylporphyrin synthesized above and dissolve 0.8 mole of SnCl in 100 mL of concentrated hydrochloric acid (analytical pure) 2 2H 2 O dissolved in 25mL of concentrated hydrochloric a...

Embodiment 2

[0043] a. Preparation of 5,10,15,20-tetra(nitro)phenylporphyrin

[0044] Add 0.1 mole of p-nitrobenzaldehyde into 120 mL of boiling propionic acid and stir for 30 min, add dropwise 10 mL of propionic acid containing 0.3 mole of pyrrole, and reflux at 130°C for 1 h. Wash and dry in vacuo. Afterwards, reflux washing with pyridine, cooling overnight, suction filtration, washing with acetone (analytical pure) until the filtrate is colorless, and after vacuum drying, it is 5,10,15,20-tetrakis(nitro)phenylporphyrin (TNPP).

[0045] b. Preparation of doped Sn(OH) x 5,10,15,20-tetra(amino)phenylporphyrin

[0046] Under the protection of nitrogen, take the 0.1 mole doped Sn(OH) prepared above x 5,10,15,20-tetra(amino)phenylporphyrin and 0.9 mole SnCl 2 2H 2 O mixed, dissolved with concentrated hydrochloric acid (analytically pure), stirred at room temperature for 2.5 hours, heated to 70°C, reacted for 30 minutes, cooled in an ice-water bath after the reaction, poured 100 ml of dei...

Embodiment 3

[0053] Preparation of a.5,10,15,20-tetra(nitro)phenylporphyrin

[0054] Add 0.1 mole of p-nitrobenzaldehyde into 150 mL of boiling propionic acid and stir for 30 min, add dropwise 10 mL of propionic acid containing 0.3 mole of pyrrole, and reflux at 130°C for 1 h. Wash and dry in vacuo. Afterwards, reflux washing with pyridine, cooling overnight, suction filtration, washing with acetone (analytical pure) until the filtrate is colorless, and after vacuum drying, it is 5,10,15,20-tetrakis(nitro)phenylporphyrin (TNPP).

[0055] b. Doping Sn(OH) x Preparation of 5,10,15,20-tetra(amino)phenylporphyrin

[0056] Under the protection of nitrogen, take 0.1 mole of 5,10,15,20-tetra(nitro)phenylporphyrin synthesized above and dissolve 1.0 mole of SnCl in 100 mL of concentrated hydrochloric acid (analytical pure) 2 2H 2 O dissolved in 25mL of concentrated hydrochloric acid (analytical pure) was added dropwise to the above system, stirred at room temperature for 2.5h, heated to 70°C, a...

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Abstract

The invention discloses a sulfur-nitrogen co-doped carbon electrocatalyst supported by an iron-tin alloy and a preparation method thereof, belonging to the field of preparation of battery cathode oxygen reduction catalysts. The present invention uses doped Sn(OH) x 5,10,15,20-tetra(amino)phenylporphyrin and 2,6-diformaldehyde pyridine at 60°C under nitrogen protection, glacial acetic acid (analytical pure) as catalyst, anhydrous FeCl 3 As a metal source, a covalent organic polymer supported by Sn‑Fe was synthesized, and after high temperature pyrolysis, FeSn 2 Alloy supported carbon materials. This novel iron-tin alloy-supported carbon-based electrocatalyst with a double-shell structure has a two-dimensional porous structure. It adopts a metal-iron-promoted P-zone non-metallic tin catalytic strategy, and the metal oxide interlayer provides good transport and transfer of charges in the system. The channel accelerates the mass transfer process, thus providing a new idea for the development of P-zone non-noble metal oxygen reduction electrocatalysts. The preparation process is simple and easy, and it is easy to realize large-scale industrial applications.

Description

technical field [0001] The invention relates to the technical field of battery cathode oxygen reduction catalysts, in particular to iron-tin alloy nanoparticles with double-shell structure derived from covalent porphyrin-based skeletons loaded with sulfur and nitrogen co-doped carbon electrocatalytic materials, that is, iron-tin alloy-loaded sulfur Nitrogen co-doped carbon electrocatalyst and preparation method thereof. Background technique [0002] In order to efficiently solve the growing contradiction between economic development and energy shortage and environmental pollution, it has become a very urgent task to develop clean, efficient, and renewable energy storage and conversion technologies (such as proton exchange membrane fuel cells, zinc-air batteries). Due to the slow rate of the oxygen reduction reaction at the cathode of the battery, the power output of the fuel cell is limited, which hinders the large-scale commercial application of this type of battery. There...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M4/90H01M12/08B82Y30/00
CPCH01M4/9041H01M4/9083H01M4/9016H01M12/08B82Y30/00Y02E60/10
Inventor 孔爱国张笑颖乔雨李瑞婧刘佳新刘璐瑶邢力丹
Owner EAST CHINA NORMAL UNIV
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