CN104785248A - Preparation method of hydrogen fuel cell catalyst and catalyst prepared by method - Google Patents
Preparation method of hydrogen fuel cell catalyst and catalyst prepared by method Download PDFInfo
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- CN104785248A CN104785248A CN201510221091.6A CN201510221091A CN104785248A CN 104785248 A CN104785248 A CN 104785248A CN 201510221091 A CN201510221091 A CN 201510221091A CN 104785248 A CN104785248 A CN 104785248A
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- polypyrrole nanotube
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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 hydrogen fuel cell catalyst and the catalyst prepared by the method. The preparation method comprises the steps of: (1) dissolving ferric trichloride in a methyl orange solution, then adding a pyrrole monomer to the methyl orange solution, and carrying out stirring reaction for 10-30 hours; (2) dispersing polypyrrole nanotubes, alkali metal hydroxides and dihalogenation alkane in a first organic solvent, and reacting to obtain halogenated polypyrrole nanotubes; (c) dispersing the halogenated polypyrrole nanotubes and methylimidazole in the first organic solvent, and reacting; (d) dispersing the modified polypyrrole nanotubes and polyvinyl pyrrolidone in water, subsequently adding a chloroplatinate solution, carrying out stirring reaction for 2-5 hours at the temperature of 10-30 DEG C, then adding sodium borohydride and continuously carrying out stirring reaction; and (e) putting platinum-loaded polypyrrole nanotubes in an inert gas atmosphere, and calcining for 1-5 hours at the temperature of 700-1100 DEG C. A carbon material formed after calcination has a relatively high specific surface area and can synergistically take effect with platinum nano particles, thus improving the catalytic efficiency.
Description
Technical field
The invention belongs to catalyst material field, relate to a kind of preparation method of catalyst for fuel cell, the preparation method being specifically related to a kind of hydrogen fuel cell catalyst and the catalyst prepared by the method.
Background technology
In a fuel cell, the chemical reaction of fuel directly can change into electric energy, and then generation current.In other words, fuel cell comprises electricity generation system, and within the system, fuel (hydrogen or methyl alcohol) directly can change into electric energy with the chemical reaction of oxidant (oxygen or air).Fuel cell utilizes the continuous generation electric energy of the fuel provided from its outside, burns or charge and discharge cycles without the need to carrying out.The generator of the hot energy that the energy efficiency of fuel cell produces higher than utilizing fuel combustion significantly, because fuel cell is by the domination of the thermodynamic efficiency limit.
Usually, in fuel cell, the chemical reaction of fuel and oxidant produces water.At present, the fuel cell on market comprises polyelectrolyte film fuel cell (PEMFC) and phosphoric acid fuel cell (PAFC), and they all use acidic electrolysis bath.Wherein, use the chemical reaction equation in the fuel cell of acidic electrolysis bath as follows:
Anode: 2H
2→ 4H
++ 4e
-;
Negative electrode: O
2+ 4H
++ 4e
-→ 2H
2o;
Overall: 2H
2+ O
2→ 2H
2o+ energy.
That is, when fuel and oxidant are supplied to anode and negative electrode respectively simultaneously, the fuel caused by catalyst in the oxidation reaction of anode and the oxygen reduction reaction produce power at negative electrode, thus produces electronics.The efficiency of catalyst improves the important parameter of fuel cell efficiency, and noble metal can be used as platinum the most stable in electrochemical reaction catalyst the most.But pure noble metal may be too expensive, to such an extent as to can not be commercial in fuel cell; Therefore need to prepare low price and the higher hydrogen fuel cell of efficiency.
Summary of the invention
The present invention seeks to the preparation method that a kind of hydrogen fuel cell catalyst is provided to overcome the deficiencies in the prior art.
For achieving the above object, the technical solution used in the present invention is: a kind of preparation method of hydrogen fuel cell catalyst, and it comprises the following steps:
A ferric trichloride is dissolved in methyl orange solution by (), then add pyrrole monomer wherein, stirring reaction 10 ~ 30 hours, and crossing leaching filter residue, is colourless with deionized water rinsing filter residue to filtrate, and dry removing moisture content obtains polypyrrole nanotube subsequently;
B () gets described polypyrrole nanotube, alkali metal hydroxide, alkylene dihalide are scattered in the first organic solvent, be placed in 40 ~ 80 DEG C of stirring reactions 10 ~ 30 hours, cross leaching filter residue, alternately rinse filter residue repeatedly with deionized water, the second organic solvent, drier removing moisture content obtains halogenation polypyrrole nanotube;
C () gets described halogenation polypyrrole nanotube and methylimidazole is scattered in described first organic solvent, be placed in 40 ~ 80 DEG C of stirring reactions 10 ~ 30 hours, cross leaching filter residue, alternately rinse filter residue repeatedly with deionized water, the second organic solvent, drier removing moisture content obtains modified polypyrrole nanotube;
D () gets described modified polypyrrole nanotube, PVP is scattered in water, add chloroplatinate solution subsequently 10 ~ 30 DEG C of stirring reactions 2 ~ 5 hours, add sodium borohydride again and continue stirring reaction 10 ~ 20 hours, centrifugal rear deionized water, the second organic solvent alternately rinse filter residue repeatedly, dryly must carry platinum polypyrrole nanotube;
E described year platinum polypyrrole nanotube was placed in inert gas atmosphere by (), 700 ~ 1100 DEG C of calcinings 1 ~ 5 hour.
Optimally, the mol ratio of described ferric trichloride, described methyl orange and described pyrrole monomer is 1 ~ 2: 0.1 ~ 0.3: 1 ~ 2.
Optimally, described alkali metal hydroxide is potassium hydroxide or NaOH, described alkylene dihalide is 1,4-dibromobutane, Isosorbide-5-Nitrae-dichloroetane, 1,6-dichloro hexane or 1,6-dibromo-hexane, described first organic solvent is DMF, ethyl acetate or dimethyl sulfoxide (DMSO), and described second organic solvent is methyl alcohol, ethanol or acetone.
Optimally, the mass ratio of described polypyrrole nanotube, described alkali metal hydroxide and described saturated dihalide is 3 ~ 5: 5 ~ 10: 10 ~ 20.
Optimally, the mass ratio of described halogenation polypyrrole nanotube and described methylimidazole is 1: 5 ~ 10.
Optimally, the ratio of described modified polypyrrole nanotube, described PVP, described chloroplatinate and described sodium borohydride is 1 ~ 5mg: 20 ~ 25mg: 0.03 ~ 0.05mmol: 0.1 ~ 0.2mmol.
Another object of the present invention is to provide a kind of hydrogen fuel cell catalyst, and it is prepared from by the preparation method of above-mentioned hydrogen fuel cell catalyst.
Because technique scheme is used, the present invention compared with prior art has following advantages: the preparation method of hydrogen fuel cell catalyst of the present invention, by forming nano platinum particle in the outer grafting of polypyrrole pipe, and calcined the material with carbon element forming supported platinum nano particle, the method is simple to operate on the one hand, be conducive to the material with carbon element forming lower-cost supported platinum nano particle on the other hand, and creating beyond thought effect: the material with carbon element formed after calcining has higher specific area and can be formed with nano platinum particle and act synergistically, thus raising catalytic efficiency.
Detailed description of the invention
The preparation method of hydrogen fuel cell catalyst of the present invention, it comprises the following steps: ferric trichloride is dissolved in methyl orange solution by (a), add pyrrole monomer wherein again, stirring reaction 10 ~ 30 hours, cross leaching filter residue, be colourless with deionized water rinsing filter residue to filtrate, dry removing moisture content obtains polypyrrole nanotube subsequently; B () gets described polypyrrole nanotube, alkali metal hydroxide, alkylene dihalide are scattered in the first organic solvent, be placed in 40 ~ 80 DEG C of stirring reactions 10 ~ 30 hours, cross leaching filter residue, alternately rinse filter residue repeatedly with deionized water, the second organic solvent, drier removing moisture content obtains halogenation polypyrrole nanotube; C () gets described halogenation polypyrrole nanotube and methylimidazole is scattered in described first organic solvent, be placed in 40 ~ 80 DEG C of stirring reactions 10 ~ 30 hours, cross leaching filter residue, alternately rinse filter residue repeatedly with deionized water, the second organic solvent, drier removing moisture content obtains modified polypyrrole nanotube; D () gets described modified polypyrrole nanotube, PVP is scattered in water, add chloroplatinate solution subsequently 10 ~ 30 DEG C of stirring reactions 2 ~ 5 hours, add sodium borohydride again and continue stirring reaction 10 ~ 20 hours, centrifugal rear deionized water, the second organic solvent alternately rinse filter residue repeatedly, dryly must carry platinum polypyrrole nanotube; E described year platinum polypyrrole nanotube was placed in inert gas atmosphere by (), 700 ~ 1100 DEG C of calcinings 1 ~ 5 hour.The method is simple to operate on the one hand, be conducive to the material with carbon element forming lower-cost supported platinum nano particle on the other hand, and creating beyond thought effect: the material with carbon element formed after calcining has higher specific area and can be formed with nano platinum particle and act synergistically, thus raising catalytic efficiency.
The mol ratio of ferric trichloride, methyl orange and pyrrole monomer is preferably 1 ~ 2: 0.1 ~ 0.3: 1 ~ 2.Alkali metal hydroxide is conventional those, preferred potassium hydroxide or NaOH; Two halogen atoms of alkylene dihalide are positioned on the carbon atom at the two ends of alkane substitute, preferred Isosorbide-5-Nitrae-dibromobutane, Isosorbide-5-Nitrae-dichloroetane, 1,6-dichloro hexane or 1,6-dibromo-hexane; First organic solvent is common high boiling organic solvent, be preferably N, dinethylformamide (DMF), ethyl acetate or dimethyl sulfoxide (DMSO) (DMSO), the second organic solvent is common low boiling point organic solvent, is preferably methyl alcohol, ethanol or acetone.The mass ratio of polypyrrole nanotube, alkali metal hydroxide and saturated dihalide is preferably 3 ~ 5: 5 ~ 10: 10 ~ 20; The mass ratio of halogenation polypyrrole nanotube and methylimidazole is preferably 1: 5 ~ 10; The ratio of modified polypyrrole nanotube, PVP, chloroplatinate and sodium borohydride is 1 ~ 5mg: 20 ~ 25mg: 0.03 ~ 0.05mmol: 0.1 ~ 0.2mmol.It should be noted that the preparation owing to relating to nano platinum particle, the control for material ratio is very important, otherwise can cause the reduction of catalyst efficiency, is not therefore that those skilled in the art can be drawn by limited number of time experiment.
To be described in detail to the preferred embodiment of the invention below:
Embodiment 1
The present embodiment provides a kind of preparation method of hydrogen fuel cell catalyst, and it comprises the following steps:
A 0.243g (1.5mmol) ferric trichloride is dissolved in 30ml methyl orange solution (methyl orange concentration is 0.5mmol/L) by (), add 105 microlitres (1.5mmol) pyrrole monomer more wherein, stirring reaction 10 hours, cross leaching filter residue, be colourless with deionized water rinsing filter residue to filtrate, remove moisture with dry 24h in the vacuum drying chamber being placed on 60 DEG C and obtain polypyrrole nanotube;
B () gets 0.03g polypyrrole nanotube, 0.05gKOH powder, 0.1437g1,4-dibromobutane ultrasonic disperse is in DMF, be placed in 80 DEG C of stirring reactions 10 hours, cross leaching filter residue, alternately rinse filter residue five times with deionized water, ethanol, then the vacuum drying chamber being placed in 60 DEG C dry 24h removing moisture content obtains bromination polypyrrole nanotube;
C () gets 0.025g bromination polypyrrole nanotube and 0.2g methylimidazole ultrasonic disperse in DMF, be placed in 40 DEG C of stirring reactions 30 hours, cross leaching filter residue, alternately rinse filter residue repeatedly with deionized water, ethanol, then the vacuum drying chamber being placed in 60 DEG C dry 24h removing moisture content obtains modified polypyrrole nanotube;
D () gets 1mg modified polypyrrole nanotube, 25mg PVP (PVP) is scattered in 18ml water, add 1ml potassium chloroplatinate solution (30mmol/L) subsequently 10 DEG C of stirring reactions 5 hours, add 4.5ml sodium borohydride (0.04mol/L) again and continue stirring reaction 20 hours, centrifugal rear deionized water, ethanol alternately rinse filter residue 3 ~ 5 times, dryly must carry platinum polypyrrole nanotube;
E () will carry platinum polypyrrole nanotube and be placed in inert gas atmosphere, 700 DEG C of calcinings 5 hours.
Embodiment 2
The present embodiment provides a kind of preparation method of hydrogen fuel cell catalyst, and it comprises the following steps:
A 1mmol ferric trichloride is dissolved in 20ml methyl orange solution (methyl orange concentration is 0.5mmol/L) by (), add 1mmol pyrrole monomer wherein again, stirring reaction 30 hours, cross leaching filter residue, be colourless with deionized water rinsing filter residue to filtrate, remove moisture with dry 24h in the vacuum drying chamber being placed on 60 DEG C and obtain polypyrrole nanotube;
B () gets 0.05g polypyrrole nanotube, 0.1gKOH powder, 0.2g1,4-dichloroetane ultrasonic disperse is in DMSO, be placed in 40 DEG C of stirring reactions 30 hours, cross leaching filter residue, alternately rinse filter residue three times with deionized water, methyl alcohol, then the vacuum drying chamber being placed in 60 DEG C dry 24h removing moisture content obtains chlorination polypyrrole nanotube;
C () gets 0.025g chlorination polypyrrole nanotube and 0.125g methylimidazole ultrasonic disperse in DMSO, be placed in 80 DEG C of stirring reactions 10 hours, cross leaching filter residue, alternately rinse filter residue five times with deionized water, methyl alcohol, then the vacuum drying chamber being placed in 60 DEG C dry 24h removing moisture content obtains modified polypyrrole nanotube;
D () gets 5mg modified polypyrrole nanotube, 25mg PVP (PVP) is scattered in 18ml water, add 1ml potassium chloroplatinate solution (50mmol/L) subsequently 30 DEG C of stirring reactions 2 hours, add 5ml sodium borohydride (0.02mol/L) again and continue stirring reaction 10 hours, centrifugal rear deionized water, ethanol alternately rinse filter residue 3 ~ 5 times, dryly must carry platinum polypyrrole nanotube;
E () will carry platinum polypyrrole nanotube and be placed in inert gas atmosphere, 1100 DEG C of calcinings 1 hour.
Embodiment 3
The present embodiment provides a kind of preparation method of hydrogen fuel cell catalyst, and it comprises the following steps:
A 2mmol ferric trichloride is dissolved in 60ml methyl orange solution (methyl orange concentration is 0.5mmol/L) by (), add 2mmol pyrrole monomer wherein again, stirring reaction 20 hours, cross leaching filter residue, be colourless with deionized water rinsing filter residue to filtrate, remove moisture with dry 24h in the vacuum drying chamber being placed on 60 DEG C and obtain polypyrrole nanotube;
B () gets 0.04g polypyrrole nanotube, 0.06gKOH powder, 0.15g1,6-dichloro hexane ultrasonic disperse is in ethyl acetate, be placed in 50 DEG C of stirring reactions 20 hours, cross leaching filter residue, alternately rinse filter residue five times with deionized water, acetone, then the vacuum drying chamber being placed in 60 DEG C dry 24h removing moisture content obtains chlorination polypyrrole nanotube;
C () gets 0.025g chlorination polypyrrole nanotube and 0.25g methylimidazole ultrasonic disperse in ethyl acetate, be placed in 60 DEG C of stirring reactions 15 hours, cross leaching filter residue, alternately rinse filter residue three times with deionized water, ethyl acetate, then the vacuum drying chamber being placed in 60 DEG C dry 24h removing moisture content obtains modified polypyrrole nanotube;
D () gets 3mg modified polypyrrole nanotube, 20mg PVP (PVP) is scattered in 18ml water, add 1ml potassium chloroplatinate solution (40mmol/L) subsequently 20 DEG C of stirring reactions 3 hours, add 5ml sodium borohydride (0.03mol/L) again and continue stirring reaction 15 hours, centrifugal rear deionized water, ethanol alternately rinse filter residue 3 ~ 5 times, dryly must carry platinum polypyrrole nanotube;
E () will carry platinum polypyrrole nanotube and be placed in inert gas atmosphere, 1000 DEG C of calcinings 2 hours.
Above-described embodiment is only for illustrating technical conceive of the present invention and feature; its object is to person skilled in the art can be understood content of the present invention and implement according to this; can not limit the scope of the invention with this; all equivalences done according to Spirit Essence of the present invention change or modify, and all should be encompassed within protection scope of the present invention.
Claims (7)
1. a preparation method for hydrogen fuel cell catalyst, is characterized in that, it comprises the following steps:
A ferric trichloride is dissolved in methyl orange solution by (), then add pyrrole monomer wherein, stirring reaction 10 ~ 30 hours, and crossing leaching filter residue, is colourless with deionized water rinsing filter residue to filtrate, and dry removing moisture content obtains polypyrrole nanotube subsequently;
B () gets described polypyrrole nanotube, alkali metal hydroxide, alkylene dihalide are scattered in the first organic solvent, be placed in 40 ~ 80 DEG C of stirring reactions 10 ~ 30 hours, cross leaching filter residue, alternately rinse filter residue repeatedly with deionized water, the second organic solvent, drier removing moisture content obtains halogenation polypyrrole nanotube;
C () gets described halogenation polypyrrole nanotube and methylimidazole is scattered in described first organic solvent, be placed in 40 ~ 80 DEG C of stirring reactions 10 ~ 30 hours, cross leaching filter residue, alternately rinse filter residue repeatedly with deionized water, the second organic solvent, drier removing moisture content obtains modified polypyrrole nanotube;
D () gets described modified polypyrrole nanotube, PVP is scattered in water, add chloroplatinate solution subsequently 10 ~ 30 DEG C of stirring reactions 2 ~ 5 hours, add sodium borohydride again and continue stirring reaction 10 ~ 20 hours, centrifugal rear deionized water, the second organic solvent alternately rinse filter residue repeatedly, dryly must carry platinum polypyrrole nanotube;
E described year platinum polypyrrole nanotube was placed in inert gas atmosphere by (), 700 ~ 1100 DEG C of calcinings 1 ~ 5 hour.
2. the preparation method of hydrogen fuel cell catalyst according to claim 1, is characterized in that: the mol ratio of described ferric trichloride, described methyl orange and described pyrrole monomer is 1 ~ 2: 0.1 ~ 0.3: 1 ~ 2.
3. the preparation method of hydrogen fuel cell catalyst according to claim 1, it is characterized in that: described alkali metal hydroxide is potassium hydroxide or NaOH, described alkylene dihalide is 1,4-dibromobutane, Isosorbide-5-Nitrae-dichloroetane, 1,6-dichloro hexane or 1,6-dibromo-hexane, described first organic solvent is DMF, ethyl acetate or dimethyl sulfoxide (DMSO), and described second organic solvent is methyl alcohol, ethanol or acetone.
4. the preparation method of hydrogen fuel cell catalyst according to claim 3, is characterized in that: the mass ratio of described polypyrrole nanotube, described alkali metal hydroxide and described saturated dihalide is 3 ~ 5: 5 ~ 10: 10 ~ 20.
5. the preparation method of hydrogen fuel cell catalyst according to claim 4, is characterized in that: the mass ratio of described halogenation polypyrrole nanotube and described methylimidazole is 1: 5 ~ 10.
6. the preparation method of hydrogen fuel cell catalyst according to claim 1, is characterized in that: the ratio of described modified polypyrrole nanotube, described PVP, described chloroplatinate and described sodium borohydride is 1 ~ 5mg: 20 ~ 25mg: 0.03 ~ 0.05mmol: 0.1 ~ 0.2mmol.
7. the hydrogen fuel cell catalyst that in claim 1 to 6 prepared by arbitrary described preparation method.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106602089A (en) * | 2017-02-04 | 2017-04-26 | 成都育芽科技有限公司 | Non-platinum-based catalyst used for fuel cell and preparation method for catalyst |
| CN106654310A (en) * | 2016-12-12 | 2017-05-10 | 成都育芽科技有限公司 | High-activity high-stability catalyst for fuel cell and preparation method of catalyst |
| CN107916159A (en) * | 2017-12-07 | 2018-04-17 | 山东冬瑞高新技术开发有限公司 | A kind of preparation method of lube oil additive |
| CN109216033A (en) * | 2018-09-04 | 2019-01-15 | 渤海大学 | A kind of quantum dot sensitized preparation method used for solar batteries to electrode material |
| CN109301262A (en) * | 2018-08-13 | 2019-02-01 | 浙江润涞科技服务有限公司 | A kind of hydrogen fuel cell catalyst of green non-pollution |
| CN115207378A (en) * | 2022-07-25 | 2022-10-18 | 陕西科技大学 | Polypyrrole nanotube electrocatalyst and preparation method and application thereof |
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2015
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106654310A (en) * | 2016-12-12 | 2017-05-10 | 成都育芽科技有限公司 | High-activity high-stability catalyst for fuel cell and preparation method of catalyst |
| CN106602089A (en) * | 2017-02-04 | 2017-04-26 | 成都育芽科技有限公司 | Non-platinum-based catalyst used for fuel cell and preparation method for catalyst |
| CN107916159A (en) * | 2017-12-07 | 2018-04-17 | 山东冬瑞高新技术开发有限公司 | A kind of preparation method of lube oil additive |
| CN107916159B (en) * | 2017-12-07 | 2020-10-09 | 淄博惠华石油添加剂有限公司 | Preparation method of lubricating oil additive |
| CN109301262A (en) * | 2018-08-13 | 2019-02-01 | 浙江润涞科技服务有限公司 | A kind of hydrogen fuel cell catalyst of green non-pollution |
| CN109301262B (en) * | 2018-08-13 | 2022-06-14 | 浙江哈克雷斯传动科技有限公司 | Green pollution-free hydrogen fuel cell catalyst |
| CN109216033A (en) * | 2018-09-04 | 2019-01-15 | 渤海大学 | A kind of quantum dot sensitized preparation method used for solar batteries to electrode material |
| CN115207378A (en) * | 2022-07-25 | 2022-10-18 | 陕西科技大学 | Polypyrrole nanotube electrocatalyst and preparation method and application thereof |
| CN115207378B (en) * | 2022-07-25 | 2023-09-05 | 陕西科技大学 | Polypyrrole nanotube electrocatalyst and preparation method and application thereof |
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Effective date of registration: 20151029 Address after: 201612 Shanghai City, Songjiang District Road, 1500 Lane 134, room 602 Applicant after: Gao Dongqing Address before: 200082 Shanghai city Yangpu District Yangshupu Road No. 2300 room B05-18 4B Applicant before: Shanghai Bo Xuan Energy Science Co., Ltd |
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