CN1128019C - Process for preparing catalyst of fuel battery with proton exchange membrane - Google Patents
Process for preparing catalyst of fuel battery with proton exchange membrane Download PDFInfo
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- CN1128019C CN1128019C CN01127116A CN01127116A CN1128019C CN 1128019 C CN1128019 C CN 1128019C CN 01127116 A CN01127116 A CN 01127116A CN 01127116 A CN01127116 A CN 01127116A CN 1128019 C CN1128019 C CN 1128019C
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- catalyst
- component
- proton exchange
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- sodium
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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
质子交换膜燃料电池催化剂的制备方法是一种质子交换膜燃料电池催化剂的制备方法，该方法为：①首先在碳粉悬浮液载体中注入催化剂前驱体，并加入碱调节pH值为4.0～9.0，然后在低温下真空干燥得到组份A；②向组份A中加入固体还原剂，经充分研磨，直到金属盐与还原剂完全发生固相反应，从而使还原出的金属盐微粒吸附于碳载体上，得到组份B；③将组份B经碱洗、酸洗、水洗后干燥，即制得碳粉负载的粉沫催化剂。The preparation method of proton exchange membrane fuel cell catalyst is a preparation method of proton exchange membrane fuel cell catalyst. The method is as follows: ① first, inject the catalyst precursor into the carbon powder suspension carrier, and add alkali to adjust the pH value to 4.0-9.0 , and then vacuum-dried at low temperature to obtain Component A; ② Add a solid reducing agent to Component A, and grind thoroughly until the metal salt and the reducing agent completely undergo a solid phase reaction, so that the reduced metal salt particles are adsorbed on carbon Component B is obtained on the carrier; ③ After the component B is washed with alkali, acid and water, it is dried to obtain a powder catalyst supported by carbon powder.
Description
One, technical field
The present invention is a kind of proton exchange fuel cell catalyst, belongs to the technical field that catalyst is made.
Two, background technology
Fuel cell becomes following best " clean energy resource " owing to have advantages such as energy conversion efficiency height, environmental pollution are little, and many national government are paid much attention to its research.Particularly Proton Exchange Membrane Fuel Cells because it can be used as the electrical source of power and the portable removable power supply of electric vehicle, and is subjected to extensive concern in recent years.The research work of Proton Exchange Membrane Fuel Cells concentrates on the research of catalyst at present, and be the most effective catalyst of Proton Exchange Membrane Fuel Cells with the multiple catalyzing system of Pt or other metal of Pt+, but, because the price of these metals is extremely expensive, and resource-constrained, thus cause battery to cost an arm and a leg, be difficult to carry out commercialization, therefore, people wish to improve as much as possible the activity of metallic catalyst and the cost that utilization rate reduces catalyst.
At present, people mainly concentrate on the research of catalyst: how on traditional preparation method basis,, further optimize the performance of catalyst by changing the condition of work of battery, and to the research of method for preparing catalyst seldom.But because traditional preparation method, as: liquid phase chemical reduction, electrochemical deposition, high temperature vapour deposition or the like, all exist the factor that some are unfavorable for improving catalyst performance, such as, exist fierce Brownian movement in the liquid-phase system; Particle aggregation under the hot conditions or the like, these factors often cause the catalyst particle diameter bigger, and agglomeration takes place particle easily simultaneously, thereby has reduced the catalytic performance of catalyst.And by the condition of work of change battery and the preparation method of electrode, can not fundamentally improve the performance of catalyst of fuel batter with proton exchange film, therefore seek more appropriate catalyst preparation method, become the task of top priority in the present fuel cell studies work.
Three, summary of the invention
It is simple that purpose of the present invention just provides a kind of technology, and the catalyst particle size of preparation is little, utilization rate height, the preparation method of the catalyst of fuel batter with proton exchange film that activity is high.
Preparation solid yardage method of the present invention is:
1. injecting catalyst presoma in carbon dust suspension carrier at first, and adding alkali, to regulate the pH value be 4.0～9.0, vacuum drying obtains component A at low temperatures then;
2. in component A, add solid reductant,, up to slaine and reducing agent solid phase reaction takes place fully, thereby the slaine particulate that restores is adsorbed on the carbon carrier, obtain component B through fully grinding;
3. with component B drying after alkali cleaning, pickling, washing, promptly make the fine catalyst of carbon dust load.
Catalyst precursor is H
2PtCl
6Or K
2PtCl
6Or the weak solution of the ruthenium of platiniferous, osmium, iridium, above total metal content is 5～35% of a carbon dust amount, wherein the content of platinum accounts for more than 20% of above total metal content.
Solid reductant is one or more in polyformaldehyde, sodium formate, sodium borohydride, sodium sulfite, sodium thiosulfate, the sodium dithionate.
With component B drying after alkali cleaning, pickling, washing is to carry out in air or argon gas or hydrogen or nitrogen or in the atmosphere of oxygen.
The present invention has following advantage:
Theoretically, the particle diameter of catalyst is more little, and then the specific area of catalyst is big more, and the utilization rate of catalyst is just high more; Simultaneously, when activity of such catalysts just high more.And the catalyst that the present invention synthesizes is found through projection Electronic Speculum (TEM) and X-diffraction (XRD) analysis: the diameter of catalyst particle is little of 2-4nm, and system amorphous substance content is higher simultaneously; And the catalyst particle diameter that traditional liquid phase reactor obtains is approximately 10-12nm, and amorphous substance content is relative also lower in the system simultaneously.Electrochemical research methods such as utilization cyclic voltammetry have been studied the catalytic oxidation of catalyst to methyl alcohol, and experimental result is also found: the catalyst that utilizes solid phase reaction to make shows more excellent electrocatalysis characteristic.
Four, the specific embodiment
Example one: take by weighing the Vulcan XC-72R activated carbon powder of 40mg Cabot company, add 1.3ml0.0386mol/L H
2PtCL
6Solution, and add 0.9974mol/L NaOH solution 3.2ml, in agate mortar, mix, ground 10 minutes.Then, the gained mixture is placed vacuum drying chamber, in 50 ℃ of vacuum drying 10-12 hours, till system moisture removes fully.
Be cooled to room temperature under vacuum protection, constantly gradation adds polyformaldehyde on a small quantity, grinds approximately more than 4 hours, makes slaine and reducing agent complete reaction.
With small amount of thermal dilute NaOH solution washing said mixture, remove unreacted polyformaldehyde, unreacted a small amount of salt is reduced fully.Pickling again, washing repeatedly with the liquor argenti nitratis ophthalmicus check, does not have chlorion in eluate repeatedly.
90 ℃ of dryings promptly make the Pt/C catalyst under air conditions, and wherein the size of Pt particle is 2-4nm.
Experiment two: take by weighing the Vulcan XC-72R activated carbon powder of 40mgCabot company, add 1.5ml0.0386mol/L H
2PtCl
6With 0.6ml 0.09635mol/L RuCl
3Solution adds 0.9974mol/L NaOH solution, mixes in agate mortar, grinds 10 minutes.The gained mixture is placed vacuum drying chamber, in 50 ℃ of vacuum drying 10-12 hours, till system moisture removes fully.
Be cooled to room temperature under vacuum protection, constantly gradation adds polyformaldehyde on a small quantity, grinds 4-5 hour, makes slaine and reducing agent complete reaction.
With small amount of thermal dilute NaOH solution washing said mixture, remove unreacted polyformaldehyde, unreacted a small amount of salt is reduced fully.Pickling again, washing repeatedly with the liquor argenti nitratis ophthalmicus check, does not have chlorion in eluate repeatedly.
90 ℃ of dryings are promptly made the Pt-Ru/c catalyst under air conditions, and its catalyst particle size is about 2-4nm.
Claims (4)
1. the preparation method of a catalyst of fuel batter with proton exchange film is characterized in that the method for preparing is:
1. injecting catalyst presoma in carbon dust suspension carrier at first, and adding alkali, to regulate the pH value be 4.0～9.0, vacuum drying obtains component A at low temperatures then;
2. in component A, add solid reductant,, up to slaine and reducing agent solid phase reaction takes place fully, thereby the slaine particulate that restores is adsorbed on the carbon carrier, obtain component B through fully grinding;
3. with component B drying after alkali cleaning, pickling, hand washing, promptly make the fine catalyst of carbon dust load.
2. according to the preparation method of claim 1 described catalyst of fuel batter with proton exchange film, it is characterized in that catalyst precursor is H
2PtCl
6Or K
2PtCl
6Or the weak solution of the ruthenium of platiniferous, osmium, iridium, above total metal content is 5～35% of a carbon dust amount, wherein the content of platinum accounts for more than 20% of above total metal content.
3. according to the preparation method of claim 1 described catalyst of fuel batter with proton exchange film, it is characterized in that solid reductant is one or more in polyformaldehyde, sodium formate, sodium borohydride, sodium sulfite, sodium thiosulfate, the sodium dithionate.
4. according to the preparation method of claim 1 described catalyst of fuel batter with proton exchange film, it is characterized in that be to carry out component B through drying after alkali cleaning, pickling, the hand washing in the atmosphere of air or argon gas or hydrogen or nitrogen or oxygen.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN01127116A CN1128019C (en) | 2001-08-17 | 2001-08-17 | Process for preparing catalyst of fuel battery with proton exchange membrane |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN01127116A CN1128019C (en) | 2001-08-17 | 2001-08-17 | Process for preparing catalyst of fuel battery with proton exchange membrane |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1346706A CN1346706A (en) | 2002-05-01 |
| CN1128019C true CN1128019C (en) | 2003-11-19 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN01127116A Expired - Fee Related CN1128019C (en) | 2001-08-17 | 2001-08-17 | Process for preparing catalyst of fuel battery with proton exchange membrane |
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| Country | Link |
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| CN (1) | CN1128019C (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100531914C (en) * | 2006-08-09 | 2009-08-26 | 华南理工大学 | solid phase reduction preparation method for platinum, carbon catalyst of fuel cell |
| JP6608800B2 (en) * | 2016-12-09 | 2019-11-20 | トヨタ自動車株式会社 | Fuel cell electrode catalyst |
| CN110556547B (en) * | 2018-05-30 | 2023-01-13 | 中国科学院深圳先进技术研究院 | Noble metal nano cage catalyst and preparation method and application thereof |
-
2001
- 2001-08-17 CN CN01127116A patent/CN1128019C/en not_active Expired - Fee Related
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| CN1346706A (en) | 2002-05-01 |
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