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Zinc-based metal organic framework material, preparation method of iron-nitrogen co-doped carbon-based oxygen reduction electrocatalyst and application

An organic framework and electrocatalyst technology, applied in circuits, electrical components, battery electrodes, etc., can solve the problems of less attention to use, and achieve the effects of simple and easy preparation method, wide source of raw materials, and low cost

Active Publication Date: 2019-12-03
SOUTHEAST UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the use of interpenetrating nonporous MOF complexes as pyrolytic precursors has so far received less attention compared to local studies on the use of porous MOFs in the preparation of carbon catalysts.

Method used

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  • Zinc-based metal organic framework material, preparation method of iron-nitrogen co-doped carbon-based oxygen reduction electrocatalyst and application
  • Zinc-based metal organic framework material, preparation method of iron-nitrogen co-doped carbon-based oxygen reduction electrocatalyst and application
  • Zinc-based metal organic framework material, preparation method of iron-nitrogen co-doped carbon-based oxygen reduction electrocatalyst and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Preparation of zinc-based metal-organic framework (Zn-TTPA):

[0041] The ligand TTPA-4 (13.4mg, 0.03mmol), terephthalic acid (10.0mg, 0.06mmol), zinc nitrate hexahydrate (17.8mg, 0.06mmol) were dissolved in 10mL of DMF and deionized water (V:V =1:1) in a mixed solvent, placed in a hydrothermal tank of tetrafluoroethylene and stirred evenly, heated to 100°C for 50 hours, slowly lowered to 15°C, collected the crystals formed, and used solvent for the crystals (N,N-di Methylformamide, water, ethanol) were washed successively, and dried at room temperature to obtain a zinc-based metal-organic framework material. The yield is about 65%.

[0042] figure 1 It is the structural diagram of the Zn-TTPA zinc-based metal organic framework material obtained in Example 1 of the present invention viewed along the c-axis direction. In Zn-TTPA, viewed along the c-axis direction, a quasi-hexagonal frame is formed on the Zn-TTPA frame shaped channel, the window size is approx.

[0...

Embodiment 2

[0046] Step 1, the preparation of precursor Fe-Zn-TTPA:

[0047] Ligand TTPA-4 (13.4mg, 0.03mmol), terephthalic acid (10.0mg, 0.06mmol), zinc nitrate hexahydrate (17.8mg, 0.06mmol), iron nitrate nonahydrate (1.01mg, 0.0025mmol) were added 10mL of DMF and deionized water (V:V=1:1) mixed solvent, heated to 100°C under stirring, stirred for 72 hours, slowly lowered to 15°C, filtered to obtain a powdery solid, the yield was about 67% .

[0048] Step 2. Preparation of iron-nitrogen co-doped carbon material

[0049] Put the powdery solid precursor Fe-Zn-TTPA material into a tube furnace, raise the temperature to 950°C at 5°C / min in a nitrogen atmosphere, keep at this temperature for 2h, and cool to room temperature at 5°C per minute, An iron-nitrogen co-doped carbon-based electrocatalyst for oxygen reduction was obtained.

[0050] image 3 It is the XRD spectrogram of the obtained zinc-based metal organic framework material Zn-TTPA and the precursor Fe-Zn-TTPA before carbonizati...

Embodiment 3

[0059] Step 1, the preparation of precursor Fe-Zn-TTPA:

[0060] Ligand TTPA-4 (17.9mg, 0.04mmol), terephthalic acid (11.7mg, 0.07mmol), zinc nitrate hexahydrate (20.8mg, 0.07mmol), iron nitrate nonahydrate (1.21mg, 0.003mmol) were added 20mL of DMF and deionized water (V:V=1:1) mixed solvent, heated to 95°C under stirring, stirred for 45 hours, slowly lowered to 30°C, filtered to obtain a powdery solid, the yield was about 64% .

[0061] Step 2. Preparation of iron-nitrogen co-doped carbon material

[0062] Put the powdery solid precursor Fe-Zn-TTPA material into a tube furnace, in an argon atmosphere, raise the temperature to 1100°C at 10°C / min, keep at this temperature for 2h, and cool to room temperature at 10°C per minute , to obtain iron-nitrogen co-doped carbon-based oxygen reduction electrocatalysts.

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Abstract

The invention discloses a zinc-based metal organic framework material, a preparation method of an iron-nitrogen co-doped carbon-based oxygen reduction electrocatalyst and an application. A catalyst ofthe invention is based on a newly designed zinc-based metal organic framework material, a precursor Fe-Zn-TTPA is prepared by a one-pot method on the basis of the zinc-based metal organic framework material, and the precursor Fe-Zn-TTPA is carbonized at a high temperature to obtain an iron-nitrogen-carbon-oxygen reduction electrocatalyst. The material is simple and easy to obtain, cost is low, and the prepared iron-nitrogen co-doped carbon-based oxygen reduction electrocatalyst is high in oxygen reduction catalytic activity, has good stability and methanol tolerance, can replace a noble metalPt / C catalyst as a catalytic material and can be applied to a fuel cell or a metal-air cell, and has a wide application prospect and practical value.

Description

technical field [0001] The invention relates to the technical field of catalysts, in particular to a zinc-based metal-organic framework material, an iron-nitrogen co-doped carbon-based oxygen reduction electrocatalyst based on the zinc-based metal-organic framework material, and a preparation method and application thereof. Background technique [0002] Fuel cells and metal-air batteries are considered promising clean energy conversion devices. However, the slow kinetic nature of the oxygen reduction reaction (ORR) at the cathode limits the energy conversion efficiency of these devices. Currently, noble platinum (e.g., Pt / C) and its alloys still represent the state-of-the-art catalysts, but high cost, scarce reserves, and poor stability severely hinder their large-scale applications. Therefore, there has been a growing interest in developing cost-effective, earth-abundant and highly efficient non-precious metal-based catalysts in this field in recent years. In this case, t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/88H01M4/86H01M4/90
CPCH01M4/9008H01M4/8882H01M4/8652Y02E60/50
Inventor 诸海滨黄佳维
Owner SOUTHEAST UNIV
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