CN103212421A - Preparation method of nano-grade electro-catalyst based on graphene - Google Patents
Preparation method of nano-grade electro-catalyst based on graphene Download PDFInfo
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- CN103212421A CN103212421A CN2013100652763A CN201310065276A CN103212421A CN 103212421 A CN103212421 A CN 103212421A CN 2013100652763 A CN2013100652763 A CN 2013100652763A CN 201310065276 A CN201310065276 A CN 201310065276A CN 103212421 A CN103212421 A CN 103212421A
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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
Abstract
The invention relates to a preparation method of a nano-grade electro-catalyst based on graphene. According to the method, a templating agent is added into an alcohol solution of graphene oxide; ultrasonic processing is carried out, and the mixture is uniformly stirred and oscillated; a mixed solution of chloroplatinic acid and a transition metal salt is dropped in; the mixture is well mixed and is subjected to an intermittent heating reaction in a microwave oven; the mixture is cooled, and the templating agent is removed by using dilute hydrochloric acid; and pump-filtration and vacuum bake-drying are carried out, such that the nano-grade electro-catalyst with graphene as a carrier is obtained. The catalyst provided by the invention has the advantages of small particles, agglomeration prevention, uniform distribution, simple preparation steps, and short preparation process. The catalyst provided by the invention can be used in alcohol fuel batteries and lithium-air batteries.
Description
Technical field
The present invention relates to a kind of Preparation of catalysts method, particularly a kind of preparation method of the nanometer electrical catalyst based on Graphene.
Background technology
Lithium-air battery catalyst commonly used at present is the Pt base of carbon load, although the Pt/C catalyst has good catalytic performance to hydrogen reduction, it is lower that its oxygen is separated out performance, causes battery efficiency to reduce.In recent years, though the research of non-platinum catalyst has obtained important breakthrough, carry the Pd-Co alloy catalyst as carbon, catalytic activity is significantly improved than other non-platinum catalyst, compares with Pt is catalyst based that still activity is lower.Therefore, aspect the catalyst based research of Pt, emphasis is to improve the dispersiveness of Pt on carrier, is improving or is guaranteeing under the active prerequisite, the load capacity of minimizing Pt.The Pt/C catalyst of preparation high dispersive has challenge, and from present research situation, in preparation process, noble metal is assembled easily, and Pt's is dispersed not high enough, and is not obvious to the load capacity that reduces Pt.Therefore, must seek new preparation method and process conditions, reduce the particle size of Pt in the catalyst, increase the decentralization and the effective rate of utilization of Pt on carrier, reduce the load capacity of Pt in the catalyst.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of nanometer electrical catalyst based on Graphene, solve existing carbon carrier when supporting Pt is catalyst based, granular size is wayward and defective such as easy reunion.
A kind of preparation method of the nanometer electrical catalyst based on Graphene, its preparation process is: the template agent is added in the alcoholic solution of graphene oxide, sonic oscillation is even, dropwise drips chloroplatinic acid and transition metal mixed salt solution then, stirs; Place micro-wave oven then, adopt the mode of heating 2～60s 20～200s at intermittence to heat, after reaction is finished, remove the template agent with watery hydrochloric acid, suction filtration, vacuum drying obtain the nanometer electrical catalyst based on Graphene to constant weight.
Described template agent is nano-calcium carbonate, nano zine oxide.
The particle size range of described template agent is 100～800nm.
Described transition metal salt is for containing V, Cr, Mn, Fe, Co, Ni, Ti, Zr, Mo, Sn, the salt of one or both among the Se and above element, and the mixture that can mix by arbitrary proportion.
The mol ratio of described Pt element and transition metal is 1:2～10.
Alcohol in the described alcoholic solution is methyl alcohol, ethanol, ethylene glycol, isopropyl alcohol and glycerine.
The content of described Graphene in catalyst is 85～99.5%.
The invention provides a kind of preparation method simply fast, the relatively mild reducing agent of applied microwave control technique and reducing property reverts to the activity of such catalysts composition surface of carrier quickly and evenly.Preparation process of the present invention is simple, and the time that needs is short, and product loss is little, and improves its catalytic reduction ability to oxygen.The catalyst granules that the inventive method prepares is little, be difficult for reuniting, and is evenly distributed, pore size is adjustable, and electrochemical catalysis is active high.The present invention adopts the selection of heating using microwave, reducing agent and dispersant that the product particle size is controlled between 1～l0nm.The present invention prepares eelctro-catalyst and can be used for alcohol fuel battery and lithium-air battery catalysis.
The specific embodiment
Technical solution of the present invention is not limited to the following cited specific embodiment, also comprises any combination between each specific embodiment.
Embodiment one
With the 0.3g particle diameter is that to add 50mL concentration be in the ethanolic solution of 1mg/mL graphene oxide for the nano zine oxide of 800nm, sonic oscillation becomes homogeneous suspension, dropwise drip 1mL0.005M chloroplatinic acid and 1mL0.01M cobalt acetate mixed solution then, stir 30min to forming even dispersion liquid; Place micro-wave oven then, the mode that adds thermal recovery heating 5s 30s at intermittence heats 10min, after question response is finished, be cooled to room temperature, hydrochloric acid with 10mL0.1M is removed the template agent, and suction filtration washs respectively 3 times with absolute ethyl alcohol and deionized water, vacuum drying obtains the nanometer electrical catalyst based on Graphene to constant weight.
Embodiment two
With the 0.5g particle diameter is that to add 50mL concentration be in the ethylene glycol solution of 1mg/mL graphene oxide for the nano zine oxide of 2 μ m, sonic oscillation becomes homogeneous suspension, dropwise drip 1mL0.01M chloroplatinic acid and 2mL0.02M nickel chloride mixed solution then, stir 30min to forming even dispersion liquid; Place micro-wave oven then, the mode that adds thermal recovery heating 30s 80s at intermittence heats 10min, after question response is finished, be cooled to room temperature, hydrochloric acid with 10mL0.1M is removed the template agent, and suction filtration washs respectively 3 times with absolute ethyl alcohol and deionized water, vacuum drying obtains the nanometer electrical catalyst based on Graphene to constant weight.
Embodiment three
With the 0.1g particle diameter is that to add 50mL concentration be in the glycerine solution of 1mg/mL graphene oxide for the nano-calcium carbonate of 200nm, sonic oscillation becomes homogeneous suspension, dropwise drip 1mL0.004M chloroplatinic acid and 2mL0.01M cobalt nitrate and 2mL0.01M mixed solution then, stir 30min to forming even dispersion liquid; Place micro-wave oven then, the mode that adds thermal recovery heating 10s 60s at intermittence heats 10min, after question response is finished, be cooled to room temperature, sulfuric acid with 10mL0.1M is removed the template agent, and suction filtration washs respectively 3 times with absolute ethyl alcohol and deionized water, vacuum drying obtains the nanometer electrical catalyst based on Graphene to constant weight.
Embodiment four
With the 0.1g particle diameter is that to add 50mL concentration be in the ethylene glycol solution of 1mg/mL graphene oxide for the nano-calcium carbonate of 1 μ m, sonic oscillation becomes homogeneous suspension, dropwise drip 1mL0.01M chloroplatinic acid and 2mL0.01M iron chloride mixed solution then, stir 30min to forming even dispersion liquid; Place micro-wave oven then, the mode that adds thermal recovery heating 50s 180s at intermittence heats 10min, after question response is finished, be cooled to room temperature, hydrochloric acid with 10mL0.1M is removed the template agent, and suction filtration washs respectively 3 times with absolute ethyl alcohol and deionized water, vacuum drying obtains the nanometer electrical catalyst based on Graphene to constant weight.
Claims (7)
1. preparation method based on the nanometer electrical catalyst of Graphene is characterized in that preparation process is: the template agent is added in the alcoholic solution of graphene oxide, sonic oscillation is even, dropwise drips chloroplatinic acid and transition metal mixed salt solution then, stirs; Place micro-wave oven then, adopt the mode of heating 2～60s 20～200s at intermittence to heat, after reaction is finished, remove the template agent with watery hydrochloric acid, suction filtration, vacuum drying obtain the nanometer electrical catalyst based on Graphene to constant weight.
2. according to the preparation method of the described a kind of nanometer electrical catalyst based on Graphene of claim l, it is characterized in that described template agent is nano-calcium carbonate, nano zine oxide.
3. according to the preparation method of the described a kind of nanometer electrical catalyst based on Graphene of claim l, it is characterized in that the particle size range of described template agent is 10～800nm.
4. according to the preparation method of the described a kind of nanometer electrical catalyst based on Graphene of claim l, it is characterized in that described transition metal salt is for containing V, Cr, Mn, Fe, Co, Ni, Ti, Zr, Mo, Sn, the salt of one or both among the Se and above element, and can be by the mixture of arbitrary proportion mixing.
5. according to the preparation method of the described a kind of nanometer electrical catalyst based on Graphene of claim l, it is characterized in that the mol ratio of Pt element and transition metal is 1:2～10.
6. according to the preparation method of the described a kind of nanometer electrical catalyst based on Graphene of claim l, it is characterized in that the alcohol in the described alcoholic solution is methyl alcohol, ethanol, ethylene glycol, isopropyl alcohol and glycerine.
7. according to the preparation method of the described a kind of nanometer electrical catalyst based on Graphene of claim l, it is characterized in that the content of described Graphene in catalyst is 85～99.5%.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103910356A (en) * | 2014-04-28 | 2014-07-09 | 南京新月材料科技有限公司 | Preparation method of three-dimensional graphene |
| CN103915633A (en) * | 2014-04-01 | 2014-07-09 | 上海交通大学 | Composite carbon fiber-loaded metal catalyst as well as preparation method and application thereof |
| 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 |
| CN104667869A (en) * | 2015-02-11 | 2015-06-03 | 四川大学 | Method for removing endocrine disrupter in water by utilizing monopersulfate and ferro-cobalt loaded dual-phase compound graphene oxide |
| CN106191985A (en) * | 2016-06-30 | 2016-12-07 | 武汉科技大学 | A kind of preparation method of stainless steel surfaces nanometic zinc oxide rod array |
| CN108923025A (en) * | 2018-06-12 | 2018-11-30 | 北京英耐时新能源科技有限公司 | A kind of preparation process of efficient pulp of lithium ion battery |
| CN111313037A (en) * | 2020-02-27 | 2020-06-19 | 贵研铂业股份有限公司 | Reduced graphene oxide loaded platinum-cobalt-nickel powder and preparation method thereof |
| CN111450831A (en) * | 2020-05-22 | 2020-07-28 | 北京化工大学 | High-performance graphene-loaded mesoporous nickel-iron alloy electrocatalyst and preparation method thereof |
| CN113611887A (en) * | 2021-08-04 | 2021-11-05 | 北京航空航天大学 | Preparation method of low-platinum-loading carbon corrosion-resistant fuel cell catalyst |
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103915633A (en) * | 2014-04-01 | 2014-07-09 | 上海交通大学 | Composite carbon fiber-loaded metal catalyst as well as preparation method and application thereof |
| CN103915633B (en) * | 2014-04-01 | 2016-08-24 | 上海交通大学 | A kind of composite carbon fiber supported metal catalyst and its preparation method and application |
| CN103910356B (en) * | 2014-04-28 | 2019-07-16 | 南京新月材料科技有限公司 | A kind of preparation method of three-dimensional grapheme |
| CN103910356A (en) * | 2014-04-28 | 2014-07-09 | 南京新月材料科技有限公司 | Preparation method of three-dimensional graphene |
| 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 |
| CN104667869A (en) * | 2015-02-11 | 2015-06-03 | 四川大学 | Method for removing endocrine disrupter in water by utilizing monopersulfate and ferro-cobalt loaded dual-phase compound graphene oxide |
| CN106191985A (en) * | 2016-06-30 | 2016-12-07 | 武汉科技大学 | A kind of preparation method of stainless steel surfaces nanometic zinc oxide rod array |
| CN106191985B (en) * | 2016-06-30 | 2019-03-19 | 武汉科技大学 | A kind of preparation method of stainless steel surface nanometic zinc oxide rod array |
| CN108923025A (en) * | 2018-06-12 | 2018-11-30 | 北京英耐时新能源科技有限公司 | A kind of preparation process of efficient pulp of lithium ion battery |
| CN108923025B (en) * | 2018-06-12 | 2020-10-23 | 北京英耐时新能源科技有限公司 | Efficient preparation process of lithium ion battery slurry |
| CN111313037A (en) * | 2020-02-27 | 2020-06-19 | 贵研铂业股份有限公司 | Reduced graphene oxide loaded platinum-cobalt-nickel powder and preparation method thereof |
| CN111450831A (en) * | 2020-05-22 | 2020-07-28 | 北京化工大学 | High-performance graphene-loaded mesoporous nickel-iron alloy electrocatalyst and preparation method thereof |
| CN113611887A (en) * | 2021-08-04 | 2021-11-05 | 北京航空航天大学 | Preparation method of low-platinum-loading carbon corrosion-resistant fuel cell catalyst |
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Application publication date: 20130724 |