CN104475090A - Cathode catalyst for proton exchange membrane fuel cell and preparation method of cathode catalyst for proton exchange membrane fuel cell - Google Patents
Cathode catalyst for proton exchange membrane fuel cell and preparation method of cathode catalyst for proton exchange membrane fuel cell Download PDFInfo
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- CN104475090A CN104475090A CN201410787246.8A CN201410787246A CN104475090A CN 104475090 A CN104475090 A CN 104475090A CN 201410787246 A CN201410787246 A CN 201410787246A CN 104475090 A CN104475090 A CN 104475090A
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- proton exchange
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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 preparation method of a cathode catalyst for a proton exchange membrane fuel cell. The preparation method comprises the following steps: uniformly attaching a Pt precursor onto graphene; and then introducing steam of a reducing agent to react with the catalyst precursor to prepare a nanometer catalyst with high metallic particle dispersion and uniformity in particle diameter. The nanometer catalyst is high in activity and high in anti-poisoning capacity and shows very high stability on the electrocatalytic oxidation of methanol. The preparation method provided by the invention has the advantages of easiness and convenience for operation in a preparation process, energy conservation and environment protection. The prepared catalyst can be used as a catalyst for a series of proton exchange membrane fuel cells which include direct methanol fuel cells.
Description
Technical field
The present invention relates to 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 low-temperature fuel cell field, has cleaning, safety, the feature such as efficient.But because high, the anti-poisoning capability of the cost of catalyst Pt is weak, causes activity stability poor, limit the large-scale application of Proton Exchange Membrane Fuel Cells.For this, researcher improves the activity of catalyst by the method improving traditional Kaolinite Preparation of Catalyst.Infusion process is a kind of very traditional common method preparing noble metal catalyst, but needs to use hydrogen reducing at about 250 DEG C, operates more loaded down with trivial details, metal particle diameter wider range, and there is potential safety hazard.Chemical reduction method is the another kind of preparation method using more support type Pt and Pt multicomponent catalyst.At mixed solution system, with boride, many alcohol, formaldehyde and formic acid as reducing agent, reduce at a certain temperature, the shortcoming of the method needs a large amount of solvents and excessive reducing agent, not only increases the cost of post processing, but also cause environmental pollution.Therefore, need to find simple and effective preparation method and carry out 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, noble metal utilisation is high, anti-poisoning capability is 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 of Pt is adsorbed on Graphene, dry, the solvent in removing system;
2), at the Graphene being adsorbed with precursor being placed in 110 ~ 180 DEG C, the steam of reducing agent formaldehyde or formic acid and the precursor of Pt is utilized to react 1.5 ~ 2.5h;
3) after completion of the reaction, room temperature cools, with absolute ethyl alcohol, distilled water cleaning, and chlorion in removing catalyst, vacuum drying, fuel battery cathode with proton exchange film catalyst.
Described Graphene obtains by the following method: by the NaNO of 1.0g graphite and 1.0g
3add to the H that 46ml concentration is 98%
2sO
4in solution, after ice bath mechanical agitation 20min, slowly add the KMnO of 6.0g
4with 80ml redistilled water, control temperature is 80 ± 5 DEG C, after continuing to stir 30min, then in reaction system, adds 200ml redistilled water and slowly add 6ml mass fraction 30wt%H
2o
2solution, filters while hot, and be neutral with redistilled water cleaning to filtrate, be distributed to by products therefrom in 500ml redistilled water, ultrasonic power is 150W ~ 200W, and ultrasonic 3h i.e. obtained homodisperse monolithic graphite alkene.
The adsorption step of precursor on Graphene of described Pt: l0mg Graphene ultrasonic disperse, 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%.
Nanoparticulate dispersed synthesized by the present invention is good, and size is even, shows significantly active high to the electroxidation of methyl alcohol, good stability, the feature that anti-catalytic oxidation methyl alcohol intermediate product ability is strong, and also preparation process is simple to operate, reducing agent can be reused, energy-conservation environmental protection again.
Product prepared by the present invention can be used for the catalyst of the series of proton exchange membrane fuel comprising DMFC.
Detailed description of the invention
Embodiment 1
By 1.0g graphite and 1.0gNaNO
3add to the H that 46ml concentration is 98%
2sO
4in solution, after ice bath mechanical agitation 20min, slowly add the KMnO of 6.0g
4with 80ml redistilled water, control temperature is 80 ± 5 DEG C, after continuing to stir 30min, then in reaction system, adds 200ml redistilled water and slowly add 6ml mass fraction 30wt%H
2o
2solution, filters while hot, and be neutral with redistilled water cleaning to filtrate, be distributed to by products therefrom in 500ml redistilled water, ultrasonic power is 150W ~ 200W, and ultrasonic 3h i.e. obtained homodisperse monolithic graphite alkene.
By the Graphene ultrasonic disperse of l00mg in 1.5ml deionized water, the content adding 13.3ul Pt is the H of 37.67ug/ul
2ptC1
66H
2the O aqueous solution, mixing, dry, the solvent of going out in above-mentioned system.At 110 DEG C, pass into the formaldehyde vapors of identical temperature and the H be adsorbed on Graphene
2ptC1
6reaction 2.0h.Room temperature cools, and with absolute ethyl alcohol, distilled water repeatedly cleaning catalyst, 50 DEG C of vacuum drying 12h, the loading obtaining Pt is the catalyst of fuel batter with proton exchange film of 0.5wt%.
Embodiment 2
The preparation of Graphene is with embodiment 1
By the Graphene ultrasonic disperse of l00mg in 1.5ml deionized water, the content adding 13.3ul Pt is the H of 37.67ug/ul
2ptC1
66H
2the O aqueous solution, mixing, dry, the solvent of going out in above-mentioned system.At 145 DEG C, pass into the formaldehyde vapors of identical temperature and the H be adsorbed on Graphene
2ptC1
6reaction 1.5h.Room temperature cools, and with absolute ethyl alcohol, distilled water repeatedly cleaning catalyst, 50 DEG C of vacuum drying 12h, the loading obtaining Pt is the fuel battery cathode with proton exchange film catalyst of 0.5wt%.
Embodiment 3
The preparation of Graphene is with embodiment 1
By the Graphene ultrasonic disperse of l0mg in 1.5ml deionized water, the content adding 66.4ul Pt is the H of 37.67ug/ul
2ptC1
66H
2the O aqueous solution, mixing, dry, the solvent of going out in above-mentioned system.At 180 DEG C, pass into the formic acid steam of identical temperature and the H be adsorbed on Graphene
2ptC1
6reaction 1.5h.Room temperature cools, and with absolute ethyl alcohol, distilled water repeatedly cleaning catalyst, 50 DEG C of vacuum drying 12h, the loading obtaining Pt is the fuel battery cathode with proton exchange film catalyst of 20wt%.
Embodiment 4
The preparation of Graphene is with embodiment 1
By the Graphene ultrasonic disperse of l0mg in 1.5ml deionized water, the content adding 29.5ul Pt is the H of 37.67ug/ul
2ptC1
66H
2the O aqueous solution, mixing, dry, the solvent of going out in above-mentioned system.At 110 DEG C, pass into the formic acid steam of identical temperature and the H be adsorbed on Graphene
2ptC1
6reaction 2.0h.Room temperature cools, and with absolute ethyl alcohol, distilled water repeatedly cleaning catalyst, 50 DEG C of vacuum drying 12h, the loading obtaining Pt is the fuel battery cathode with proton exchange film catalyst of 10wt%.
Claims (3)
1. a preparation method for fuel battery cathode with proton exchange film catalyst, is characterized in that, comprises the steps:
1) precursor of Pt is adsorbed on Graphene, dry, the solvent in removing system;
2), at the Graphene being adsorbed with precursor being placed in 110 ~ 180 DEG C, the steam of reducing agent formaldehyde or formic acid and the precursor of Pt is utilized to react 1.5 ~ 2.5h;
3) after completion of the reaction, room temperature cools, with absolute ethyl alcohol, distilled water cleaning, and chlorion in removing catalyst, vacuum drying, fuel battery cathode with proton exchange film catalyst.
2. a kind of preparation method of fuel battery cathode with proton exchange film catalyst as described in claim l, it is characterized in that, described Graphene obtains by the following method: by the NaNO of 1.0g graphite and 1.0g
3add to the H that 46ml concentration is 98%
2sO
4in solution, after ice bath mechanical agitation 20min, slowly add the KMnO of 6.0g
4with 80ml redistilled water, control temperature is 80 ± 5 DEG C, after continuing to stir 30min, then in reaction system, adds 200ml redistilled water and slowly add 6ml mass fraction 30wt%H
2o
2solution, filters while hot, and be neutral with redistilled water cleaning to filtrate, be distributed to by products therefrom in 500ml redistilled water, ultrasonic power is 150W ~ 200W, and ultrasonic 3h i.e. obtained homodisperse monolithic graphite alkene.
3. a kind of preparation method of fuel battery cathode with proton exchange film catalyst as described in claim l, is characterized in that, the adsorption step of precursor on Graphene of described Pt: l0mg Graphene ultrasonic disperse, 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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|---|---|---|---|
| CN201410787246.8A CN104475090A (en) | 2014-12-17 | 2014-12-17 | Cathode catalyst for proton exchange membrane fuel cell and preparation method of cathode catalyst for proton exchange membrane fuel cell |
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| CN201410787246.8A CN104475090A (en) | 2014-12-17 | 2014-12-17 | Cathode catalyst for proton exchange membrane fuel cell and preparation method of cathode catalyst for proton exchange membrane fuel cell |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103120938A (en) * | 2013-03-04 | 2013-05-29 | 北京化工大学常州先进材料研究院 | Preparation method of Pd/graphene nano electro-catalyst |
| CN103157463A (en) * | 2013-03-04 | 2013-06-19 | 北京化工大学常州先进材料研究院 | Preparing method of proton exchange membrane fuel cell cathode catalyst |
| CN103212421A (en) * | 2013-03-01 | 2013-07-24 | 北京化工大学常州先进材料研究院 | Preparation method of nano-grade electro-catalyst based on graphene |
| CN103212408A (en) * | 2013-02-28 | 2013-07-24 | 北京化工大学常州先进材料研究院 | Preparation method of high-CO-toxicity-resistant Pt-M/graphene catalyst |
-
2014
- 2014-12-17 CN CN201410787246.8A patent/CN104475090A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103212408A (en) * | 2013-02-28 | 2013-07-24 | 北京化工大学常州先进材料研究院 | Preparation method of high-CO-toxicity-resistant Pt-M/graphene catalyst |
| CN103212421A (en) * | 2013-03-01 | 2013-07-24 | 北京化工大学常州先进材料研究院 | Preparation method of nano-grade electro-catalyst based on graphene |
| CN103120938A (en) * | 2013-03-04 | 2013-05-29 | 北京化工大学常州先进材料研究院 | Preparation method of Pd/graphene nano electro-catalyst |
| CN103157463A (en) * | 2013-03-04 | 2013-06-19 | 北京化工大学常州先进材料研究院 | Preparing method of proton exchange membrane fuel cell cathode catalyst |
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Application publication date: 20150401 |