CN117199414A - Anode catalyst of hydrogen fuel cell and preparation method and application thereof - Google Patents
Anode catalyst of hydrogen fuel cell and preparation method and application thereof Download PDFInfo
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- CN117199414A CN117199414A CN202311252661.9A CN202311252661A CN117199414A CN 117199414 A CN117199414 A CN 117199414A CN 202311252661 A CN202311252661 A CN 202311252661A CN 117199414 A CN117199414 A CN 117199414A
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- 239000003054 catalyst Substances 0.000 title claims abstract description 79
- 239000000446 fuel Substances 0.000 title claims abstract description 26
- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 21
- 239000001257 hydrogen Substances 0.000 title claims abstract description 20
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 60
- 229920000767 polyaniline Polymers 0.000 claims abstract description 41
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 19
- 239000000203 mixture Substances 0.000 claims abstract description 15
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000002105 nanoparticle Substances 0.000 claims abstract description 10
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 9
- 239000002131 composite material Substances 0.000 claims abstract description 8
- 229910052751 metal Inorganic materials 0.000 claims abstract description 7
- 239000002184 metal Substances 0.000 claims abstract description 7
- 239000000758 substrate Substances 0.000 claims abstract description 6
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 19
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 8
- 239000011259 mixed solution Substances 0.000 claims description 8
- 239000003638 chemical reducing agent Substances 0.000 claims description 7
- 239000002245 particle Substances 0.000 claims description 6
- 238000006722 reduction reaction Methods 0.000 claims description 6
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 4
- 239000002270 dispersing agent Substances 0.000 claims description 4
- 239000002904 solvent Substances 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 3
- 239000012279 sodium borohydride Substances 0.000 claims description 3
- 229910000033 sodium borohydride Inorganic materials 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- KLFRPGNCEJNEKU-FDGPNNRMSA-L (z)-4-oxopent-2-en-2-olate;platinum(2+) Chemical compound [Pt+2].C\C([O-])=C\C(C)=O.C\C([O-])=C\C(C)=O KLFRPGNCEJNEKU-FDGPNNRMSA-L 0.000 claims description 2
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims description 2
- 229960005070 ascorbic acid Drugs 0.000 claims description 2
- 235000010323 ascorbic acid Nutrition 0.000 claims description 2
- 239000011668 ascorbic acid Substances 0.000 claims description 2
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 claims description 2
- 239000006229 carbon black Substances 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- 239000008103 glucose Substances 0.000 claims description 2
- 229910021389 graphene Inorganic materials 0.000 claims description 2
- 238000011068 loading method Methods 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 238000009210 therapy by ultrasound Methods 0.000 claims description 2
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 2
- 230000000694 effects Effects 0.000 abstract description 9
- 231100000572 poisoning Toxicity 0.000 abstract description 6
- 230000000607 poisoning effect Effects 0.000 abstract description 6
- 230000008859 change Effects 0.000 abstract description 4
- 239000012528 membrane Substances 0.000 abstract description 4
- 239000000463 material Substances 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 9
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 8
- 238000009826 distribution Methods 0.000 description 5
- 239000007789 gas Substances 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
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- 238000003917 TEM image Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 239000011159 matrix material Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 229910002849 PtRu Inorganic materials 0.000 description 2
- 238000000026 X-ray photoelectron spectrum Methods 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 239000002803 fossil fuel Substances 0.000 description 2
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 238000000634 powder X-ray diffraction Methods 0.000 description 2
- 238000001291 vacuum drying Methods 0.000 description 2
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910002091 carbon monoxide Inorganic materials 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000002484 cyclic voltammetry Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- CFQCIHVMOFOCGH-UHFFFAOYSA-N platinum ruthenium Chemical compound [Ru].[Pt] CFQCIHVMOFOCGH-UHFFFAOYSA-N 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000000967 suction filtration Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
- 238000001075 voltammogram Methods 0.000 description 1
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Abstract
The invention belongs to the technical field of fuel cell catalysts, and particularly relates to a hydrogen fuel cell anode catalyst, a preparation method and application thereof. The catalyst comprises a carbon-polyaniline composite substrate and metal platinum nano particles loaded on the substrate; the carbon-polyaniline composite material is a mixture of carbon and polyaniline. The preparation method of the hydrogen fuel cell anode catalyst provided by the invention has the advantages that the preparation process is simple, compared with the commercial Pt/C catalyst, the preparation method has smaller change by simple polyaniline addition, the material is cheap and easy to obtain, the CO poisoning resistance and stability of the Pt/C catalyst are greatly improved on the premise of not influencing the activity of the catalyst, and the large-scale commercial application of the proton exchange membrane fuel cell is facilitated.
Description
Technical Field
The invention belongs to the technical field of fuel cell catalysts, and particularly relates to a hydrogen fuel cell anode catalyst, a preparation method and application thereof.
Background
The shortage of fossil fuel and the change of environment promote the main body of the energy structure to change from fossil fuel to cleaner hydrogen energy, and the proton exchange membrane fuel cell taking hydrogen as fuel is expected to play an important role in a hydrogen energy system due to the characteristics of high efficiency, high energy density, quick start and low scale cost. The utilization of gray hydrogen is a problem that proton exchange membrane fuel cells need to face based on the high cost and low yield of large-scale green hydrogen production technology. The reformed gas inevitably carries CO and H 2 S、NH 3 When the reformed gas containing these impurity gases is supplied to the fuel cell, the performance of the fuel cell is significantly degraded. The most harmful of the impurity gases is CO, trace CO can seriously obstruct the adsorption and reaction of hydrogen at the working temperature of the fuel cell, and further increasing the concentration of the hydrogen can lead to the cost index increase on the basis of the content of CO in the current gas, so that the development of the CO-resistant catalyst of the fuel cell is a promising strategy.
Disclosure of Invention
In order to solve the problem of CO poisoning of the anode catalyst of the fuel cell, the invention provides the anode catalyst of the fuel cell, and a preparation method and application thereof.
In order to achieve the above object, the technical scheme of the present invention is as follows:
in one aspect, the invention provides a platinum-based hydrogen fuel cell anode catalyst comprising a carbon-polyaniline composite substrate and metallic platinum nanoparticles supported on the substrate;
the carbon-polyaniline composite material is a mixture of carbon and polyaniline.
In the above technical scheme, further, the polyaniline content in the carbon-polyaniline composite material is 1-80wt%, preferably 5-20wt%.
In the catalyst, the loading of the metal platinum nano particles is 10-40wt%.
In the technical scheme, further, the specific surface active area of the catalyst is more than 50m 2 /g Pt 。
In the above technical scheme, further, the particle size of the metal platinum nanoparticle is 1.5-5nm.
In another aspect, the present invention provides a method for preparing the anode catalyst, which includes the following steps:
(1) Mixing polyaniline and a carbon source in a dispersing agent, and performing ultrasonic dispersion to obtain a mixed solution;
(2) And (3) dissolving the mixed solution obtained in the step (1) and a platinum source in a solvent, adding a reducing agent into the mixed solution for reduction reaction, washing and drying to obtain the catalyst.
In the above technical scheme, further, the dispersing agent is any one of glycol and ethanol, the temperature of the ultrasound is 10-50 ℃ and the time is 10-60min.
In the above technical scheme, further, the carbon source is any one of conductive carbon black XC-72R and reduced graphene oxide.
In the above technical solution, further, the platinum source is any one of chloroplatinic acid, platinum acetylacetonate and the like.
In the above technical scheme, further, the solvent is any one of glycol, ethanol and water; the reducing agent is any one of sodium borohydride, ascorbic acid and glucose; the mass ratio of the reducing agent to the metal salt is 1:50.
in the above technical scheme, further, the temperature of the reduction reaction is 80-100 ℃, and the time of the reduction reaction is 3 hours.
The invention also provides an application of the anode catalyst in a hydrogen fuel cell.
The beneficial effects of the invention are as follows:
compared with the prior art, in the fuel cell anode catalyst provided by the invention, the metal platinum nano particles are deposited on the surface of the matrix of the mixture of polyaniline and carbon, the platinum nano particles on the surface of the mixture of polyaniline and carbon are uniformly distributed, and the size distribution is between 1.5 and 5nm, so that the particle size of platinum on the surface of the Pt/C catalyst is reduced to a certain extent compared with that of platinum on the surface of the Pt/C catalyst serving as a reference. Polyaniline adsorbs water to form surface active oxygen, and the formed surface active oxygen can assist the oxidation of CO on the surface of platinum, so that more active sites are provided for the oxidation of hydrogen, the catalytic activity of the anode catalyst under high CO concentration is guaranteed, and the CO resistance activity of the anode catalyst under experimental conditions is superior to that of commercial platinum ruthenium catalysts.
The preparation method of the hydrogen fuel cell anode catalyst provided by the invention has the advantages that the preparation process is simple, compared with the commercial Pt/C catalyst, the preparation method has smaller change and low-cost and easily-obtained materials by adding simple polyaniline in the synthesis process of the commercial Pt/C catalyst, the CO poisoning resistance and stability of the Pt/C catalyst are greatly improved on the premise of not influencing the activity of the catalyst, and the large-scale commercial application of the proton exchange membrane fuel cell is facilitated.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are needed in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic illustration of a process flow for preparing a hydrogen fuel cell anode catalyst according to the present invention;
FIG. 2 is a representation of the structure and morphology of the catalysts of example 1, example 5, a is a scanning electron microscope image of example 1, b is an elemental distribution diagram of example 1, c and e are TEM images at low and high power for the catalyst of example 1, where e is the particle size distribution diagram of the catalyst, d and f are TEM images at low and high power for the catalyst of example 5, where f is the particle size distribution diagram of the catalyst;
FIG. 3 is an X-ray powder diffraction pattern and an X-ray photoelectron spectrum of the catalysts of example 1, example 3 and comparative example 1, a is an X-ray powder diffraction pattern b is an X-ray photoelectron spectrum; FIG. 4 is a Fourier transform infrared plot of the catalysts of example 3 and comparative example 1;
FIG. 5 is a graph of the electrochemical activity of the catalysts of example 1, example 3, example 4 and comparative examples 1, 2, a being a linear voltammogram, b being a bar graph of the mass activity at a potential of 0.7V, c being a cyclic voltammogram d being the electrochemically active area;
FIG. 6 is a graph showing the CO resistance test of the catalysts of example 1 and comparative example 1, a is a graph showing the LSV test of the catalyst of comparative example 1 before and after the CO poisoning process, b is a graph showing the CO-strip of the catalyst of comparative example 1, c is a graph showing the LSV test of the catalyst of example 1 before and after the CO poisoning process, and d is a graph showing the CO-strip of the catalyst of example 1;
FIG. 7 is a potentiostatic curve of the catalysts of examples 1-5, comparative examples 1-2.
Detailed Description
The present invention will be described in further detail with reference to the drawings and examples, in order to make the objects, technical solutions and advantages of the present invention more apparent. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
Example 1
The present example provides a platinum-based hydrogen fuel cell anode catalyst consisting of a matrix of a conductive carbon black XC-72R and polyaniline mixture and metallic platinum nanoparticles supported on the matrix;
the preparation method of the catalyst comprises the following steps:
s1, taking a 50ml round-bottom flask, and adding 30mg of a mixture of conductive carbon black XC-72 and polyaniline, wherein the polyaniline content in the mixture is 5wt%;
s2, adding 30ml of ethylene glycol into the mixture, and performing ultrasonic treatment at 15 ℃ for 1h to obtain a mixed solution;
s3, adding 1.425ml of ethylene glycol with the concentration of 0.03g/ml of chloroplatinic acid into the mixed solution, magnetically stirring for 30min, adding sodium borohydride which is taken as a reducing agent and is dissolved in 30ml of ethylene glycol solution, heating the mixture to 90 ℃ by using an oil bath, and keeping the temperature for 3h at the rotating speed of 450 rpm;
s4, carrying out suction filtration, washing three times by using ethanol and water, placing the mixture into a vacuum drying oven, and standing overnight at 80 ℃ in the vacuum drying oven, wherein the obtained catalyst is named as Pt/C-PANI-5.
Example 2
The catalyst was prepared as in example 1, except that the polyaniline content in the mixture of conductive carbon black XC-72 and polyaniline was 10wt%, and the catalyst obtained was designated Pt/C-PANI-10.
Example 3
The catalyst was prepared as in example 1, except that the polyaniline content in the mixture of conductive carbon black XC-72 and polyaniline was 20wt%, and the catalyst obtained was designated Pt/C-PANI-20.
Example 4
The catalyst was prepared as in example 1, except that the polyaniline content in the mixture of conductive carbon black XC-72 and polyaniline was 40wt%, and the catalyst obtained was designated Pt/C-PANI-40.
Example 5
The catalyst was prepared as in example 1, except that the polyaniline content in the mixture of conductive carbon black XC-72 and polyaniline was 80wt%, and the catalyst obtained was designated Pt/C-PANI-80.
Comparative example 1
The catalyst was prepared as in example 1, except that the support contained only conductive carbon black XC-72, and the resulting catalyst was designated Pt/C.
Comparative example 2
Commercial PtRu/C catalysts (TKK, 60%).
Analysis of results:
from fig. 2, it can be seen that polyaniline is discretely distributed on the surface of carbon black, macroscopically without aggregation, and from TEM images, it can be seen that the addition amount of polyaniline has little influence on the particle size of the Pt/C catalyst. From fig. 3 and 4, it can be seen that polyaniline has been added to the Pt/C catalyst, and that the addition of polyaniline has no effect on the spatial structure and crystal plane distribution of platinum in the catalyst, and that the electronic structure of platinum has not been changed. As can be seen from fig. 5, the addition of polyaniline has little effect on the activity of the catalyst HOR. However, as can be seen from FIG. 6, the addition of polyaniline reduces the decay of the catalyst before and after CO poisoning. Meanwhile, as can be seen from fig. 7, the addition of low-content polyaniline has a positive effect on CO resistance of the catalyst, and this trend gradually decreases with increasing addition amount of polyaniline, but is still stronger than that of the sample to which polyaniline is not added. Under the given low-concentration CO experiment condition, the activity and HOR performance decay rate of the Pt/C-PANI catalyst are better than those of the Pt/C catalyst and PtRu/C catalyst.
The above embodiments are only for illustrating the present invention, not for limiting the present invention, and various changes and modifications may be made by one of ordinary skill in the relevant art without departing from the spirit and scope of the present invention, and therefore, all equivalent technical solutions are also within the scope of the present invention, and the scope of the present invention is defined by the claims.
Claims (10)
1. A hydrogen fuel cell anode catalyst, characterized in that the catalyst comprises a carbon-polyaniline composite substrate and metal platinum nanoparticles supported on the substrate;
the carbon-polyaniline composite material is a mixture of carbon and polyaniline.
2. The catalyst of claim 1, wherein the polyaniline content of the carbon-polyaniline composite material is 1-80wt%.
In the catalyst, the loading of the metal platinum nano particles is 10-40wt%.
3. The catalyst of claim 1, wherein the catalyst has a specific surface area > 50m 2 /g Pt 。
4. The catalyst of claim 1, wherein the metallic platinum nanoparticles have a particle size of 1.5-5nm.
5. A method for preparing the anode catalyst according to any one of claims 1 to 4, comprising the steps of:
(1) Mixing polyaniline and a carbon source in a dispersing agent, and performing ultrasonic dispersion to obtain a mixed solution;
(2) And (3) dissolving the mixed solution obtained in the step (1) and a platinum source in a solvent, adding a reducing agent into the mixed solution for reduction reaction, washing and drying to obtain the catalyst.
6. The preparation method according to claim 5, wherein the dispersing agent is any one of ethylene glycol and ethanol, and the ultrasonic treatment is performed at a temperature of 10-50 ℃ for 10-60min.
7. The method according to claim 5, wherein the carbon source is any one of an XC-72R carbon black and a reduced graphene oxide.
8. The method according to claim 5, wherein the platinum source is any one of chloroplatinic acid and platinum acetylacetonate.
9. The preparation method according to claim 5, wherein the solvent is any one of ethylene glycol, ethanol and water; the reducing agent is any one of sodium borohydride, ascorbic acid and glucose; the mass ratio of the reducing agent to the platinum source is 1:50; the temperature of the reduction reaction is 80-100 ℃, and the time of the reduction reaction is 3 hours.
10. Use of an anode catalyst according to any one of claims 1-4 in a hydrogen fuel cell.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202311252661.9A CN117199414A (en) | 2023-09-26 | 2023-09-26 | Anode catalyst of hydrogen fuel cell and preparation method and application thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202311252661.9A CN117199414A (en) | 2023-09-26 | 2023-09-26 | Anode catalyst of hydrogen fuel cell and preparation method and application thereof |
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| CN202311252661.9A Pending CN117199414A (en) | 2023-09-26 | 2023-09-26 | Anode catalyst of hydrogen fuel cell and preparation method and application thereof |
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- 2023-09-26 CN CN202311252661.9A patent/CN117199414A/en active Pending
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