CN114243054B - Storage method of fuel cell catalyst slurry - Google Patents
Storage method of fuel cell catalyst slurry Download PDFInfo
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- CN114243054B CN114243054B CN202111526640.2A CN202111526640A CN114243054B CN 114243054 B CN114243054 B CN 114243054B CN 202111526640 A CN202111526640 A CN 202111526640A CN 114243054 B CN114243054 B CN 114243054B
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- catalyst
- slurry
- catalyst slurry
- storage
- perfluorosulfonic acid
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- 239000003054 catalyst Substances 0.000 title claims abstract description 85
- 239000002002 slurry Substances 0.000 title claims abstract description 70
- 238000003860 storage Methods 0.000 title claims abstract description 39
- 238000000034 method Methods 0.000 title claims abstract description 26
- 239000000446 fuel Substances 0.000 title claims abstract description 10
- 229920000554 ionomer Polymers 0.000 claims abstract description 36
- 238000003756 stirring Methods 0.000 claims abstract description 26
- UQSQSQZYBQSBJZ-UHFFFAOYSA-N fluorosulfonic acid Chemical compound OS(F)(=O)=O UQSQSQZYBQSBJZ-UHFFFAOYSA-N 0.000 claims abstract description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 16
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 6
- 238000013019 agitation Methods 0.000 claims description 6
- 229910052799 carbon Inorganic materials 0.000 claims description 6
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 4
- 239000013543 active substance Substances 0.000 claims description 4
- 239000012046 mixed solvent Substances 0.000 claims description 4
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 239000011149 active material Substances 0.000 claims description 2
- 238000001816 cooling Methods 0.000 claims 4
- 239000002245 particle Substances 0.000 abstract description 17
- 238000001179 sorption measurement Methods 0.000 abstract description 14
- 238000005054 agglomeration Methods 0.000 abstract description 5
- 230000002776 aggregation Effects 0.000 abstract description 5
- 230000000694 effects Effects 0.000 abstract description 4
- 230000009286 beneficial effect Effects 0.000 abstract description 3
- 239000007787 solid Substances 0.000 abstract description 3
- 230000000052 comparative effect Effects 0.000 description 24
- 239000012528 membrane Substances 0.000 description 7
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Substances [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 5
- 229920003937 Aquivion® Polymers 0.000 description 4
- 230000010287 polarization Effects 0.000 description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- 229920000557 Nafion® Polymers 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 238000010586 diagram Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 229910052697 platinum Inorganic materials 0.000 description 2
- 238000005057 refrigeration Methods 0.000 description 2
- 238000000518 rheometry Methods 0.000 description 2
- 238000004062 sedimentation Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 230000009471 action Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000005253 cladding Methods 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 239000003273 ketjen black Substances 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 230000000607 poisoning effect Effects 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 150000003460 sulfonic acids Chemical class 0.000 description 1
- 230000036962 time dependent Effects 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M8/00—Fuel cells; Manufacture thereof
- H01M8/04—Auxiliary arrangements, e.g. for control of pressure or for circulation of fluids
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M8/00—Fuel cells; Manufacture thereof
- H01M8/04—Auxiliary arrangements, e.g. for control of pressure or for circulation of fluids
- H01M8/04007—Auxiliary arrangements, e.g. for control of pressure or for circulation of fluids related to heat exchange
- H01M8/04029—Heat exchange using liquids
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M8/00—Fuel cells; Manufacture thereof
- H01M8/04—Auxiliary arrangements, e.g. for control of pressure or for circulation of fluids
- H01M8/04007—Auxiliary arrangements, e.g. for control of pressure or for circulation of fluids related to heat exchange
- H01M8/04052—Storage of heat in the fuel cell system
-
- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Landscapes
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Sustainable Development (AREA)
- Sustainable Energy (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Catalysts (AREA)
- Inert Electrodes (AREA)
Abstract
The invention provides a storage method of fuel cell catalyst slurry, the catalyst slurry comprises perfluorosulfonic acid ionomer, and the EW value of the perfluorosulfonic acid ionomer is 625-980; the storage method is to stir the catalyst slurry at 2-10 ℃ at fixed time. The storage tank used for storage is provided with a stirring device and a refrigerating device, and the refrigerating layer on the periphery of the storage tank can provide a lower temperature for the storage of the slurry, so that the agglomeration of catalyst particles and the further adsorption of ionomer on the catalyst are prevented, and the stability of the microstructure of the catalyst slurry is maintained. The stirring device provides a timing stirring effect for the slurry and prevents the solid particles from settling. The storage method can maintain stable slurry structure, thereby greatly prolonging the storage time of the catalyst slurry and being beneficial to the storage and transportation of the slurry. In addition, the storage method ensures uniformity of battery performance and can improve output performance of the whole electric pile.
Description
Technical Field
The invention belongs to the field of fuel cells, and particularly relates to a storage method of fuel cell catalyst slurry.
Background
In commercial large-scale production of fuel cells, catalyst slurry needs to be reserved to meet the continuous production demand. In addition, some businesses that are not capable of producing catalyst slurries will also face transportation problems for the catalyst slurries. Therefore, in this case, storage of the catalyst slurry will be unavoidable. It is well known that catalyst slurries are heterogeneous, unstable systems, and over time the slurry will settle. In addition, storage of the catalyst slurry can also cause changes in the microstructure of the slurry, resulting in inconsistent catalytic layer structure and cell performance of the catalyst slurry after storage with fresh slurry. Such non-uniformity in the performance of the individual cells will reduce the overall output performance of the stack. Meanwhile, the distribution of water, gas and heat of the galvanic pile is uneven, and a series of problems such as opposite poles, local hot spots and the like can occur. Therefore, how to store the fuel cell catalyst slurry is important.
Disclosure of Invention
The present invention has been made to solve the above-mentioned problems occurring in the prior art, and an object of the present invention is to provide a storage method of a catalyst slurry for a fuel cell, which is capable of maintaining the stability of the microstructure of the catalyst slurry so that the microstructure of the catalyst slurry after storage is consistent with that of fresh slurry, thereby maintaining the uniformity of the cell performance.
The technical scheme of the invention is as follows:
a method of storing a fuel cell catalyst slurry comprising a perfluorosulfonic acid ionomer having an EW value of 625 to 980, the method comprising periodically agitating the catalyst slurry at a temperature of 2 ℃ to 10 ℃.
Based on the above technical scheme, preferably, the timing stirring includes a stirring interval and a stirring duration, the stirring interval does not perform stirring action on the catalyst slurry, the stirring interval is 60-120 min, and the stirring duration is 30-60 min.
Based on the above technical scheme, preferably, the storage is realized through the holding vessel, the holding vessel contains refrigerating plant and agitating unit, refrigerating plant's refrigeration layer cladding is at the periphery of holding vessel.
Based on the above technical solution, preferably, the catalyst slurry further comprises a mixed solvent of a catalyst, water and alcohol; in the catalyst slurry, the mass fraction of the catalyst and the perfluorosulfonic acid ionomer, namely the solid content, is 0.1-3%.
Based on the technical scheme, preferably, the catalyst comprises a carbon carrier and a catalytic active substance, and the mass ratio of the perfluorosulfonic acid ionomer to the catalyst carbon carrier in the catalyst slurry is 0.3-1.2:1; in the catalyst, the mass percentage of active substances is 10-70%. The carbon carrier is one of Ketjen Black, vulcan XC-72 and BP 2000. The catalytically active material is one of Pt, ptCo, ptIr, ptPd, ptRu, ptAu.
Based on the technical scheme, preferably, the alcohol is volatile alcohol, the volatile alcohol is one of methanol, ethanol, isopropanol and n-propanol, and the mass percentage of the volatile alcohol in the mixed solvent is 10% -90%.
Advantageous effects
(1) The storage method adopts stirring and low-temperature means, and the regular stirring can prevent the sedimentation of catalyst particles, so that compared with continuous stirring, the regular stirring is beneficial to saving energy consumption on the basis of not affecting the performance of catalyst slurry.
(2) The storage method of the present invention is applicable to catalyst slurries containing perfluorosulfonic acid ionomers having an EW of 650-980, which have a lower proportion of backbone units such that the adsorption of the ionomer onto the catalyst is strongly time dependent, i.e., the adsorption of the ionomer increases with time. The increased adsorption of the ionomer results in coverage of the active sites of the catalyst, which enhances the poisoning effect of the ionomer, and also increases the resistance of oxygen to passage through the ionomer membrane, increasing mass transfer resistance, resulting in reduced cell performance. The high temperature can lead to the reduction of electrostatic repulsive force and the occurrence of bridging attractive force, so that the agglomeration of catalyst particles is accelerated, the increase of catalyst particle size is caused, and meanwhile, further adsorption of ionomer on the catalyst is promoted. In addition, the storage method of the invention ensures the uniformity of the battery performance and can improve the output performance of the whole electric pile.
Drawings
FIG. 1 is a schematic diagram of a storage tank according to the present invention.
FIG. 2 is a flow chart of the catalyst slurry of comparative examples 1, 2 and example 1 of the present invention.
FIG. 3 is a graph of catalyst slurry particle size and ionomer adsorption ratio for comparative examples 1, 2, 5 and example 1 of the present invention.
FIG. 4 is a graph showing polarization curves of the membrane electrode prepared from the catalyst slurry of comparative examples 1, 2, 5 and example 1 according to the present invention under hydrogen air conditions.
FIG. 5 is a graph showing polarization curves of the catalyst pastes of comparative example 3 and comparative example 4 according to the present invention under hydrogen air conditions.
Detailed Description
The invention will now be described in further detail with reference to the accompanying drawings.
The specific operation process is as follows:
comparative example 1
A dispersed catalyst slurry comprising an Aquivion perfluorosulfonic acid ionomer having an EW value of 720.
Comparative example 2
The dispersed catalyst slurry containing the Aquivion perfluorosulfonic acid ionomer having an EW value of 720 was allowed to stand at 20 ℃ for 2 days.
Comparative example 3
A dispersed catalyst slurry comprising Nafion perfluorosulfonic acid ionomer having an EW value of 1100.
Comparative example 4
The dispersed catalyst slurry containing Nafion perfluorinated sulfonic acid ionomer with EW value of 1100 is stored for 2 days under the condition of 20 ℃ and stirring interval of 60min and stirring time of 30 min.
Comparative example 5
The dispersed catalyst slurry containing the Aquivion perfluorosulfonic acid ionomer with an EW value of 720 is stored for 2 days at 20 ℃ with stirring interval of 60min and stirring time of 30 min.
Example 1
The dispersed catalyst slurry containing the Aquivion perfluorosulfonic acid ionomer with an EW value of 720 was stored for 2 days at 5 ℃ with stirring intervals of 60min and stirring time of 30 min.
FIG. 1 is a schematic diagram of a storage tank according to the present invention. The refrigeration layer of the storage tank can provide a lower temperature for the storage of the slurry, preventing agglomeration of the catalyst particles and further adsorption of the ionomer on the catalyst, thereby maintaining the stability of the microstructure of the catalyst slurry. The stirring device provides a timing stirring effect for the slurry and prevents the sedimentation of solid particles.
Steady state rheology tests were performed on the above catalyst slurries. As shown in fig. 2, which is a graph showing a comparison of steady state rheology of comparative examples 1, 2 and example 1, the catalyst slurry of example 1 shows the same rheological properties as the catalyst slurry of comparative example 1, while the rheological properties of the catalyst slurry of comparative example 2 are significantly changed, indicating that the storage method of the present invention can maintain the stability of the microstructure of the catalyst slurry.
The above catalyst slurry was diluted 1000-fold with the same solvent as the catalyst slurry for particle size measurement. And filtering the catalyst slurry by using a disposable filter membrane filter, drying the filtrate, weighing the mass of the non-adsorbed ionomer, and comparing the mass with the amount of the added ionomer to obtain the adsorption rate of the ionomer on the catalyst. Fig. 3 is a graph comparing particle sizes and ionomer adsorption rates of comparative examples 1, 2, and 5 and example 1. The particle size and ionomer adsorption of the catalyst slurry of example 1 were the same as those of comparative example 1, while the particle size of comparative example 2 was larger, indicating that the catalyst particles were agglomerated while the ionomer adsorption was increased and the catalyst slurry structure was changed. The particle size of comparative example 5 increased less significantly than comparative example 2 due to the stirring effect, however, the higher storage temperature accelerated the agglomeration of the catalyst particles, resulting in an increase in the particle size of comparative example 5, while allowing further adsorption of the ionomer on the catalyst. Therefore, the storage method can prevent the agglomeration of the catalyst particles and the further adsorption of the ionomer on the catalyst, thereby maintaining the stable structure of the catalyst slurry, greatly prolonging the storage time of the slurry and being beneficial to the storage and transportation of the slurry.
The catalyst slurry is sprayed on a proton exchange membrane to prepare a catalytic layer, wherein the loading capacity of cathode platinum is 0.1mg/cm 2 Anode platinum loading was 0.2mg/cm 2 And then hot-pressing the membrane electrode with the gas diffusion layer to obtain the membrane electrode. The resulting membrane electrode was subjected to electrochemical testing, and fig. 4 is a graph showing the polarization curves of comparative examples 1, 2, 5 and example 1 under hydrogen air conditions. Similarly, example 1 exhibited battery performance equivalent to that of comparative example 1While the battery performance of comparative examples 2 and 5 was degraded, it was shown that the low temperature and agitation of the storage method of the present invention can maintain the structural characteristics of the catalyst slurry, so that the microstructure of the catalyst layer was not changed, and the uniformity of the battery performance was ensured. Fig. 5 is a polarization graph of comparative example 3 and comparative example 4. It can be clearly seen that the catalyst slurry using Nafion perfluorosulfonic acid ionomer having an EW of 1100 did not significantly differ in cell performance before and after storage, since ionomers having an EW higher than 980 have a higher proportion of backbone units and the adsorption of the ionomer did not change over time. The invention provides a storage method for catalyst slurry with a certain EW value, which solves the problem of difficult storage of the catalyst slurry.
The present invention is not limited to the above-mentioned embodiments, and any person skilled in the art, using the above-mentioned disclosure, can make various changes or modifications equivalent to the equivalent embodiments without departing from the scope of the present invention.
Claims (7)
1. A method of storing a fuel cell catalyst slurry comprising a perfluorosulfonic acid ionomer, wherein the perfluorosulfonic acid ionomer has an EW value of 625-980; the storage method is to stir the catalyst slurry at 2-10 ℃ at fixed time.
2. The method of claim 1, wherein the timed agitation comprises an agitation interval and an agitation period, the agitation interval being 60 to 120 minutes and the agitation period being 30 to 60 minutes.
3. The method of claim 1, wherein the storing is performed by a storage tank comprising a cooling device and a stirring device, the cooling device comprising a cooling layer, the cooling layer surrounding the storage tank.
4. The storage method according to claim 1, wherein the catalyst slurry further comprises a catalyst and a mixed solvent of water and alcohol; in the catalyst slurry, the total mass fraction of the catalyst and the perfluorosulfonic acid ionomer is 0.1-3%.
5. The method of claim 4, wherein the catalyst comprises a carbon support and a catalytically active material, and the mass ratio of perfluorosulfonic acid ionomer to carbon support in the catalyst slurry is 0.3-1.2:1; in the catalyst, the mass percentage of active substances is 10-70%.
6. The method of claim 5, wherein the carbon support is one or more of Ketien Black, vulcan XC-72, BP 2000; the active substance is one or more of Pt, ptCo, ptIr, ptPd, ptRu, ptAu.
7. The method according to claim 4, wherein the alcohol is a volatile alcohol, the volatile alcohol is one or more of methanol, ethanol, isopropanol and n-propanol, and the mass percentage of the volatile alcohol in the mixed solvent is 10% -90%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111526640.2A CN114243054B (en) | 2021-12-13 | 2021-12-13 | Storage method of fuel cell catalyst slurry |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111526640.2A CN114243054B (en) | 2021-12-13 | 2021-12-13 | Storage method of fuel cell catalyst slurry |
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| Publication Number | Publication Date |
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| CN114243054A CN114243054A (en) | 2022-03-25 |
| CN114243054B true CN114243054B (en) | 2023-11-07 |
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Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20110110600A (en) * | 2010-04-01 | 2011-10-07 | 한국과학기술연구원 | A method of preparing a membrane-electrode assembly for a fuel cell |
| KR20110114992A (en) * | 2010-04-14 | 2011-10-20 | 한국과학기술연구원 | A catalyst slurry composition, a method for preparing a membrane-electrode assembly for fuel cell using the same and the membrane-electrode assembly for fuel cell prepared therefrom |
| CN102437343A (en) * | 2011-11-17 | 2012-05-02 | 华南理工大学 | Membrane electrode containing hydrophilic high polymer in anode catalytic layer and preparation method thereof |
| CN105051957A (en) * | 2012-08-29 | 2015-11-11 | 索尔维克雷有限责任两合公司 | Colloidal dispersions comprising precious metal particles and acidic ionomer components and methods of their manufacture and use |
| CN105390704A (en) * | 2014-09-02 | 2016-03-09 | 通用汽车环球科技运作有限责任公司 | electrode design with optimal ionomer content for polymer electrolyte membrane fuel cell |
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| CN112421085A (en) * | 2020-10-21 | 2021-02-26 | 浙江巨化技术中心有限公司 | Perfluorosulfonic acid resin proton membrane for hydrogen fuel cell and preparation method thereof |
| CN113745551A (en) * | 2021-08-13 | 2021-12-03 | 国家电投集团氢能科技发展有限公司 | Anode catalyst layer slurry and preparation method thereof |
-
2021
- 2021-12-13 CN CN202111526640.2A patent/CN114243054B/en active Active
Patent Citations (9)
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| KR20110110600A (en) * | 2010-04-01 | 2011-10-07 | 한국과학기술연구원 | A method of preparing a membrane-electrode assembly for a fuel cell |
| KR20110114992A (en) * | 2010-04-14 | 2011-10-20 | 한국과학기술연구원 | A catalyst slurry composition, a method for preparing a membrane-electrode assembly for fuel cell using the same and the membrane-electrode assembly for fuel cell prepared therefrom |
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| CN114243054A (en) | 2022-03-25 |
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