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The preparation method of orr catalyst

A catalyst and metal-organic framework technology, applied in the field of ORR catalyst preparation, can solve problems such as unsatisfactory results

Active Publication Date: 2021-05-18
TSINGHUA UNIV +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Among these ORR catalytic materials, metal-organic frameworks (MOFs) have been applied in proton conduction, electrocatalysis, etc. In the field, heteroatoms (B, N, S, P, etc.) prepared from metal-organic frameworks as precursors can enhance electrocatalytic activity after doping into carbon substrates or combining with metals / metal oxides, but the effects are not satisfactory.

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  • The preparation method of orr catalyst
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  • The preparation method of orr catalyst

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preparation example Construction

[0035] The technical scheme of the preparation method of the ORR catalyst of the present invention is as follows, comprising the following steps:

[0036] 1) Dissolve the cobalt salt and 2-(p-N-imidazolyl)phenyl-1H-4,5-imidazoledicarboxylic acid ligand in water and acetonitrile solvent, and add acid to adjust the pH value of the solution after ultrasonic and stirring 2 to 4, and then hydrothermal reaction occurs at a constant temperature of 140 to 155°C for 48 to 96 hours; after cooling to room temperature, the obtained product is washed in turn and dried naturally to form a black-green transparent cobalt-containing multi-nitrogen metal organic compound. Framework material precursor (chemical formula: [Co(p-IPhHIDC)]n);

[0037] 2) The precursor material [Co(p-IPhHIDC)] prepared in step 1) n , after being thoroughly ground, ultrasonically dispersed in chloroplatinic acid (H 2 PtCl 6 ·6H 2 O) in the ethylene glycol solution, this mixed solution is placed in the microwave sy...

Embodiment 1

[0044] 1. 0.05mmol, 11.9mg of CoCl 2 ·6H 2 O and 0.03 mmol, 8.9 mg of 2-(p-N-imidazolyl)phenyl-1H-4,5-imidazoledicarboxylic acid ligand (p-IPhH3IDC) were dissolved in 2 mL of acetonitrile and 5 mL of water, mixed well and added concentrated HCl Adjust the pH to 2, and conduct a hydrothermal reaction at 150°C for 96 hours; after the reaction, the product obtained is centrifuged, washed three times with acetone, washed three times with water, and dried naturally at room temperature to obtain a black-green transparent cobalt-containing multi-nitrogen metal-organic framework Material. figure 1 Shown is the XRD pattern of the resulting product.

[0045] 2. After the material obtained in step 1 and the ethylene glycol solution of chloroplatinic acid are in a molar ratio of 1:0.02 ultrasonically dispersed, in N 2 Place it in a microwave synthesizer at 113°C under protection, and react with 10s / 10s intermittent microwave for 16min to make H 2 PtCl 6 Restored to simple Pt; in orde...

Embodiment 2

[0051] 1. 0.05mmol, 11.9mg of CoCl 2 ·6H 2 O and 0.03 mmol, 8.9 mg of 2-(p-N-imidazolyl) phenyl-1H-4,5-imidazole dicarboxylic acid ligand (p-IPhH3IDC,) were dissolved in 2 mL of acetonitrile and 5 mL of water, mixed well and added to HCl was adjusted to pH 4, and hydrothermal reaction was carried out at 150°C for 96 hours; after the reaction, the product obtained was centrifuged, washed three times with acetone, and washed three times with water, and dried naturally at room temperature to obtain a black-green transparent cobalt-containing multi-nitrogen metal organic compound. Framework material (Co-MNMOF).

[0052] 2. After the precursor Co-MNMOF material and the ethylene glycol solution of chloroplatinic acid are dispersed uniformly by ultrasonic at a molar ratio of 1:0.05, the N 2 Place it in a microwave synthesizer at 113°C under protection, and react with 10s / 10s intermittent microwave for 16min to make H 2 PtCl 6 Restored to simple Pt; in order to prevent the metal (...

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Abstract

The invention provides a preparation method of an ORR catalyst. The preparation method of the ORR catalyst comprises the following steps: 1) making a precursor of a cobalt-containing polynitrogen metal-organic framework material; 2) dispersing the precursor in an ethylene glycol solution containing chloroplatinic acid, and performing microwave synthesis / extraction reaction , to prepare a cobalt polynitrogen metal organic framework material containing platinum participating in the post-coordination; 3) performing a calcination treatment on the cobalt polynitrogen metal organic framework material participating in the platinum post-coordination to obtain an ORR catalyst. Using Pt-enhanced multi-nitrogen imidazole carboxylic acid cobalt-based metal-organic framework materials to prepare electrocatalysts by redox, the operation process is simple; at the same time, the platinum content in the catalyst is reduced, and the prepared catalyst metal-organic framework has a microporous structure. It is helpful for the transmission of protons and gases, and the product has high catalytic performance.

Description

technical field [0001] The invention belongs to the technical field of oxidation-reduction electrocatalysis, and in particular relates to a preparation method of an ORR catalyst. Background technique [0002] Since the development of human civilization, material and spiritual civilization have been highly developed. As human society continues to develop at a high speed, the importance of energy is self-evident. With the continuous use of the three major ore energy sources, problems such as energy reserves, over-exploitation and environmental pollution have become more and more serious. Although every innovation and breakthrough in energy technology has had a huge impact on the development of productivity and social change, all these social advances today are built on the basis of extensive use of fossil fuels. Facing the demand for energy from global economic and population growth, the depletion of traditional energy sources, and the deteriorating human living environment, ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M4/92
CPCH01M4/921H01M4/926Y02E60/50
Inventor 梁茜王诚王海峰王利生
Owner TSINGHUA UNIV
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