CN109962248A - A kind of preparation method of the fuel-cell catalyst with moisture-keeping functions - Google Patents
A kind of preparation method of the fuel-cell catalyst with moisture-keeping functions Download PDFInfo
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- CN109962248A CN109962248A CN201711427253.7A CN201711427253A CN109962248A CN 109962248 A CN109962248 A CN 109962248A CN 201711427253 A CN201711427253 A CN 201711427253A CN 109962248 A CN109962248 A CN 109962248A
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- added
- fuel
- transition metal
- water
- preparation
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- 239000003054 catalyst Substances 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 50
- 239000000047 product Substances 0.000 claims abstract description 35
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 23
- 238000002156 mixing Methods 0.000 claims abstract description 23
- 229910052809 inorganic oxide Inorganic materials 0.000 claims abstract description 22
- 239000002253 acid Substances 0.000 claims abstract description 20
- 229910052723 transition metal Inorganic materials 0.000 claims abstract description 20
- 229960000935 dehydrated alcohol Drugs 0.000 claims abstract description 16
- 238000006243 chemical reaction Methods 0.000 claims abstract description 14
- 239000012279 sodium borohydride Substances 0.000 claims abstract description 14
- 229910000033 sodium borohydride Inorganic materials 0.000 claims abstract description 14
- 239000007795 chemical reaction product Substances 0.000 claims abstract description 12
- 229910000510 noble metal Inorganic materials 0.000 claims abstract description 12
- 150000003624 transition metals Chemical class 0.000 claims abstract description 12
- -1 transition metal salt Chemical class 0.000 claims abstract description 10
- 150000003839 salts Chemical class 0.000 claims abstract description 9
- 239000004094 surface-active agent Substances 0.000 claims abstract description 9
- 239000000126 substance Substances 0.000 claims abstract description 7
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 4
- 235000019441 ethanol Nutrition 0.000 claims abstract description 4
- 238000010438 heat treatment Methods 0.000 claims abstract description 4
- 229960004756 ethanol Drugs 0.000 claims abstract description 3
- 238000001035 drying Methods 0.000 claims description 26
- 238000003756 stirring Methods 0.000 claims description 13
- NAQMVNRVTILPCV-UHFFFAOYSA-N hexane-1,6-diamine Chemical compound NCCCCCCN NAQMVNRVTILPCV-UHFFFAOYSA-N 0.000 claims description 10
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 claims description 9
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims description 9
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 8
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 8
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 8
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 5
- 238000004140 cleaning Methods 0.000 claims description 5
- 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 4
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims description 4
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 4
- 239000004202 carbamide Substances 0.000 claims description 4
- 239000003795 chemical substances by application Substances 0.000 claims description 4
- 239000008103 glucose Substances 0.000 claims description 4
- 229910052697 platinum Inorganic materials 0.000 claims description 4
- 229920000877 Melamine resin Polymers 0.000 claims description 3
- 235000010489 acacia gum Nutrition 0.000 claims description 3
- 239000001785 acacia senegal l. willd gum Substances 0.000 claims description 3
- QGBSISYHAICWAH-UHFFFAOYSA-N dicyandiamide Chemical compound NC(N)=NC#N QGBSISYHAICWAH-UHFFFAOYSA-N 0.000 claims description 3
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 3
- 229910052737 gold Inorganic materials 0.000 claims description 3
- 239000010931 gold Substances 0.000 claims description 3
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims description 3
- 229910052751 metal Inorganic materials 0.000 claims description 3
- 239000002184 metal Substances 0.000 claims description 3
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 claims description 3
- 229920000128 polypyrrole Polymers 0.000 claims description 3
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 claims description 3
- 239000001509 sodium citrate Substances 0.000 claims description 3
- YFSUTJLHUFNCNZ-UHFFFAOYSA-M 1,1,2,2,3,3,4,4,5,5,6,6,7,7,8,8,8-heptadecafluorooctane-1-sulfonate Chemical compound [O-]S(=O)(=O)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)F YFSUTJLHUFNCNZ-UHFFFAOYSA-M 0.000 claims description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 2
- 229910002651 NO3 Inorganic materials 0.000 claims description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 2
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 2
- 239000002280 amphoteric surfactant Substances 0.000 claims description 2
- 239000003945 anionic surfactant Substances 0.000 claims description 2
- 125000002843 carboxylic acid group Chemical group 0.000 claims description 2
- 229910017052 cobalt Inorganic materials 0.000 claims description 2
- 239000010941 cobalt Substances 0.000 claims description 2
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 2
- 229910052802 copper Inorganic materials 0.000 claims description 2
- 239000010949 copper Substances 0.000 claims description 2
- 238000001914 filtration Methods 0.000 claims description 2
- 125000002791 glucosyl group Chemical group C1([C@H](O)[C@@H](O)[C@H](O)[C@H](O1)CO)* 0.000 claims description 2
- 229910052742 iron Inorganic materials 0.000 claims description 2
- 229920002521 macromolecule Polymers 0.000 claims description 2
- 229910052759 nickel Inorganic materials 0.000 claims description 2
- NHNBFGGVMKEFGY-UHFFFAOYSA-N nitrate group Chemical group [N+](=O)([O-])[O-] NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 2
- 229910052763 palladium Inorganic materials 0.000 claims description 2
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 2
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 2
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 2
- 239000010970 precious metal Chemical class 0.000 claims description 2
- 230000009467 reduction Effects 0.000 claims description 2
- 229910052709 silver Inorganic materials 0.000 claims description 2
- 239000004332 silver Substances 0.000 claims description 2
- BWYYYTVSBPRQCN-UHFFFAOYSA-M sodium;ethenesulfonate Chemical compound [Na+].[O-]S(=O)(=O)C=C BWYYYTVSBPRQCN-UHFFFAOYSA-M 0.000 claims description 2
- 125000000542 sulfonic acid group Chemical group 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 claims 2
- 229920006316 polyvinylpyrrolidine Polymers 0.000 claims 1
- 229910000314 transition metal oxide Inorganic materials 0.000 claims 1
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 abstract description 4
- 238000001816 cooling Methods 0.000 abstract 1
- 230000036571 hydration Effects 0.000 abstract 1
- 238000006703 hydration reaction Methods 0.000 abstract 1
- 239000000446 fuel Substances 0.000 description 21
- 206010013786 Dry skin Diseases 0.000 description 15
- 239000012528 membrane Substances 0.000 description 14
- 210000004027 cell Anatomy 0.000 description 13
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 10
- 239000013049 sediment Substances 0.000 description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 6
- 230000003197 catalytic effect Effects 0.000 description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 5
- 229910052681 coesite Inorganic materials 0.000 description 5
- 230000003750 conditioning effect Effects 0.000 description 5
- 229910052906 cristobalite Inorganic materials 0.000 description 5
- 239000000377 silicon dioxide Substances 0.000 description 5
- 229910052682 stishovite Inorganic materials 0.000 description 5
- 229910052905 tridymite Inorganic materials 0.000 description 5
- 238000006555 catalytic reaction Methods 0.000 description 4
- 230000001376 precipitating effect Effects 0.000 description 4
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 3
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 239000002131 composite material Substances 0.000 description 3
- 230000005611 electricity Effects 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- QGLKJKCYBOYXKC-UHFFFAOYSA-N nonaoxidotritungsten Chemical compound O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 QGLKJKCYBOYXKC-UHFFFAOYSA-N 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- 239000011734 sodium Substances 0.000 description 3
- 229910052708 sodium Inorganic materials 0.000 description 3
- 229910001930 tungsten oxide Inorganic materials 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 229910021580 Cobalt(II) chloride Inorganic materials 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 229920000557 Nafion® Polymers 0.000 description 2
- KAESVJOAVNADME-UHFFFAOYSA-N Pyrrole Chemical compound C=1C=CNC=1 KAESVJOAVNADME-UHFFFAOYSA-N 0.000 description 2
- 229920002472 Starch Polymers 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 210000000170 cell membrane Anatomy 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 229910021389 graphene Inorganic materials 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 2
- 239000002048 multi walled nanotube Substances 0.000 description 2
- 239000002105 nanoparticle 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
- 238000000926 separation method Methods 0.000 description 2
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 2
- 239000008107 starch Substances 0.000 description 2
- 235000019698 starch Nutrition 0.000 description 2
- 230000007704 transition Effects 0.000 description 2
- WBIQQQGBSDOWNP-UHFFFAOYSA-N 2-dodecylbenzenesulfonic acid Chemical compound CCCCCCCCCCCCC1=CC=CC=C1S(O)(=O)=O WBIQQQGBSDOWNP-UHFFFAOYSA-N 0.000 description 1
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 1
- 229910021591 Copper(I) chloride Inorganic materials 0.000 description 1
- 206010011224 Cough Diseases 0.000 description 1
- SNRUBQQJIBEYMU-UHFFFAOYSA-N Dodecane Natural products CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 description 1
- 239000004909 Moisturizer Substances 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- 229910021536 Zeolite Inorganic materials 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 235000008429 bread Nutrition 0.000 description 1
- 235000013339 cereals Nutrition 0.000 description 1
- 238000005253 cladding Methods 0.000 description 1
- OXBLHERUFWYNTN-UHFFFAOYSA-M copper(I) chloride Chemical compound [Cu]Cl OXBLHERUFWYNTN-UHFFFAOYSA-M 0.000 description 1
- 239000011258 core-shell material Substances 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
- 125000003438 dodecyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 229940060296 dodecylbenzenesulfonic acid Drugs 0.000 description 1
- 230000009881 electrostatic interaction Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000007717 exclusion Effects 0.000 description 1
- 235000019253 formic acid Nutrition 0.000 description 1
- 238000007306 functionalization reaction Methods 0.000 description 1
- 239000011964 heteropoly acid Substances 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 239000002923 metal particle Substances 0.000 description 1
- 230000001333 moisturizer Effects 0.000 description 1
- 239000011943 nanocatalyst Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- PIBWKRNGBLPSSY-UHFFFAOYSA-L palladium(II) chloride Chemical compound Cl[Pd]Cl PIBWKRNGBLPSSY-UHFFFAOYSA-L 0.000 description 1
- 229920000767 polyaniline Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000036647 reaction Effects 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 229910001961 silver nitrate Inorganic materials 0.000 description 1
- DAJSVUQLFFJUSX-UHFFFAOYSA-M sodium;dodecane-1-sulfonate Chemical compound [Na+].CCCCCCCCCCCCS([O-])(=O)=O DAJSVUQLFFJUSX-UHFFFAOYSA-M 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 1
- 229910001428 transition metal ion Inorganic materials 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
- 239000010457 zeolite Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/88—Processes of manufacture
- H01M4/8825—Methods for deposition of the catalytic active composition
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/90—Selection of catalytic material
- H01M4/9041—Metals or alloys
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/90—Selection of catalytic material
- H01M4/92—Metals of platinum group
- H01M4/925—Metals of platinum group supported on carriers, e.g. powder carriers
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Nanotechnology (AREA)
- Manufacturing & Machinery (AREA)
- Physics & Mathematics (AREA)
- Composite Materials (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Crystallography & Structural Chemistry (AREA)
- Catalysts (AREA)
Abstract
The invention discloses a kind of preparation methods of fuel-cell catalyst with moisture-keeping functions, include the following steps: that nano inorganic oxide is dispersed in water by (1), surfactant is added, adjusting solution ph is 1-6, after mixing evenly, transition metal salt is added, after mixing evenly, reducing agent sodium borohydride is added or hydration hydrazine reaction obtains the inorganic oxide of carrying transition metal；(2) disperse the inorganic oxide of carrying transition metal in water or ethyl alcohol, be added itrogenous organic substance, after being uniformly mixed, be transferred in autoclave, in 100-200 DEG C heating 1-72 hours；Take out it is dry after, under an inert atmosphere, after being heated to 500-1100 DEG C, heating 0.5-3 hours, cooling product；(3) it disperses the product of step (2) in water or dehydrated alcohol, noble metal acid or salt is added, after being stirred to react 0.5-5 hours, product is cleaned, dry end product.
Description
Technical field
The present invention relates to a kind of preparation methods of fuel-cell catalyst with moisture-keeping functions, belong to catalyst preparation skill
Art field.
Background technique
Fuel cell is a kind of device that chemical energy is converted directly into electric energy, and core is to use catalyst oxygen also
Former and hydroxide or alcohol oxidation, Oxidation of Formic Acid etc..
Fuel cell is faced with the commercialized starting stage, and a major issue for influencing commercializing fuel cells is fuel
The cost of battery, the cost of Fuel Cell Control System and the cost of fuel cell pack are suitable, any to can simplify fuel cell
The behave of system can reduce the cost of fuel cell system.The stable operation of fuel cell and quick response and fuel electricity
Quick Heat And Water Balance in pond is related, and fuel cell membrane electrode is under the environment of water logging or drying, is all difficult to play fuel
The high-performance benefits of battery.For this purpose, improving the moisture-retaining capacity of membrane electrode itself, dependence of the fuel cell to water is reduced, on the one hand
Running stability of fuel battery can be improved, on the other hand can greatly simplify the control system of fuel cell, be fuel electricity
The important directions of pond development.
Increase by one layer of hydrophilic carbon microporous layers between the Catalytic Layer and carbon microporous layers of fuel cell membrane electrode
(S.Hirakata et al., Electrochimica Acta 120,240-247,2014), since its pore size is smaller,
It is more conducive to the exclusion of water, simultaneously because the water-wet behavior of itself, under conditions of humidity is low, and can hold water within film
It is a kind of method for obtaining self-humidifying membrane electrode in electrode.
SiO2、TiO2、ZnO、ZrO2、WO3、ZrO2-SiO2(Zr/Si=0.5) etc. important inorganic oxide, have and lead matter
Nano compound α-ZrP, the Cs of subfunction2.5H0.5PWO40, heteropoly acid and functionalization multi-walled carbon nanotube (MWCNT), cover
De- stone (MMT), zeolite, SiO2Etc. be often used as moisturizer be added into proton exchange membrane Catalytic Layer (R.Zeng et al.,
Electrochimica Acta, 52,3895-3900,2007；L.Y.Hong et al., Electrochimica Acta, 56,
3108-3114,2011；J.Zeng et al., J.Membr.Sci., 397-398,92-101,2012；C.Bai et al.,
J.Power Sources, 184,197-203,2008；I.Choi et al., Applied Catalysis B:
Environmental, 168-169,220-227,2015), to improve the performance of keeping humidity of the membrane electrode of preparation.Tang Haolin et al.
(L.Chen et al., Int.J.Hydrogen Energy, 37,4694-4698,2012；J.R.Li et al.,
Chem.Commun., 49,6537-6539,2013) pass through SiO2Interaction between Nafion solution forms ordering
SiO2With Nafion composite membrane, the proton conductivity of composite membrane is improved, especially under low humidity conditions, composite membrane still shows
Good proton conductivity out, improves the moisture retention of proton exchange membrane, and improves the proton electricity of its high temperature (being higher than 100 DEG C)
Conductance.
Lv Weizhong (the battery such as Lv Weizhong, 40 (3), 127-130,2010), Hagihara (H.Hagihara et al.,
Electrochimica Acta 51,3979-3985,2006) et al., a small amount of Platinum Nanoparticles are added in proton exchange membrane
Grain generates water using platinum catalysis hydrogen through the membrane and oxygen reaction, to keep proton exchange membrane in dry environments in film
Water content and Proton conducting guarantee the stable operation of fuel cell.
And the prior art use inorganic oxide and other Nano compounds poorly conductive, if be used in Catalytic Layer or
In carbon microporous layers, increase is prepared to the resistance of membrane electrode, reduces the performance of fuel cell.
Summary of the invention
Aiming at the problems existing in the prior art, the purpose of the present invention is to provide a kind of, and the fuel with moisture-keeping functions is electric
The preparation method of pond catalyst.
To achieve the above object, the invention adopts the following technical scheme:
A kind of preparation method of the fuel-cell catalyst with moisture-keeping functions, includes the following steps:
(1) nano inorganic oxide is dispersed in water, surfactant is added, adjusting solution ph is 1-6, and stirring is equal
After even, one or more transition metal salts are added, after mixing evenly, reducing agent sodium borohydride or hydrazine hydrate are added, also by metal
Original is deposited on inorganic oxide surface；After product dehydrated alcohol or water clean for several times, drying obtains the nothing of carrying transition metal
Machine oxide；
(2) it disperses the inorganic oxide of carrying transition metal in water or ethyl alcohol, itrogenous organic substance is added, is stirred
Uniformly after, be transferred in autoclave, in 100-200 DEG C heating 1-72 hours；After taking out drying, under an inert atmosphere, it is heated to
It 500-1100 DEG C, heats 0.5-3 hours；Later, 50 DEG C are down to hereinafter, taking out product；
(3) step (2) product is taken, is scattered in water or dehydrated alcohol, after mixing evenly, noble metal acid or salt is added, stirs
After mixing reaction 0.5-5 hours, product filtering washing, with diluted acid in cleaning 0.5-2 hours of -100 DEG C of room temperature；After being washed with water, do
It is dry to obtain end product.
Preferably, after noble metal acid or salt are added in the step (3), sodium borohydride or hydrazine hydrate reduction are added
Agent is stirred to react 0.5-2 hours.
In the present invention, the transition metal salt is nitrate, chloride or the sulfate of transition metal；The transition gold
Belonging to is iron, cobalt, nickel or copper, and the noble metal is platinum, gold, silver or palladium.
In the present invention, the surfactant is the anionic surfactant containing sulfonic acid group or carboxylic acid group, or
Person is amphoteric surfactant, including neopelex, dodecyl sodium sulfate, perfluorooctane sulfonate, vinyl sulfonic acid
Sodium, sodium citrate or Arabic gum.
The itrogenous organic substance is glucose, urea, melamine, dicyandiamide, hexamethylene diamine, polyvinyl pyrrole
It coughs up, nitrogenous small organic molecule or the macromolecule such as polyvinylpyrrolidone, polyaniline or polypyrrole.
Preferably, in step (1), the concentration of transition metal salt is 0.001~1.0mol/L, and surfactant is in solution
In mass fraction be 0.001%~5%.
Preferably, in the step (1) or step (3), the amount and transition of sodium borohydride or hydrazine hydrate be added are reacted
The molar ratio of metal salt or precious metal salt is (1~10): 1.
Preferably, in the step (2), the inorganic oxide of carrying transition metal and the mass ratio of itrogenous organic substance are
(50~0.001): 1.
In the present invention, the quality of noble metal is the 0~70% of catalyst quality in gained catalyst.
The invention has the benefit that
The present invention adjusts the Zeta of inorganic oxide surface by adjusting solution ph and kinds of surfactants and concentration
Current potential improves the dispersibility of inorganic oxide nanoparticles, simultaneously as electrostatic interaction, in nano inorganic oxide table
Richness product inorganic transition metal ion in face makes transition metal be deposited on nano inorganic oxide surface, shape under the action of reducing agent
At shell.On this basis, by hydro-thermal reaction and high-temperature process, nitrogen is coated on nano inorganic oxide transition metal shell
Class graphene layer is adulterated, as carrier, the nanocatalyst or cladding noble metal shell for preparing carried noble metal form multilayer
The catalyst of core-shell structure.
The present invention using nano inorganic oxide as catalyst carrier so that the water energy that generates of fuel cell reaction it is enough quickly from
The surface of catalyst is opened, and is stored in water in Catalytic Layer in nano inorganic oxide moisture lock, improves low-moisture conditions
The ionic conductivity of lower Catalytic Layer and proton exchange membrane, to improve the performance of membrane electrode.Meanwhile in nano inorganic oxide table
Bread covers N doping class graphene, and the nano-noble metal particle or shell of the electric conductivity and load that improve nano inorganic oxide exist
Stability under electrochemical environment improves the catalytic activity of catalyst.
Detailed description of the invention
Fig. 1 is the variation diagram of catalyst structure in preparation process of the invention.
Specific embodiment
The present invention will be further described with reference to the accompanying drawings and examples.It is emphasized that following embodiment is only
It is exemplary, the range and its application being not intended to be limiting of the invention.
Embodiment 1
The silicon dioxde solution 200mL of 0.025mol/L is configured, the dodecyl that mass fraction is 0.05% is then added
Sodium sulfonate, it is 3 that hydrochloric acid conditioning solution pH value, which is added, after mixing evenly, 0.025mol/L CoCl is added2Solution 200mL, stirring
After uniformly, sodium borohydride 0.05mol/L is added, stirs lower reaction 2 hours, solution colour blackening, reaction product is black precipitate
Object filters or is centrifugated out sediment, and reaction product, 50 DEG C of dryings are cleaned multiple times with water.
Above-mentioned product 1g, melamine 1g is taken to be scattered in dehydrated alcohol, 200 DEG C of autoclave are reacted 72 hours, are taken out dry
After dry, under an inert atmosphere, 900 DEG C be heated to, constant temperature 2 hours, later, is down to 50 DEG C hereinafter, taking out product.
Above-mentioned product 0.5g is taken, is scattered in 200mL dehydrated alcohol, chloroplatinic acid 1.25g is added, sodium borohydride is added
0.386g is stirred to react 1 hour, after reaction product is cleaned multiple times with water, is cleaned with 80 DEG C of diluted acid, is then washed with water repeatedly,
50 DEG C of dryings.Obtain structure in Fig. 1 " 2 " catalyst.
Embodiment 2
0.05mol/L silicon dioxde solution 200mL is configured, the dodecyl sodium sulfate of mass fraction 0.1% is then added,
It is 3 that hydrochloric acid conditioning solution pH value, which is added, after mixing evenly, 0.025mol/L FeCl is added3And NiCl2Solution 100mL, wherein Fe
: Ni=1: 1, after mixing evenly, sodium borohydride 0.05mol/L is added, stirs lower reaction 2 hours, solution colour blackening, separation is heavy
Sediment, 50 DEG C of dryings are cleaned multiple times with water in starch.
Above-mentioned product 1g, dicyandiamide 1g is taken to be scattered in dehydrated alcohol, 200 DEG C of autoclave are reacted 48 hours, and drying is taken out
Afterwards, under an inert atmosphere, 1000 DEG C are heated to, constant temperature 2 hours, later, is down to 50 DEG C hereinafter, taking out product.With 80 DEG C of diluted acid
Then cleaning washes with water repeatedly 50 DEG C of dryings.Obtain structure in Fig. 1 " 1 " catalyst.
Embodiment 3
0.025mol/L silicon dioxde solution 200mL is configured, the dodecyl sodium sulfonate of mass fraction 0.05% is then added
Sodium, it is 3 that hydrochloric acid conditioning solution pH value, which is added, after mixing evenly, 0.025mol/L FeCl is added3And CoCl2Solution 100mL,
Middle Fe: Co=1: 1, after mixing evenly, sodium borohydride 0.05mol/L is added, stirs lower reaction 2 hours, solution colour blackening, point
From sediment, sediment, 50 DEG C of dryings are cleaned multiple times with water.
Above-mentioned product 1g, hexamethylene diamine 1g is taken to be dispersed in water, 200 DEG C of autoclave are reacted 72 hours, and drying is taken out
Afterwards, under an inert atmosphere, 900 DEG C are heated to, constant temperature 2 hours, later, is down to 50 DEG C hereinafter, taking out product.
Above-mentioned product 0.5g is taken, is scattered in 200mL dehydrated alcohol, chloroplatinic acid 1.25g is added, hydrazine hydrate 5mL is added, stirs
Reaction 1 hour is mixed, after reaction product is cleaned multiple times with water, is cleaned with 80 DEG C of diluted acid, repeatedly 50 DEG C of dryings are then washed with water.
Obtain structure in Fig. 1 " 2 " catalyst.
Embodiment 4
0.025mol/L burnett's solution 200mL is configured, the dodecyl sodium sulfate of mass fraction 0.01% is then added,
It is 3 that hydrochloric acid conditioning solution pH value, which is added, after mixing evenly, 0.025mol/L NiCl is added2And CoCl2Solution 100mL, wherein Ni
: Co=1: 1, after mixing evenly, sodium borohydride 0.05mol/L is added, stirs lower reaction 2 hours, solution colour blackening, separation is heavy
Precipitating, 50 DEG C of dryings are cleaned multiple times with water in starch.
Above-mentioned product 1g, urea 1g is taken to be scattered in dehydrated alcohol, 200 DEG C of autoclave are reacted 72 hours, and drying is taken out
Afterwards, under an inert atmosphere, 900 DEG C are heated to, constant temperature 2 hours, later, is down to 50 DEG C hereinafter, taking out product.
Above-mentioned product 0.5g is taken, is scattered in 200mL dehydrated alcohol, chloroplatinic acid 1.25g is added, hydrazine hydrate 5mL is added, stirs
Reaction 1 hour is mixed, after reaction product is cleaned multiple times with water, is cleaned with 50 DEG C of diluted acid, repeatedly 50 DEG C of dryings are then washed with water.
Obtain structure in Fig. 1 " 2 " catalyst.
Embodiment 5
0.025mol/L burnett's solution 200mL is configured, the dodecyl benzene sulfonic acid of mass fraction 0.05% is then added
Sodium, it is 3 that hydrochloric acid conditioning solution pH value, which is added, after mixing evenly, 0.025mol/L FeCl is added3And NiCl2Solution 100mL,
Middle Fe: Ni=1: 1, after mixing evenly, sodium borohydride 0.05mol/L is added, stirs lower reaction 2 hours, solution colour blackening, point
From sediment, sediment, 50 DEG C of dryings are cleaned multiple times with water.
Above-mentioned product 1g, urea 1g is taken to be scattered in dehydrated alcohol, 200 DEG C of autoclave are reacted 72 hours, and drying is taken out
Afterwards, under an inert atmosphere, 900 DEG C are heated to, constant temperature 2 hours, later, is down to 50 DEG C hereinafter, taking out product.
Above-mentioned product 0.5g is taken, is scattered in 200mL dehydrated alcohol, chloroplatinic acid 1.25g is added, is stirred to react 1 hour, is used
It after reaction product is cleaned multiple times in water, is cleaned with 80 DEG C of diluted acid, then washes with water repeatedly 50 DEG C of dryings.Obtain structure in Fig. 1
" 3 " catalyst.
Embodiment 6
0.025mol/L tungsten oxide solution 200mL is configured, the sodium citrate of mass fraction 0.05% is then added, salt is added
Acid-conditioning solution pH value is 3, after mixing evenly, 0.025mol/L FeCl is added3Water is added after mixing evenly in solution 100mL
Hydrazine 0.5mol/L is closed, 80 DEG C of stirrings lower reaction 2 hours, precipitating was cleaned multiple times with water in solution colour blackening, sediment separate out, and 50
DEG C drying.
Above-mentioned product 1g, polypyrrole 1g is taken to be scattered in dehydrated alcohol, 200 DEG C of autoclave are reacted 72 hours, and drying is taken out
Afterwards, under an inert atmosphere, 1100 DEG C are heated to, constant temperature 2 hours, later, is down to 50 DEG C hereinafter, taking out product.
Above-mentioned product 0.5g is taken, is scattered in 200mL deionized water, silver nitrate 0.8g is added, is stirred to react 1 hour, is used
It after reaction product is cleaned multiple times in water, is cleaned with 80 DEG C of diluted acid, then washes with water repeatedly 50 DEG C of dryings.Obtain structure in Fig. 1
" 3 " catalyst.
Embodiment 7
0.025mol/L tungsten oxide solution 200mL is configured, the Arabic gum of mass fraction 0.05% is then added, sulphur is added
Acid-conditioning solution pH value is 5, after mixing evenly, 0.025mol/L FeCl is added3And NiCl2Solution 100mL, Fe: Ni=1: 1,
After mixing evenly, hydrazine hydrate 0.5mol/L is added, 80 DEG C of stirrings lower reaction 2 hours, solution colour blackening, sediment separate out was used
Precipitating, 50 DEG C of dryings are cleaned multiple times in water.
Above-mentioned product 1g, glucose 1g, hexamethylene diamine 0.5g is taken to be scattered in dehydrated alcohol, 200 DEG C of autoclave anti-
Answer 72 hours, take out it is dry after, under an inert atmosphere, be heated to 800 DEG C, constant temperature 2 hours, then be heated up to 1000 DEG C, constant temperature 1 was small
When, later, 50 DEG C are down to hereinafter, taking out product.
Above-mentioned product 0.5g is taken, is scattered in 200mL water, chloroplatinic acid 1.25g is added, is stirred to react 1 hour, it is multiple with water
It after cleaning reaction product, is cleaned with 80 DEG C of diluted acid, then washes with water repeatedly 50 DEG C of dryings.Obtain structure in Fig. 1 " 3 " catalysis
Agent.
Embodiment 8
0.025mol/L tungsten oxide solution 200mL is configured, the dodecyl sodium sulfate of mass fraction 0.05% is then added,
It is 5 that sulfuric acid regulation solution pH value, which is added, after mixing evenly, 0.025mol/L CuCl is added2Solution 100mL, after mixing evenly,
Sodium borohydride 0.5mol/L is added, is stirred to react 2 hours, solution colour blackening, sediment separate out, precipitating is cleaned multiple times with water,
50 DEG C of dryings.
Above-mentioned product 1g, glucose 1g, hexamethylene diamine 0.5g is taken to be scattered in dehydrated alcohol, 200 DEG C of autoclave anti-
Answer 72 hours, take out it is dry after, under an inert atmosphere, be heated to 800 DEG C, constant temperature 2 hours, then be heated up to 1000 DEG C, constant temperature 1 was small
When, later, 50 DEG C are down to hereinafter, taking out product.
Above-mentioned product 0.5g is taken, is scattered in 200mL water, palladium chloride 0.5g is added, is stirred to react 1 hour, it is multiple with water
It after cleaning reaction product, is cleaned with diluted acid room temperature, then washes with water repeatedly 50 DEG C of dryings.Obtain structure in Fig. 1 " 3 " catalysis
Agent.
Claims (10)
1. a kind of preparation method of the fuel-cell catalyst with moisture-keeping functions, which comprises the steps of:
(1) nano inorganic oxide is dispersed in water, surfactant is added, adjusting solution ph is 1-6, is stirred evenly
Afterwards, one or more transition metal salts are added, after mixing evenly, reducing agent sodium borohydride or hydrazine hydrate is added, metal is restored
It is deposited on inorganic oxide surface；After product dehydrated alcohol or water clean for several times, drying obtains the inorganic of carrying transition metal
Oxide；
(2) it disperses the inorganic oxide of carrying transition metal in water or ethyl alcohol, itrogenous organic substance is added, is uniformly mixed
Afterwards, be transferred in autoclave, in 100-200 DEG C heating 1-72 hours；After taking out drying, under an inert atmosphere, it is heated to 500-
It 1100 DEG C, heats 0.5-3 hours；It is down to 50 DEG C later hereinafter, taking out product；
(3) step (2) products therefrom is taken, is scattered in water or dehydrated alcohol, after mixing evenly, noble metal acid or salt is added, stirs
After mixing reaction 0.5-5 hours, product filtering washing, with diluted acid in cleaning 0.5-2 hours of -100 DEG C of room temperature；After being washed with water, do
It is dry to obtain end product.
2. the preparation method of fuel-cell catalyst according to claim 1, which is characterized in that in the step (3)
After noble metal acid or salt is added, sodium borohydride or hydrazine hydrate reduction agent are added, is stirred to react 0.5-2 hours.
3. the preparation method of fuel-cell catalyst according to claim 1 or 2, which is characterized in that the transition metal
Salt is nitrate, chloride or the sulfate of transition metal；The transition metal is iron, cobalt, nickel or copper, and the noble metal is
Platinum, gold, silver or palladium.
4. the preparation method of fuel-cell catalyst according to claim 1 or 2, which is characterized in that the surface-active
Agent is anionic surfactant or amphoteric surfactant containing sulfonic acid group or carboxylic acid group.
5. the preparation method of fuel-cell catalyst according to claim 4, which is characterized in that the surfactant is
Neopelex, dodecyl sodium sulfate, perfluorooctane sulfonate, sodium vinyl sulfonate, sodium citrate or Arabic gum.
6. the preparation method of fuel-cell catalyst according to claim 1 or 2, which is characterized in that described nitrogenous organic
Object is glucose, urea, melamine, dicyandiamide, hexamethylene diamine, polyvinylpyrrolidine, polyvinylpyrrolidone, gathers
The nitrogenous small organic molecule or macromolecule of aniline or polypyrrole.
7. the preparation method of fuel-cell catalyst according to claim 1 or 2, which is characterized in that in the step (1)
In, the concentration of transition metal salt is 0.001~1.0mol/L, the mass fraction of surfactant in the solution is 0.001%~
5%.
8. the preparation method of fuel-cell catalyst according to claim 1 or 2, which is characterized in that in the step (1)
Or in step (3), reacts the amount of sodium borohydride or hydrazine hydrate be added and the molar ratio of transition metal salt or precious metal salt is (1
~10): 1.
9. the preparation method of fuel-cell catalyst according to claim 1 or 2, which is characterized in that in the step (2)
In, the inorganic oxide of carrying transition metal and the mass ratio of itrogenous organic substance are (50~0.001): 1.
10. the preparation method of fuel-cell catalyst according to claim 1 or 2, which is characterized in that in gained catalyst
The quality of noble metal is the 0~70% of catalyst quality.
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| US20030224926A1 (en) * | 2002-04-30 | 2003-12-04 | Wei Xing | Method of preparing nano-level platinum/carbon electrocatalyst for cathode of fuel cell |
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| CN106654307A (en) * | 2017-01-10 | 2017-05-10 | 大连理工大学 | Preparation method and application of noble metal@graphite layer core-shell structured electro-catalyst |
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| US20030224926A1 (en) * | 2002-04-30 | 2003-12-04 | Wei Xing | Method of preparing nano-level platinum/carbon electrocatalyst for cathode of fuel cell |
| CN103721705A (en) * | 2014-01-14 | 2014-04-16 | 武汉理工大学 | Porous TiO2 fiber loaded noble metal formaldehyde room-temperature oxidation catalyst and preparation method thereof |
| CN105810956A (en) * | 2014-12-31 | 2016-07-27 | 北京有色金属研究总院 | Method for preparing doped graphene or graphene-like compound |
| CN105845952A (en) * | 2016-04-11 | 2016-08-10 | 上海电力学院 | Preparation method for positive electrode catalyst of fuel cell |
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