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A kind of preparation method of high specific surface area porous carbon doped iridium electrolysis water oxygen evolution catalyst

A high specific surface area, porous carbon technology, applied in electrolytic components, electrolytic process, electrodes, etc., can solve the problems of large particle size, interpenetration, long reaction cycle, etc.

Active Publication Date: 2020-01-17
SHANGHAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, MOF-5 materials prepared by traditional methods often have disadvantages such as poor crystallinity, large particle size, serious interpenetration phenomenon, and long reaction cycle.

Method used

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  • A kind of preparation method of high specific surface area porous carbon doped iridium electrolysis water oxygen evolution catalyst
  • A kind of preparation method of high specific surface area porous carbon doped iridium electrolysis water oxygen evolution catalyst
  • A kind of preparation method of high specific surface area porous carbon doped iridium electrolysis water oxygen evolution catalyst

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] 1. Take 10g of 5A dehydration molecular sieves and sinter at 400°C for 12 hours, then add 500mL of N,N-dimethylformamide (DMF) solvent to dewater for 24 hours before use.

[0027] 2. Take 0.8939g zinc nitrate hexahydrate [Zn(NO 3 ) 2 ·6H 2 O] and 1.8913g trimesic acid (H 3 BDC) was dissolved in 80 mL of N,N-dimethylformamide (DMF), then 0.0111 g of polyvinylpyrrolidone (PVP) was added, stirred vigorously to dissolve, and 6 µL of hydrogen peroxide (H 2 o 2 , 30%), after stirring slowly, the precursor solution was obtained.

[0028] 3. Heat the precursor solution obtained in 2 in a 100ml autoclave at 100°C for 5 hours to obtain white MOF-5 crystals. See attached figure 1 , figure 1 a is the XRD pattern of MOF-5, the abscissa is the diffraction angle 2θ, the unit is degree (°), and the ordinate is the diffraction intensity. Typical MOF-5 characteristic peaks can be seen in the figure; see the attached figure 2 , figure 2 This is the scanning electron microscope ...

Embodiment 2

[0038] 1. Take 10g of 5A dewatering molecular sieves and sinter at 400°C for 12 hours, then add 500mL of N-methylpyrrolidone (NMP) solvent to dewater for 24 hours before use.

[0039] 2. Take 0.8939g zinc nitrate hexahydrate [Zn(NO 3 ) 2 ·6H 2 O] and 1.8913g trimesic acid (H 3 BDC) was dissolved in 80mL of NMP solvent, then added 0.0111g polyvinylpyrrolidone (PVP), stirred vigorously to dissolve, and slowly added 6µL hydrogen peroxide (H 2 o 2 , 30%), stirred slowly and fully dissolved to obtain the precursor solution.

[0040] 3. Heat the precursor solution obtained in 2 in a 100ml autoclave at 140°C for 5 hours to obtain white MOF-5 crystals.

[0041] 4. Get 2g of MOF-5 prepared in 3 and iridium chloride (IrCl 3 ) 2g was added into 100ml of NMP solvent and soaked for 48 hours, washed with corresponding solvent after centrifugation, repeated 3 times, and vacuum dried at 150°C for 2 hours to obtain HAPC / Ir precursor.

[0042] 5. The dried HAPC / Ir precursor in 4 was sint...

Embodiment 3

[0050] 1. Take 10g of 5A dewatering molecular sieves and sinter at 400°C for 12 hours, then add 500mL of N,N-diethylacetamide (DEF) solution to dewater for 24 hours before use.

[0051] 2. Take 0.8939g zinc nitrate hexahydrate [Zn(NO 3 ) 2 ·6H 2 O] and 1.8913g trimesic acid (H 3 BDC) was dissolved in 180mL of DEF, then 0.0111g of polyvinylpyrrolidone (PVP) was added, stirred vigorously to dissolve, and 120µL of hydrogen peroxide (H 2 o 2 , 30%) and stirred slowly to obtain the precursor solution.

[0052] 3. Heat the precursor solution obtained in 2 in a 200ml autoclave at 140°C for 24 hours to obtain white MOF-5 crystals. MOF-5 was tested by X-ray diffraction (XRD), the abscissa is the diffraction angle 2θ, the unit is degree (°), and the ordinate is the diffraction intensity; typical MOF-5 characteristic peaks can be seen in the XRD diagram; MOF-5 In the scanning electron microscope image, smooth cubic particles can be seen, the particle size is about 8 μm, and the pre...

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Abstract

The invention provides a preparation method of a high specific surface area porous carbon doped iridium (HAPC / Ir) catalyst for water electrolysis for generating hydrogen, and belongs to the technicalfields of chemical power supply and new materials. According to the preparation method, MOF-5 is taken as the template, and the prepared material is applied to electrode materials. Through an impregnation method, iridium ions are merged to an organic frame made of MOF-5 through impregnation to obtain a precursor, and finally the precursor is made into the high specific surface area porous carbon doped iridium (HAPC / Ir) catalyst. The method and operation are simple, the equipment requirements are low, and high specific surface area porous carbon materials can be prepared massively. The technical process has the characteristics that the corrosion resistant performance of a positive electrode catalyst for water hydrolysis is enhanced in acidic electrolyte, and moreover, the stability of the catalyst is improved. Furthermore, the raw material (HAPC / Ir) is mild, nontoxic and safe, the resources of part materials are wide, and the industrial prospect is good.

Description

technical field [0001] The invention discloses a method for preparing a large amount of high specific surface area porous carbon-doped iridium (HAPC / Ir) with a simple method, and using it as an anode material for electrolysis of water to construct high specific surface area, high active sites and low iridium loading anode catalyst material for water electrolysis. Background technique [0002] Hydrogen energy has attracted widespread attention as the clean energy that is most likely to replace fossil energy in the world today. Proton exchange membrane water electrolysis device is an efficient, pollution-free and environmentally friendly way to produce hydrogen. Among them, the oxygen evolution reaction (OER) is an important catalytic process for water electrolysis. However, the OER reaction requires a large overpotential to obtain a sufficient reaction current for practical applications. The rational design of electrocatalysts to accelerate OER kinetics has been the core of ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C25B11/06C25B1/04
CPCC25B1/04C25B11/093Y02E60/36
Inventor 曹文娟赵宏滨方建慧徐甲强张久俊
Owner SHANGHAI UNIV
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