CN102895997A - Preparation method for direct methanol fuel cell supported Pt-based anode catalyst - Google Patents
Preparation method for direct methanol fuel cell supported Pt-based anode catalyst Download PDFInfo
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- CN102895997A CN102895997A CN2012104106415A CN201210410641A CN102895997A CN 102895997 A CN102895997 A CN 102895997A CN 2012104106415 A CN2012104106415 A CN 2012104106415A CN 201210410641 A CN201210410641 A CN 201210410641A CN 102895997 A CN102895997 A CN 102895997A
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Abstract
The invention discloses a preparation method for a direct methanol fuel cell supported Pt-based anode catalyst. The preparation method comprises the following steps: adding graphene to N-methyl pyrrolidinone to prepare dispersion liquid; preparing polyaniline to be N-methyl pyrrolidinone solution in a mass ratio of the graphene to the polyaniline; mixing the dispersion liquid with the polyaniline solution, filtering the mixture; dissolving the filter cake to deionized water and solvent of ethylene glycol; adding chloroplatinic acid to the solution of the filter cake in the total mass ratio of Pt to graphene and polyaniline; and acquiring the direct methanol fuel cell supported Pt-based anode catalyst with the grain size of 2-3 nm by reacting, filtering, washing and drying. The preparation method has the advantages of a simple process, good controllability of conditions during the process, improving the dispersion of the graphene, the distribution uniformity of the Pt catalyst in the graphene space and the stability of the catalyst. As shown by the test, the catalyst has excellent performances.
Description
Technical field
The present invention relates to a kind of preparation method of DMFC support type Pt base anode catalyst, belong to the anode catalysts for direct methanol fuel cell technology.
Background technology
DMFC (DMFC) is a kind of novel TRT that directly chemical energy is converted into the environment-friendly type of electric energy.Its outstanding advantages is that the methyl alcohol source is abundant, low price, and its aqueous solution is easy to carry about with one and stores.Therefore DMFC is particularly suitable for the movable power source as various uses.And anode electrocatalyst is the core component of DMFC, and the quality of its performance directly has influence on the performance of fuel cell.The DMFC anode adopts loaded catalyst.The research direction of present DMFC anode catalyst mainly concentrates on and adopts grapheme material is carrier, improves spatial distribution state and the catalytic performance of its catalyst.Yet the Graphene of structural integrity is the two dimensional crystal that is combined by the hexatomic ring that does not contain any labile bond, and chemical stability is high, and its surface is inert condition, a little less than the interaction of Pt metallic particles.And stronger Van der Waals force is arranged between graphene film and the sheet, produce easily and assemble, make it be difficult to water-soluble and commonly used organic solvent.In order to make Graphene in application process, can be good at disperseing, usually need to carry out functionalization to it.The functionalization of Graphene not only solved the solubility problem in eelctro-catalyst system preparation process, and also providing can the inducing catalyst load or the functional group of embedding, even directly makes catalyst and Graphene compound with covalent bond or non-covalent bond.
At present the method for modifying of the Graphene carrier of DMFC anode catalyst is mainly adopted mode (the Yanchun Zhao of polymer in-situ polymerization on the Graphene top layer, Lu Zhan, Jianniao Tian, Sulian Nie, Zhen Ning, Electrochimica Acta, 2011,56:1967-1972).The basic process of the method is, Graphene and polymer monomer are mixed, add the initator initiation reaction and obtain the graphene-polymer composite. for example adopt the method for in-situ polymerization to prepare the graphene-polypyrrole compound, first Graphene and pyrrole monomer are dissolved in the alkaline solution, under freezing point temperature, add again initator and carry out polymerization.The method is that polymer foil is coated on the graphene sheet layer, has realized the modification of Graphene.But owing in polymer fluid, need to add simultaneously grapheme material, so that the viscosity of polymer fluid changes, the control that causes polymeric reaction condition is difficulty comparatively, occur easily polymer only be gathered in occur that the conducting polymer modified or organic molecule be gathered in graphene sheet layer certain a bit or bulk deposition in the edge of graphene sheet layer.Graphene after will modifying is as carrier, with conducting polymer or organic molecule during as the site of anchored platinum catalyst, caused metallic particles spatial distribution and particle diameter inhomogeneous and particle diameter is excessive (about 6nm).The sub-ability of the conduction of conducting polymer is weaker than grapheme material, when graphene sheet layer is all coated by conducting polymer, to affect the transmission of electronics at the carbon hexatomic ring, reduced electric conductivity and other premium properties of catalyst carrier, and then cause the decline of whole eelctro-catalyst performance.In said method, need to be dissolved in simultaneously Graphene and polymer monomer in the alkaline aqueous solution, so be not suitable for the polymer-modified and modification of polymerization reaction take place under the acid condition, this is so that this preparation method's narrow application range is not suitable for large-scale application.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of DMFC load type platinum anode catalyst.The method has the simple and controlled characteristics of condition of process, and prepared catalyst Pt particle is evenly distributed at carrier surface, uniform particle diameter, and catalyst performance is high.
The present invention is realized by the following technical programs, a kind of preparation method of DMFC support type Pt base anode catalyst, described support type Pt base anode catalyst is that composite take Graphene and polyaniline is as carrier, the carrier loaded catalyst gross mass that accounts for is 20% Pt, it is characterized in that comprising following process:
Be the graphene nanometer sheet of 1～20nm with thickness, add in the 1-METHYLPYRROLIDONE, ultrasonic dispersion, being mixed with concentration is 0.5～2mg/ml graphene dispersing solution; Mass ratio by Graphene and polyaniline is 1:(0.01～0.025), polyaniline is added the solution that Uniform Dispersion in the 1-METHYLPYRROLIDONE makes 0.2～0.3mg/ml polyaniline, at normal temperature with under stirring, graphene dispersing solution is mixed 12～36h with the solution of polyaniline, after filtration, filter cake is dissolved in the mixed solvent of deionized water and ethylene glycol, through stirring and ultrasonic dispersion, get the graphene solution of Polyaniline-modified, be 0.025:1 by the quality of Pt and Graphene and polyaniline total mass ratio, 110～130 ℃ of temperature with under stirring, graphene solution adding molar concentration to Polyaniline-modified is the 0.1M platinum acid chloride solution, behind reaction 3～5h, after filtration, filter cake washs respectively to the solution without till the ethylene glycol with deionized water and ethanol, vacuum drying, and obtaining particle diameter is the DMFC support type Pt base anode catalyst of 2～3nm.
Advantage of the present invention, the method process is simple, and process conditional controllability is good, has improved the dispersiveness of Graphene and Pt catalyst granules in the stability of Graphene spatial distribution uniformity and catalyst.Show through electro-chemical test, in acid medium, this catalyst to the catalytic performance of methanol electro-oxidizing reaction apparently higher than without grapheme modified or in-situ polymerization grapheme modified be the catalyst performance of carrier.
Description of drawings
Fig. 1 is the prepared catalyst of the embodiment of the invention 1 cyclic voltammetry curve that is used for the DMFC anodic methanol oxidation and the comparison diagram of the prepared Pt/ graphen catalyst of Comparative Examples 1 for the cyclic voltammetry curve of DMFC anodic methanol oxidation.
Among the figure: cyclic curve 1 is the embodiment of the invention 1, and cyclic curve 2 is Comparative Examples 1.
Fig. 2 is the prepared catalyst of the embodiment of the invention 2 cyclic voltammetry curve that is used for the DMFC anodic methanol oxidation and the comparison diagram of the prepared Pt/ graphen catalyst of Comparative Examples 1 for the cyclic voltammetry curve of DMFC anodic methanol oxidation.
Among the figure: cyclic curve 1 is the embodiment of the invention 2, and cyclic curve 2 is Comparative Examples 1.
Fig. 3 is the prepared catalyst of the embodiment of the invention 2 cyclic voltammetry curve that is used for the DMFC anodic methanol oxidation and the comparison diagram of the prepared Pt/ polyaniline-graphite alkene catalyst of Comparative Examples 2 for the cyclic voltammetry curve of DMFC anodic methanol oxidation.
Among the figure: cyclic curve 1 is the embodiment of the invention 2, and cyclic curve 2 is Comparative Examples 2.
Fig. 4 is the prepared catalyst of the embodiment of the invention 5 cyclic voltammetry curve that is used for the DMFC anodic methanol oxidation and the comparison diagram of the prepared Pt/ polyaniline-graphite alkene catalyst of Comparative Examples 3 for the cyclic voltammetry curve of DMFC anodic methanol oxidation.
Among the figure: cyclic curve 1 is the embodiment of the invention 5, and cyclic curve 2 is Comparative Examples 3.
Fig. 5 is the transmission electron microscope photo of the prepared catalyst of the embodiment of the invention 5.As can be seen from the figure the particle diameter of Pt is 2～3nm in the prepared catalyst.
The specific embodiment
Embodiment 1:
0.1g 5～20nm Graphene microplate adds in the 100ml deionized water, ultrasonic 2h under the cell pulverization machine, and filter membrane filters; After the filtration Graphene be dissolved in the 200ml 1-METHYLPYRROLIDONE, normal temperature magnetic agitation 3min, ultrasonic 2h obtains the dispersion liquid of Graphene; 2.04mg polyaniline joins 10mlN-crassitude ketone solvent; Get the 1-METHYLPYRROLIDONE solution of polyaniline, the 1-METHYLPYRROLIDONE solution of 200ml graphene dispersing solution and 10ml polyaniline is mixed magnetic agitation 24h; Filter with filter membrane, filter cake is dissolved in the mixed solution of 50ml deionized water and 300ml ethylene glycol, stir, ultrasonic 1h, adding 13.06ml concentration is the platinum acid chloride solution of 0.1M, treats that temperature rises to 125 ℃, reaction 4h.Cool the temperature to room temperature, filter, filter cake washs respectively with deionized water and ethanol; 75 ℃ of lower vacuum drying, obtaining particle diameter is the Pt/ polyaniline-graphite alkene catalyst of 2～3nm.Getting this catalyst 3mg is dissolved in ethanol and the Nafion solvent, after it is coated on the carbon paper as anode, be 0～1.24V at current potential, sweep speed under the 10mV/s, the cyclic voltammetry curve figure that records methanol oxidation by the analog fuel battery as shown in Figure 1, catalyst performance of the present invention obviously is better than Comparative Examples 1 prepared catalyst performance as can be seen from Figure.
Embodiment 2:
Other conditions of present embodiment are identical with embodiment 1, and different is: change 5～20nm Graphene microplate into 1～5nm graphene nanometer sheet, obtaining particle diameter is the Pt/ polyaniline-graphite alkene catalyst of 2～3nm.Getting this catalyst 3mg is dissolved in ethanol and the Nafion solvent, after it is coated on the carbon paper as anode, be 0～1.24V at current potential, sweep speed under the 10mV/s, recorded the cyclic voltammetry curve figure of methanol oxidation by the analog fuel battery shown in accompanying drawing 1 and accompanying drawing 2, catalyst performance of the present invention obviously is better than Comparative Examples 1 and Comparative Examples 2 prepared catalyst performances as can be seen from Figure.
Embodiment 3:
0.1g1～5nm graphene nanometer sheet is dissolved in the 100ml deionized water, ultrasonic 2h under the cell pulverization machine filters; The Graphene that obtains is dissolved in the 200ml 1-METHYLPYRROLIDONE, mechanical agitation, and ultrasonic 2h adds the 25mg polyaniline in the 10mlN-methyl pyrrolidone solution, and the 1-METHYLPYRROLIDONE solution of 200ml dispersion liquid and 10ml polyaniline is mixed, and stirs 12h; Filter, filter cake is dissolved in the mixed solution of the deionized water of 1:4 and ethylene glycol, stir, ultrasonic, adding 16ml concentration is the chloroplatinic acid of 0.1M, treats that temperature rises to 125 ℃, reaction 4h.Cool the temperature to room temperature, sediment spends the washing of ionic hydration ethanol, filters; 75 ℃ of lower vacuum drying, obtaining particle diameter is the Pt/ polyaniline-graphite alkene catalyst of 2～3nm.Getting this catalyst 3mg is dissolved in ethanol and the Nafion solvent, after it is coated on the carbon paper as anode, be 0～1.24V at current potential, sweep speed under the 10mV/s, the cyclic voltammetry curve that is recorded methanol oxidation by the analog fuel battery shows that catalyst performance of the present invention is better than the catalyst that Graphene is carrier.
Embodiment 4:
It is identical with embodiment 3 that this implements other conditions, and the consumption that only changes polyaniline is 11.1mg, adds accordingly the chloroplatinic acid that 14.21ml concentration is 0.1M, drying, and obtaining particle diameter is the Pt/ polyaniline-graphite alkene eelctro-catalyst of 2～3nm.Getting this catalyst 3mg is dissolved in ethanol and the Nafion solvent, after it is coated on the carbon paper as anode, be 0～1.24V at current potential, sweep speed under the 10mV/s, the cyclic voltammetry curve that is recorded methanol oxidation by the analog fuel battery shows that catalyst performance of the present invention is better than the catalyst that Graphene is carrier.
Embodiment 5:
With the standby graphite oxide of Hummers legal system, get 0.1g and be dissolved in the deionized water, ultrasonic 2h places hydrothermal reaction kettle, and 180 ℃ of lower reaction 3h are cooled to room temperature, filter; 0.1g Graphene (thickness is less than 10 layers) is dissolved in the 100ml deionized water, ultrasonic 2h under the cell pulverization machine filters; Be dissolved in the 200ml 1-METHYLPYRROLIDONE, stir, ultrasonic 2h, the 1-METHYLPYRROLIDONE solution of adding polyaniline (2.04mg) stirs 12h; Filter, filter cake is dissolved in the mixed solution of the deionized water of 1:4 and ethylene glycol, stir, ultrasonic, adding 13.06ml concentration is the chloroplatinic acid of 0.1M, treats that temperature rises to 125 ℃, reaction 4h.Cool the temperature to room temperature, sediment spends the washing of ionic hydration ethanol, filters; 75 ℃ of lower vacuum drying, obtaining particle diameter is the Pt/ polyaniline-graphite alkene catalyst of 2～3nm.Getting this catalyst 3mg is dissolved in ethanol and the Nafion solvent, after it is coated on the carbon paper as anode, be 0～1.24V at current potential, sweep speed under the 10mV/s, the cyclic voltammetry curve that records methanol oxidation by the analog fuel battery as shown in Figure 4, catalyst performance of the present invention obviously is better than Comparative Examples 3 prepared catalyst performances as can be seen from Figure.
Comparative Examples 1:
The Graphene microplate of 0.1g 1～5nm is added in the 100ml deionized water, and ultrasonic 2h under the cell pulverization machine is 20 with the aperture
The Filter paper filtering of m is dissolved in filter cake in the mixed solution of 50ml deionized water and 300ml ethylene glycol, stirs, and ultrasonic 1h, adding 12.8ml concentration is the platinum acid chloride solution of 0.1M, treats that temperature rises to 125 ℃, reaction 4h.Cool the temperature to room temperature, sediment filters with deionized water and ethanol washing; 75 ℃ of lower vacuum drying, obtaining particle diameter is the Pt/ graphen catalyst of 2～3nm.Get this catalyst 3mg and be dissolved in ethanol and the Nafion solvent, after it is coated on the carbon paper as anode, be 0～1.24V at current potential, sweep speed under the 10mV/s, the cyclic voltammetry curve figure that records methanol oxidation by the analog fuel battery is as shown in Figure 1.
Comparative Examples 2:
The graphene nanometer sheet of 0.1g 1～5nm is added in the 100ml deionized water, and ultrasonic 2h under the cell pulverization machine is 20 with the aperture
The Filter paper filtering of m is dissolved in filter cake in the hydrochloric acid solution of 100ml 1M, adds aniline again in system, at normal pressure, temperature is under 0～5 ℃, drips the hydrochloric acid solution of ammonium persulfate, reaction 12h, filter, again filter cake is dissolved in the mixed solution of 50ml deionized water and 300ml ethylene glycol, stir, ultrasonic 1h, adding 13.06ml concentration is the platinum acid chloride solution of 0.1M, treats that temperature rises to 125 ℃, reaction 4h.Cool the temperature to room temperature, sediment filters with deionized water and ethanol washing; 75 ℃ of lower vacuum drying, obtaining particle diameter is the Pt/ polyaniline-graphite alkene catalyst of 2～3nm.Get this catalyst 3mg and be dissolved in ethanol and the Nafion solvent, after it is coated on the carbon paper as anode, be 0～1.24V at current potential, sweep speed under the 10mV/s, the cyclic voltammetry curve figure that records methanol oxidation by the analog fuel battery is as shown in Figure 3.
Comparative Examples 3:
The Graphene of 0.1g hydro-thermal method redox graphene preparation is added in the 100ml deionized water, and ultrasonic 2h under the cell pulverization machine is 20 with the aperture
The Filter paper filtering of m is dissolved in filter cake in the hydrochloric acid solution of 100ml 1M, adds aniline again in system, at normal pressure, temperature is under 0～5 ℃, drips the hydrochloric acid solution of ammonium persulfate, reaction 12h, filter, again filter cake is dissolved in the mixed solution of 50ml deionized water and 300ml ethylene glycol, stir, ultrasonic 1h, adding 13.06ml concentration is the platinum acid chloride solution of 0.1M, treats that temperature rises to 125 ℃, reaction 4h.Cool the temperature to room temperature, sediment filters with deionized water and ethanol washing; 75 ℃ of lower vacuum drying, obtaining particle diameter is the Pt/ polyaniline-graphite alkene catalyst of 2～3nm.Get this catalyst 3mg and be dissolved in ethanol and the Nafion solvent, after it is coated on the carbon paper as anode, be 0～1.24V at current potential, sweep speed under the 10mV/s, the cyclic voltammetry curve figure that records methanol oxidation by the analog fuel battery is as shown in Figure 4.
Claims (1)
1. the preparation method of DMFC support type Pt base anode catalyst, described support type Pt base anode catalyst is that composite take Graphene and polyaniline is as carrier, the carrier loaded catalyst gross mass that accounts for is 20% Pt, it is characterized in that comprising following process: be the graphene nanometer sheet of 1～20nm with thickness, add in the 1-METHYLPYRROLIDONE, ultrasonic dispersion, being mixed with concentration is 0.5～2mg/ml graphene dispersing solution; Mass ratio by Graphene and polyaniline is 1:(0.01～0.025), polyaniline is added the solution that Uniform Dispersion in the 1-METHYLPYRROLIDONE makes 0.2～0.3mg/ml polyaniline, at normal temperature with under stirring, graphene dispersing solution is mixed 12～36h with the solution of polyaniline, after filtration, filter cake is dissolved in the mixed solvent of deionized water and ethylene glycol, through stirring and ultrasonic dispersion, get the graphene solution of Polyaniline-modified, be 0.025:1 by the quality of Pt and Graphene and polyaniline total mass ratio, 110～130 ℃ of temperature with under stirring, graphene solution adding molar concentration to Polyaniline-modified is the 0.1M platinum acid chloride solution, behind reaction 3～5h, after filtration, filter cake washs respectively to the solution without till the ethylene glycol with deionized water and ethanol, vacuum drying, and obtaining particle diameter is the DMFC support type Pt base anode catalyst of 2～3nm.
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Cited By (7)
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| CN103372428A (en) * | 2013-05-10 | 2013-10-30 | 南昌大学 | Preparation method of nitrogen-doped graphene loaded platinum nano-particle catalyst |
| CN103623864A (en) * | 2013-11-25 | 2014-03-12 | 天津大学 | Method for preparing Pt-based anode catalyst of direct liquid flow methanol fuel cell |
| CN105576257A (en) * | 2015-12-21 | 2016-05-11 | 太原理工大学 | Method using underwater arc discharge to prepare graphene supported Pt catalyst |
| CN105633423A (en) * | 2015-12-27 | 2016-06-01 | 同济大学 | Preparation method for reduced graphene-polyaniline loaded manganece-cerium oxide electro-catalyst |
| CN105817240A (en) * | 2016-04-15 | 2016-08-03 | 华中科技大学 | Pt doped phosphatizing cobalt bead catalyst carried by methanol carbon dioxide and preparation method of Pt doped phosphatizing cobalt bead catalyst |
| CN108610788A (en) * | 2016-12-26 | 2018-10-02 | 天津喜蕊科技有限公司 | A kind of formaldehyde of radiator bottom eliminates the preparation method of coating |
| CN113571712A (en) * | 2021-07-06 | 2021-10-29 | 天津新氢动力科技有限公司 | Preparation method of corrosion-resistant catalyst layer of fuel cell for forklift |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103372428A (en) * | 2013-05-10 | 2013-10-30 | 南昌大学 | Preparation method of nitrogen-doped graphene loaded platinum nano-particle catalyst |
| CN103372428B (en) * | 2013-05-10 | 2015-01-21 | 南昌大学 | Preparation method of nitrogen-doped graphene loaded platinum nano-particle catalyst |
| CN103623864A (en) * | 2013-11-25 | 2014-03-12 | 天津大学 | Method for preparing Pt-based anode catalyst of direct liquid flow methanol fuel cell |
| CN105576257A (en) * | 2015-12-21 | 2016-05-11 | 太原理工大学 | Method using underwater arc discharge to prepare graphene supported Pt catalyst |
| CN105633423A (en) * | 2015-12-27 | 2016-06-01 | 同济大学 | Preparation method for reduced graphene-polyaniline loaded manganece-cerium oxide electro-catalyst |
| CN105817240A (en) * | 2016-04-15 | 2016-08-03 | 华中科技大学 | Pt doped phosphatizing cobalt bead catalyst carried by methanol carbon dioxide and preparation method of Pt doped phosphatizing cobalt bead catalyst |
| CN108610788A (en) * | 2016-12-26 | 2018-10-02 | 天津喜蕊科技有限公司 | A kind of formaldehyde of radiator bottom eliminates the preparation method of coating |
| CN113571712A (en) * | 2021-07-06 | 2021-10-29 | 天津新氢动力科技有限公司 | Preparation method of corrosion-resistant catalyst layer of fuel cell for forklift |
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Application publication date: 20130130 |