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Preparation and application of a nitrogen-functionalized carbon material loaded with metal-organic framework compounds

A metal-organic framework and organic framework technology, applied in structural parts, electrical components, battery electrodes, etc., can solve the problems that limit the development of direct alcohol fuel cells, lack of natural resources, expensive metal Pt, etc., and achieve good methanol poisoning resistance , The preparation process is simple, the effect of reducing the reduction ability

Active Publication Date: 2019-03-29
NORTHWEST NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, metal Pt is relatively expensive, and is easily poisoned by methanol, and its natural resources are scarce.
This greatly limits the development of direct alcohol fuel cells

Method used

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  • Preparation and application of a nitrogen-functionalized carbon material loaded with metal-organic framework compounds
  • Preparation and application of a nitrogen-functionalized carbon material loaded with metal-organic framework compounds
  • Preparation and application of a nitrogen-functionalized carbon material loaded with metal-organic framework compounds

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] 1. Preparation of catalyst 10%MIL(Fe)-PPy-800

[0033] a. Polypyrrole preparation: ultrasonically dissolve 0.784g methyl orange in 480mL water, add 3.888g FeCl 3 , stirred to dissolve, slowly added pyrrole 480μL, stirred for 24h, the product was filtered and washed, dried overnight, and ground.

[0034] b. MIL-101 (Fe) preparation: take 0.675g FeCl 3 ·6H 2 O and 0.206g of terephthalic acid were added to 15mL of DMF, and the mixed solution was ultrasonically mixed for half an hour to make it evenly mixed; then it was placed in a polytetrafluoroethylene-lined stainless steel reactor and heated at 110°C for 20 hours; the obtained brown The solid was filtered off, the crude product was washed with hot ethanol at reflux, the product was filtered off and dried in an oven at 60°C.

[0035] c. Preparation of 10% MIL(Fe)-PPy-800: Take the above 0.5g polypyrrole (PPy), dissolve it in 30mL absolute ethanol, add 0.05g MIL-101(Fe), physically mix and stir for 3h, 80℃ Dry it unde...

Embodiment 2

[0039]1. Preparation of catalyst 30%MIL(Fe)-PPy-800

[0040] a. Polypyrrole preparation: with embodiment 1;

[0041] b. MIL-101 (Fe) preparation: same as Example 1;

[0042] c. Preparation of 30% MIL(Fe)-PPy-800: Take the above 0.5g polypyrrole (PPy), dissolve it in 30mL absolute ethanol, add 0.15g MIL-101(Fe), physically mix and stir for 3h, 80℃ Dry it under vacuum, grind it, and carbonize it at 800°C for 3h in a nitrogen atmosphere.

[0043] 2. Oxygen reduction test

[0044] Test condition and method are with embodiment 1, and test result is as Figure 5 shown. Depend on Figure 5 It can be seen that when the scan rate is 10mV / s, the onset potential of oxygen reduction is 0.79V, the half-wave potential is -0.0445V, and the peak potential reaches -0.084V. Catalyst 30% MIL(Fe)-PPy-800 performed better than 20% commercial Pt / C catalyst.

Embodiment 3

[0046] 1. Preparation of catalyst 50%MIL(Fe)-PPy-700

[0047] a. Polypyrrole preparation: with embodiment 1;

[0048] b. MIL-101 (Fe) preparation: same as Example 1;

[0049] c. Preparation of 50% MIL(Fe)-PPy-700: Take the above 0.5g polypyrrole (PPy), dissolve it in 30mL absolute ethanol, add 0.25g MIL-101(Fe), physically mix and stir for 3h, at 80℃ Vacuum-dried, ground, and carbonized at 700 ° C for 3 hours in a nitrogen atmosphere, that is.

[0050] 2. Oxygen reduction test

[0051] Weigh 5mg of 50% MIL(Fe)-PPy-700, add 0.5mL absolute ethanol and 20μL Nafion (Dupont, 5wt%) solution, sonicate for 30min, take 3μL and apply it on the glassy carbon electrode. The test was carried out in a three-electrode system, the Pt wire electrode was used as the counter electrode, the Ag / AgCl electrode was used as the reference electrode, the glassy carbon electrode coated with catalyst was used as the working electrode, and 0.1M KOH was used as the electrolyte for testing. Such as Fi...

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Abstract

The invention discloses preparation of a metal organic framework compound-loaded nitrogen functionalized carbon material. The preparation comprises the following steps of mixing polypyrrole and a metal organic framework compound by a physical stirring method in an organic solvent, and carbonizing in the nitrogen atmosphere at high temperature. The preparation has the advantages that the prepared carbon material sample is carbon nanotube-loaded flaky carbide, the diameter of a nanotube is about 70nm, and the loading amount of metal organic framework compound is 10%-70%; after proofing by an oxide reduction property test, when the nitrogen functionalized carbon material is used as a catalyst, the oxygen reduction property in the alkaline environment is better than the oxygen reduction property of commercial Pt / C; the methanol poisoning-resistant capacity is good, and the reduction capacity is not obviously reduced after circulating for 10000 cycles; the preparation process of the catalyst is simple; any noble metal is not used, so that the catalyst is a cathode oxygen reduction catalyst which may replace the commercial Pt / C in future, and the industrial application prospect is good.

Description

technical field [0001] The present invention relates to the preparation of a nitrogen-functionalized carbon material loaded with non-precious metals, in particular to the preparation of a nitrogen-functionalized carbon material loaded with a metal-organic framework compound, which is mainly used in the oxygen reduction catalytic reaction of the methanol fuel cell cathode, plague composite material technology field and the field of methanol fuel cell technology. Background technique [0002] Fuel cells, an energy conversion device that directly converts chemical energy stored in fuels and oxidants into electrical energy, have been rapidly developed due to their green and recyclable advantages. Proton exchange membrane fuel cell (PEMFC) is expected to become one of the power sources to replace the current automobile power due to its advantages of low operating temperature, fast start-up and high power density. First, hydrogen enters the battery from the anode, is catalyzed by...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M4/90
CPCH01M4/9083Y02E60/50
Inventor 童金辉马江平王文慧李卿刘方方马文梅
Owner NORTHWEST NORMAL UNIVERSITY