CN103157463A - Preparing method of proton exchange membrane fuel cell cathode catalyst - Google Patents
Preparing method of proton exchange membrane fuel cell cathode catalyst Download PDFInfo
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- CN103157463A CN103157463A CN201310067496XA CN201310067496A CN103157463A CN 103157463 A CN103157463 A CN 103157463A CN 201310067496X A CN201310067496X A CN 201310067496XA CN 201310067496 A CN201310067496 A CN 201310067496A CN 103157463 A CN103157463 A CN 103157463A
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- catalyst
- proton exchange
- graphene
- precursor
- exchange membrane
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/50—Fuel cells
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Abstract
The invention provides a preparing method of a proton exchange membrane fuel cell cathode catalyst. A precursor of platinum (Pt) can be evenly attached on grapheme. A reducing agent can be passed into steam so as to react with a precursor of a catalyst and then the nano-catalyst which is highly dispersive in metallics and uniform in grain diameter can be prepared. The electrocatalytic oxidation is conducted on the methyl alcohol through the nano-catalyst so that the methyl alcohol is high in activity and strong in poison tolerance. The methyl alcohol shows up strong stability. The preparing method of the proton exchange membrane fuel cell cathode catalyst is simple in operation, energy-saving and environment-friendly. The catalyst can be prepared to be used as the catalyst of a series of proton exchange membrane fuel cells, wherein the series of proton exchange membrane fuel cells comprise direct methanol fuel cells.
Description
Technical field
The present invention relates to the fuel-cell catalyst preparation method, particularly a kind of preparation method of fuel battery cathode with proton exchange film catalyst.
Background technology
Proton Exchange Membrane Fuel Cells belongs to the low-temperature fuel cell field, has cleaning, safety, the characteristics such as efficient.But a little less than, anti-poisoning capability high due to the cost of catalyst Pt, cause activity stability poor, limited the large-scale application of Proton Exchange Membrane Fuel Cells.For this, the researcher improves the activity of catalyst by the method for improving traditional Kaolinite Preparation of Catalyst.Infusion process is a kind of common method of very traditional preparation noble metal catalyst, but need to use hydrogen reducing at about 250 ℃, operate more loaded down with trivial details, metal particle diameter wider range, and have potential safety hazard.Chemical reduction method is another kind of more support type Pt and the preparation method of Pt multicomponent catalyst of using.At mixed solution system,, to reduce at a certain temperature as reducing agent with boride, many alcohol, formaldehyde and formic acid, the shortcoming of the method is to need a large amount of solvents and excessive reducing agent, not only increases the cost of post processing, but also causes environmental pollution.Therefore, need to seek simple and effective preparation method and come Kaolinite Preparation of Catalyst, improve the performance of catalyst.
Summary of the invention
The object of the present invention is to provide the preparation method of the fuel battery cathode with proton exchange film catalyst that a kind of preparation process is simple, environmental pollution is little, the catalyst activity that the method prepares is high, the noble metal utilization rate is high, anti-poisoning capability strong, good stability.
The present invention seeks to be achieved through the following technical solutions:
A kind of preparation method of fuel battery cathode with proton exchange film catalyst comprises the steps:
1) precursor with Pt is adsorbed on Graphene, and drying is removed the solvent in system;
2) absorption there is the Graphene of precursor be placed under 110～180 ℃, utilizes the steam of reducing agent formaldehyde or formic acid and precursor reaction 1.5～2.5h of Pt;
3) reaction complete after, room temperature is cooling, cleans with absolute ethyl alcohol, distilled water, removes chlorion in catalyst, vacuum drying, fuel battery cathode with proton exchange film catalyst.
Described Graphene makes by the following method: with the NaNO of 1.0g graphite and 1.0g
3Add to 46ml concentration and be 98% H
2SO
4In solution, slowly add the KMnO of 6.0g after ice bath mechanical agitation 20min
4With the 80ml redistilled water, controlling temperature is 80 ± 5 ℃, after continuing to stir 30min, then adds the 200ml redistilled water and slowly adds 6ml mass fraction 30wt%H in reaction system
2O
2Solution filters while hot, and it is neutral cleaning to filtrate with redistilled water, and products therefrom is distributed in the 500ml redistilled water, and ultrasonic power is 150W～200W, and ultrasonic 3h namely makes homodisperse monolithic Graphene.
The adsorption step of the precursor of described Pt on Graphene: the 10mg Graphene is ultrasonic to be scattered in 1.0ml～2ml deionized water, adds H
2PtC1
66H
2The O aqueous solution, mixing, after reduction, the mass loading amount of Pt is 0.5%～20%.
The nanoparticulate dispersed that the present invention synthesized is good, and size evenly shows obvious activity to the electroxidation of methyl alcohol high, good stability, the strong characteristics of anti-catalytic oxidation methyl alcohol intermediate product ability, and also preparation process is simple to operate, reducing agent can be reused, energy-conservation environmental protection again.
The prepared product of the present invention can be used for comprising the catalyst of the series of proton exchange membrane fuel of DMFC.
The specific embodiment
Embodiment 1
With 1.0g graphite and 1.0gNaNO
3Add to 46ml concentration and be 98% H
2SO
4In solution, slowly add the KMnO of 6.0g after ice bath mechanical agitation 20min
4With the 80ml redistilled water, controlling temperature is 80 ± 5 ℃, after continuing to stir 30min, then adds the 200ml redistilled water and slowly adds 6ml mass fraction 30wt%H in reaction system
2O
2Solution filters while hot, and it is neutral cleaning to filtrate with redistilled water, and products therefrom is distributed in the 500ml redistilled water, and ultrasonic power is 150W～200W, and ultrasonic 3h namely makes homodisperse monolithic Graphene.
Be scattered in the 1.5ml deionized water the Graphene of l00mg is ultrasonic, the content that adds 13.3ul Pt is the H of 37.67ug/ul
2PtC1
66H
2The O aqueous solution, mixing, drying is gone out solvent in above-mentioned system.Under 110 ℃, pass into the formaldehyde vapors and the H that is adsorbed on Graphene of uniform temp
2PtC1
6Reaction 2.0h.Room temperature is cooling, uses repeatedly cleaning catalyst of absolute ethyl alcohol, distilled water, 50 ℃ of vacuum drying 12h, and the loading that obtains Pt is the catalyst of fuel batter with proton exchange film of 0.5wt%.
Embodiment 2
The preparation of Graphene is with embodiment 1
Be scattered in the 1.5ml deionized water the Graphene of l00mg is ultrasonic, the content that adds 13.3ul Pt is the H of 37.67ug/ul
2PtC1
66H
2The O aqueous solution, mixing, drying is gone out solvent in above-mentioned system.Under 145 ℃, pass into the formaldehyde vapors and the H that is adsorbed on Graphene of uniform temp
2PtC1
6Reaction 1.5h.Room temperature is cooling, uses repeatedly cleaning catalyst of absolute ethyl alcohol, distilled water, 50 ℃ of vacuum drying 12h, and the loading that obtains Pt is the fuel battery cathode with proton exchange film catalyst of 0.5wt%.
Embodiment 3
The preparation of Graphene is with embodiment 1
Be scattered in the 1.5ml deionized water the Graphene of l0mg is ultrasonic, the content that adds 66.4ul Pt is the H of 37.67ug/ul
2PtC1
66H
2The O aqueous solution, mixing, drying is gone out solvent in above-mentioned system.Under 180 ℃, pass into the formic acid steam and the H that is adsorbed on Graphene of uniform temp
2PtC1
6Reaction 1.5h.Room temperature is cooling, uses repeatedly cleaning catalyst of absolute ethyl alcohol, distilled water, 50 ℃ of vacuum drying 12h, and the loading that obtains Pt is the fuel battery cathode with proton exchange film catalyst of 20wt%.
Embodiment 4
The preparation of Graphene is with embodiment 1
Be scattered in the 1.5ml deionized water the Graphene of l0mg is ultrasonic, the content that adds 29.5ul Pt is the H of 37.67ug/ul
2PtC1
66H
2The O aqueous solution, mixing, drying is gone out solvent in above-mentioned system.Under 110 ℃, pass into the formic acid steam and the H that is adsorbed on Graphene of uniform temp
2PtC1
6Reaction 2.0h.Room temperature is cooling, uses repeatedly cleaning catalyst of absolute ethyl alcohol, distilled water, 50 ℃ of vacuum drying 12h, and the loading that obtains Pt is the fuel battery cathode with proton exchange film catalyst of 10wt%.
Claims (3)
1. the preparation method of a fuel battery cathode with proton exchange film catalyst, is characterized in that, comprises the steps:
1) precursor with Pt is adsorbed on Graphene, and drying is removed the solvent in system;
2) absorption there is the Graphene of precursor be placed under 110～180 ℃, utilizes the steam of reducing agent formaldehyde or formic acid and precursor reaction 1.5～2.5h of Pt;
3) reaction complete after, room temperature is cooling, cleans with absolute ethyl alcohol, distilled water, removes chlorion in catalyst, vacuum drying, fuel battery cathode with proton exchange film catalyst.
2. as the preparation method of a kind of fuel battery cathode with proton exchange film catalyst as described in claim l, it is characterized in that, described Graphene makes by the following method: with the NaNO of 1.0g graphite and 1.0g
3Add to 46ml concentration and be 98% H
2SO
4In solution, slowly add the KMnO of 6.0g after ice bath mechanical agitation 20min
4With the 80ml redistilled water, controlling temperature is 80 ± 5 ℃, after continuing to stir 30min, then adds the 200ml redistilled water and slowly adds 6ml mass fraction 30wt%H in reaction system
2O
2Solution filters while hot, and it is neutral cleaning to filtrate with redistilled water, and products therefrom is distributed in the 500ml redistilled water, and ultrasonic power is 150W～200W, and ultrasonic 3h namely makes homodisperse monolithic Graphene.
3. as the preparation method of a kind of fuel battery cathode with proton exchange film catalyst as described in claim l, it is characterized in that the adsorption step of the precursor of described Pt on Graphene: the l0mg Graphene is ultrasonic to be scattered in 1.0ml～2ml deionized water, adds H
2PtC1
66H
2The O aqueous solution, mixing, after reduction, the mass loading amount of Pt is 0.5%～20%.
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| CN201310067496XA CN103157463A (en) | 2013-03-04 | 2013-03-04 | Preparing method of proton exchange membrane fuel cell cathode catalyst |
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| CN201310067496XA CN103157463A (en) | 2013-03-04 | 2013-03-04 | Preparing method of proton exchange membrane fuel cell cathode catalyst |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104475090A (en) * | 2014-12-17 | 2015-04-01 | 北京化工大学常州先进材料研究院 | Cathode catalyst for proton exchange membrane fuel cell and preparation method of cathode catalyst for proton exchange membrane fuel cell |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101733094A (en) * | 2009-12-14 | 2010-06-16 | 浙江大学 | Pt-CeO2/graphene electro-catalyst and preparation method thereof |
| CN102179244A (en) * | 2011-04-13 | 2011-09-14 | 山西大学 | Preparation method of catalyst of proton exchange membrane fuel cell |
| CN102423705A (en) * | 2011-10-17 | 2012-04-25 | 中国科学院山西煤炭化学研究所 | Oxygen reduction catalyst for fuel cell, and preparation method thereof |
-
2013
- 2013-03-04 CN CN201310067496XA patent/CN103157463A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101733094A (en) * | 2009-12-14 | 2010-06-16 | 浙江大学 | Pt-CeO2/graphene electro-catalyst and preparation method thereof |
| CN102179244A (en) * | 2011-04-13 | 2011-09-14 | 山西大学 | Preparation method of catalyst of proton exchange membrane fuel cell |
| CN102423705A (en) * | 2011-10-17 | 2012-04-25 | 中国科学院山西煤炭化学研究所 | Oxygen reduction catalyst for fuel cell, and preparation method thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104475090A (en) * | 2014-12-17 | 2015-04-01 | 北京化工大学常州先进材料研究院 | Cathode catalyst for proton exchange membrane fuel cell and preparation method of cathode catalyst for proton exchange membrane fuel cell |
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Application publication date: 20130619 |