CN112473691A - Preparation method of low-platinum hollow polyhedral nano-structured catalyst - Google Patents
Preparation method of low-platinum hollow polyhedral nano-structured catalyst Download PDFInfo
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- CN112473691A CN112473691A CN202011367566.XA CN202011367566A CN112473691A CN 112473691 A CN112473691 A CN 112473691A CN 202011367566 A CN202011367566 A CN 202011367566A CN 112473691 A CN112473691 A CN 112473691A
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- Prior art keywords
- platinum
- catalyst
- low
- polyhedral
- hollow polyhedral
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- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Substances [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 title claims abstract description 96
- 239000003054 catalyst Substances 0.000 title claims abstract description 75
- 229910052697 platinum Inorganic materials 0.000 title claims abstract description 51
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 30
- 238000000034 method Methods 0.000 claims abstract description 24
- 238000006243 chemical reaction Methods 0.000 claims abstract description 19
- 239000002243 precursor Substances 0.000 claims abstract description 14
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000001301 oxygen Substances 0.000 claims abstract description 12
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 11
- 230000003197 catalytic effect Effects 0.000 claims abstract description 9
- 239000002082 metal nanoparticle Substances 0.000 claims abstract description 8
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 7
- 239000002904 solvent Substances 0.000 claims description 16
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 12
- 239000011261 inert gas Substances 0.000 claims description 10
- 229910052751 metal Inorganic materials 0.000 claims description 9
- 239000002184 metal Substances 0.000 claims description 9
- 238000006722 reduction reaction Methods 0.000 claims description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- 239000004094 surface-active agent Substances 0.000 claims description 8
- 150000001298 alcohols Chemical class 0.000 claims description 6
- 229910052786 argon Inorganic materials 0.000 claims description 6
- 239000003638 chemical reducing agent Substances 0.000 claims description 6
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 6
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 6
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical group O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 4
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 4
- GVPFVAHMJGGAJG-UHFFFAOYSA-L cobalt dichloride Chemical compound [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 0.000 claims description 4
- DDXLVDQZPFLQMZ-UHFFFAOYSA-M dodecyl(trimethyl)azanium;chloride Chemical compound [Cl-].CCCCCCCCCCCC[N+](C)(C)C DDXLVDQZPFLQMZ-UHFFFAOYSA-M 0.000 claims description 4
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 claims description 4
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- 150000003839 salts Chemical class 0.000 claims description 4
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 3
- 239000012279 sodium borohydride Substances 0.000 claims description 3
- 229910000033 sodium borohydride Inorganic materials 0.000 claims description 3
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims description 2
- QGLWBTPVKHMVHM-KTKRTIGZSA-N (z)-octadec-9-en-1-amine Chemical compound CCCCCCCC\C=C/CCCCCCCCN QGLWBTPVKHMVHM-KTKRTIGZSA-N 0.000 claims description 2
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims description 2
- CDVAIHNNWWJFJW-UHFFFAOYSA-N 3,5-diethoxycarbonyl-1,4-dihydrocollidine Chemical compound CCOC(=O)C1=C(C)NC(C)=C(C(=O)OCC)C1C CDVAIHNNWWJFJW-UHFFFAOYSA-N 0.000 claims description 2
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims description 2
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Natural products OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 2
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 2
- 239000005642 Oleic acid Substances 0.000 claims description 2
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims description 2
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 2
- 238000010521 absorption reaction Methods 0.000 claims description 2
- MQRWBMAEBQOWAF-UHFFFAOYSA-N acetic acid;nickel Chemical compound [Ni].CC(O)=O.CC(O)=O MQRWBMAEBQOWAF-UHFFFAOYSA-N 0.000 claims description 2
- 239000011668 ascorbic acid Substances 0.000 claims description 2
- 229960005070 ascorbic acid Drugs 0.000 claims description 2
- 235000010323 ascorbic acid Nutrition 0.000 claims description 2
- 239000012298 atmosphere Substances 0.000 claims description 2
- 238000005119 centrifugation Methods 0.000 claims description 2
- 229940011182 cobalt acetate Drugs 0.000 claims description 2
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 claims description 2
- 229910001981 cobalt nitrate Inorganic materials 0.000 claims description 2
- QAHREYKOYSIQPH-UHFFFAOYSA-L cobalt(II) acetate Chemical compound [Co+2].CC([O-])=O.CC([O-])=O QAHREYKOYSIQPH-UHFFFAOYSA-L 0.000 claims description 2
- FJDJVBXSSLDNJB-LNTINUHCSA-N cobalt;(z)-4-hydroxypent-3-en-2-one Chemical compound [Co].C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O FJDJVBXSSLDNJB-LNTINUHCSA-N 0.000 claims description 2
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 claims description 2
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 claims description 2
- ZKXWKVVCCTZOLD-UHFFFAOYSA-N copper;4-hydroxypent-3-en-2-one Chemical compound [Cu].CC(O)=CC(C)=O.CC(O)=CC(C)=O ZKXWKVVCCTZOLD-UHFFFAOYSA-N 0.000 claims description 2
- 150000004985 diamines Chemical class 0.000 claims description 2
- 150000002148 esters Chemical class 0.000 claims description 2
- PVFSDGKDKFSOTB-UHFFFAOYSA-K iron(3+);triacetate Chemical compound [Fe+3].CC([O-])=O.CC([O-])=O.CC([O-])=O PVFSDGKDKFSOTB-UHFFFAOYSA-K 0.000 claims description 2
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims description 2
- 150000002576 ketones Chemical class 0.000 claims description 2
- TYQCGQRIZGCHNB-JLAZNSOCSA-N l-ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(O)=C(O)C1=O TYQCGQRIZGCHNB-JLAZNSOCSA-N 0.000 claims description 2
- 229940078494 nickel acetate Drugs 0.000 claims description 2
- BMGNSKKZFQMGDH-FDGPNNRMSA-L nickel(2+);(z)-4-oxopent-2-en-2-olate Chemical compound [Ni+2].C\C([O-])=C\C(C)=O.C\C([O-])=C\C(C)=O BMGNSKKZFQMGDH-FDGPNNRMSA-L 0.000 claims description 2
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 claims description 2
- CCCMONHAUSKTEQ-UHFFFAOYSA-N octadecene Natural products CCCCCCCCCCCCCCCCC=C CCCMONHAUSKTEQ-UHFFFAOYSA-N 0.000 claims description 2
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims description 2
- PIBWKRNGBLPSSY-UHFFFAOYSA-L palladium(II) chloride Chemical compound Cl[Pd]Cl PIBWKRNGBLPSSY-UHFFFAOYSA-L 0.000 claims description 2
- YJVFFLUZDVXJQI-UHFFFAOYSA-L palladium(ii) acetate Chemical compound [Pd+2].CC([O-])=O.CC([O-])=O YJVFFLUZDVXJQI-UHFFFAOYSA-L 0.000 claims description 2
- JKDRQYIYVJVOPF-FDGPNNRMSA-L palladium(ii) acetylacetonate Chemical compound [Pd+2].C\C([O-])=C\C(C)=O.C\C([O-])=C\C(C)=O JKDRQYIYVJVOPF-FDGPNNRMSA-L 0.000 claims description 2
- GPNDARIEYHPYAY-UHFFFAOYSA-N palladium(ii) nitrate Chemical compound [Pd+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O GPNDARIEYHPYAY-UHFFFAOYSA-N 0.000 claims description 2
- MBUJACWWYFPMDK-UHFFFAOYSA-N pentane-2,4-dione;platinum Chemical compound [Pt].CC(=O)CC(C)=O MBUJACWWYFPMDK-UHFFFAOYSA-N 0.000 claims description 2
- 229910052700 potassium Inorganic materials 0.000 claims description 2
- 239000011591 potassium Substances 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 239000001509 sodium citrate Substances 0.000 claims description 2
- 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 2
- 230000009467 reduction Effects 0.000 abstract description 8
- 239000002086 nanomaterial Substances 0.000 abstract description 7
- 230000003647 oxidation Effects 0.000 abstract description 6
- 230000008569 process Effects 0.000 abstract description 4
- 238000009776 industrial production Methods 0.000 abstract description 2
- 239000010411 electrocatalyst Substances 0.000 abstract 1
- 230000001737 promoting effect Effects 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 21
- 239000000463 material Substances 0.000 description 20
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 12
- 239000000446 fuel Substances 0.000 description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 7
- 229910002837 PtCo Inorganic materials 0.000 description 7
- 230000000694 effects Effects 0.000 description 7
- 239000002105 nanoparticle Substances 0.000 description 7
- 229910000510 noble metal Inorganic materials 0.000 description 7
- 229910052763 palladium Inorganic materials 0.000 description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- 238000011161 development Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 230000007613 environmental effect Effects 0.000 description 4
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- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 239000011258 core-shell material Substances 0.000 description 3
- 239000003517 fume Substances 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000012512 characterization method Methods 0.000 description 2
- 125000004122 cyclic group Chemical group 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000011031 large-scale manufacturing process Methods 0.000 description 2
- 239000002091 nanocage Substances 0.000 description 2
- 229910017604 nitric acid Inorganic materials 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000012956 testing procedure Methods 0.000 description 2
- 101710134784 Agnoprotein Proteins 0.000 description 1
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- 229910021580 Cobalt(II) chloride Inorganic materials 0.000 description 1
- 241000282414 Homo sapiens Species 0.000 description 1
- 230000010718 Oxidation Activity Effects 0.000 description 1
- 229910002844 PtNi Inorganic materials 0.000 description 1
- 230000010757 Reduction Activity Effects 0.000 description 1
- 238000003917 TEM image Methods 0.000 description 1
- 239000012300 argon atmosphere Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 229910002091 carbon monoxide Inorganic materials 0.000 description 1
- 239000002134 carbon nanofiber Substances 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
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- 230000007797 corrosion Effects 0.000 description 1
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- 238000003912 environmental pollution Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- -1 graphite alkyne Chemical class 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- QWPPOHNGKGFGJK-UHFFFAOYSA-N hypochlorous acid Chemical compound ClO QWPPOHNGKGFGJK-UHFFFAOYSA-N 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical class C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
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- 238000005406 washing Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Images
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/89—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with noble metals
- B01J23/8913—Cobalt and noble metals
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/48—Silver or gold
- B01J23/50—Silver
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/89—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with noble metals
- B01J23/892—Nickel and noble metals
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/89—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with noble metals
- B01J23/8926—Copper and noble metals
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- B01J35/23—
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- B01J35/33—
-
- B01J35/40—
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- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- 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
- H01M4/921—Alloys or mixtures with metallic elements
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/50—Fuel cells
Abstract
The invention provides a preparation method of a low-platinum hollow polyhedral nano-structured catalyst, which comprises the following steps: firstly, preparing a platinum metal precursor solution; then preparing a polyhedral A metal nanoparticle solution; and finally, adding a proper amount of the polyhedral A metal nanoparticle solution into a platinum metal precursor solution, and reacting to obtain the low-platinum hollow polyhedral nanostructured catalyst. The low-platinum hollow polyhedral nano-structured catalyst with different structures, components and sizes can be prepared by changing reaction conditions. The catalyst has a hollow polyhedral nano structure, has good catalytic activity and stability for oxygen reduction and methanol oxidation, and can be applied to electrocatalysts of various energy conversion devices. The preparation method is simple, high in yield and high in catalytic activity, is suitable for large-scale industrial production, and has important significance for promoting the commercialization process of various energy conversion devices.
Description
Technical Field
The invention relates to the field of electrocatalysis, in particular to a preparation method of a low-platinum hollow polyhedral nano-structured catalyst.
Background
With the rapid development of economic society, people are confronted with energy shortage and environmental problems, and development of green energy and exploration of new energy conversion technologies are imperative. The fuel cell adopts sustainable energy as fuel, has the excellent characteristics of environmental protection, high energy conversion rate and the like, and is considered to be one of the ultimate solutions for solving the future energy crisis of human beings. Fuel cells include proton exchange membrane fuel cells, direct alcohol fuel cells, direct acid fuel cells and the like, and these fuel cell catalysts all use expensive and scarce noble metal platinum as a main active component, so that the high cost of the fuel cells has become an important factor for restricting the commercialization process of the fuel cells. Meanwhile, commercial Pt/C catalysts are susceptible to poisoning and deactivation by methanol and carbon monoxide during the reaction process, and the carbon support thereof is easily corroded under the operating conditions of the fuel cell to cause the separation and migration of Pt nanoparticles, which finally results in the loss of active sites, and these problems also severely restrict the further development of the fuel cell. Therefore, the preparation and research of the catalyst with low cost, high activity and high stability are of great significance to the development and popularization of fuel cells.
The low-platinum hollow polyhedral nano-structured catalyst can greatly expose catalytic active sites of the catalyst and enhance the material transmission performance in the reaction process, and is considered to be a very effective method for improving the catalytic activity of the catalyst and reducing the cost of the catalyst. Li et al first prepared a typical palladium icosahedron material by an oil bath method, and further added a platinum precursor solution to the palladium icosahedron solution to prepare a Pd @ Pt core-shell polyhedral material with palladium as a core and platinum as a shell. Then the obtained Pd @ Pt core-shell polyhedral material is placed in a concentrated nitric acid solution for overnight reaction, and finally the ultrathin icosahedral platinum-rich nanocage with a hollow polyhedral nano structure is obtained (J.Am.chem.Soc.,2016,138, 1494-ion 1497). The prepared hollow polyhedral nano-structure low-platinum material greatly improves the utilization rate of platinum atoms, and the catalyst has better electrocatalytic activity under a three-electrode system. However, the method has the advantages of high experimental difficulty, complex operation and control, high energy consumption and high environmental hazard, and simultaneously, a large amount of noble metals are used, so that the problem of the consumption of the noble metals is not fundamentally solved.
Xia et al firstly prepared various palladium polyhedral structure materials (tetrahedron, cube, decahedron and icosahedron) by a multi-step hydrothermal method, and controllably deposited a plurality of platinum atomic layers on the palladium surface to prepare the Pd @ Pt core-shell polyhedral material taking palladium as a core and platinum as a shell. The obtained material is further placed in a mixed solution of hydrochloric acid and ferric trichloride and soaked for 4 hours at 100 ℃, and finally the hollow polyhedral nano-structured low-platinum nanocage or hollow octahedral material is obtained (Science 2015,349, 412-416). Although the material prepared by the technology shows certain oxygen reduction activity, the activity of the material has a large distance from the requirement of practical application, and meanwhile, the problem of the consumption of noble metals is not fundamentally solved.
Yamauchi et al first prepared Ag cubes, then grown mesoporous Pt layers on the prepared Ag cubes by using a non-ionic surfactant as a soft template to realize preparation of Ag @ Pt cube materials, and then mixed the obtained Ag @ Pt cube materials with an excess of nitric acid solution and stirred the mixture solution at room temperature for 3 days to selectively dissolve Ag nuclei, finally obtaining mesoporous platinum hollow cube materials (chem. commun.,2014,50, 15337-. The preparation method of the catalyst has great environmental pollution, and the methanol oxidation activity of the catalyst has a larger difference compared with that of a commercial Pt/C catalyst.
Chinese patent (ZL 200310114338.1) discloses a method for preparing nano-scale metal hollow spheres by directly carrying out a displacement reaction between cobalt nanoparticles serving as sacrificial templates and a metal salt solution. First, the disclosed method can only prepare a single noble metal hollow sphere, and the particle size distribution thereof is not uniform. Second, the hollow metal spheres produced by the disclosed method do not describe or provide proof materials that may be used in catalytic reactions.
Although many efforts are made to apply the low-platinum hollow polyhedral nano-structured catalyst to various energy conversion technologies, the existing catalyst still has the problems of complex preparation technology, great environmental hazard, large consumption of noble metal, poor catalyst activity and stability, no contribution to industrial production and the like. Therefore, it is necessary to develop a simple, economical, environment-friendly, and suitable for large-scale production, and a preparation method of the catalyst with high activity and high stability in the hollow polyhedral nano-structure with low platinum content is provided.
Disclosure of Invention
Therefore, the invention provides a preparation method of a low-platinum hollow polyhedral nano-structured catalyst, which solves the problems.
The technical scheme of the invention is realized as follows: the preparation method of the low-platinum hollow polyhedral nano-structured catalyst comprises the following steps:
(1) preparing a platinum metal precursor solution: dissolving platinum metal salt and a surfactant in a first solvent, then introducing inert gas, and reacting to obtain a platinum metal precursor solution.
(2) Preparing a polyhedral A metal nanoparticle solution: dissolving A metal salt and a surfactant in a first solvent, then introducing inert gas, adding a reducing agent after reaction, and continuing the reaction to obtain the polyhedral A metal nanoparticle solution.
(3) Preparing a low-platinum hollow polyhedral nanostructured catalyst: and (3) adding a certain amount of the polyhedral A metal nanoparticle solution into a platinum metal precursor solution, keeping the inert gas atmosphere, and reacting to obtain the low-platinum hollow polyhedral nanostructured catalyst.
(4) Mixing the low-platinum hollow polyhedral nano-structured catalyst material obtained in the step (3) with a carrier and a second solvent to obtain a supported low-platinum hollow polyhedral nano-structured catalyst, wherein the second solvent is water, ethanol or isopropanol; the carrier is XC-72R carbon black, a carbon nano tube, carbon nano fibers, graphene or graphite alkyne, and the load capacity of the low-platinum hollow nano material on the carrier is 1-50 wt%.
Further, the platinum metal salt in the step (1) is acetylacetone platinum, chloroplatinic acid, potassium chloroplatinate or diamine tetrachloroplatinate; the surfactant is one or more of dodecyl trimethyl ammonium chloride, hexadecyl trimethyl ammonium bromide and polyvinylpyrrolidone; the first solvent is deionized water, alcohols, a mixture of the alcohols and ketone, a mixture of the alcohols and ester, oleylamine, octadecene or oleic acid; the inert gas is argon or nitrogen; the concentration range of the platinum metal salt in the precursor solution is 0.05-10 mg/mL.
Further, the metal salt A in the step (2) is ferric chloride, ferric nitrate, ferric acetate, ferric acetylacetonate, cobalt chloride, cobalt nitrate, cobalt acetate, cobalt acetylacetonate, nickel chloride, nickel nitrate, nickel acetate, nickel acetylacetonate, copper chloride, copper nitrate, copper acetylacetonate, palladium chloride, palladium nitrate, palladium acetate, palladium acetylacetonate; the surfactant is one or more of dodecyl trimethyl ammonium chloride, hexadecyl trimethyl ammonium bromide and polyvinylpyrrolidone; the reducing agent is sodium borohydride, citric acid, ascorbic acid or sodium citrate; the first solvent and the first solvent in the step (1) are the same solvent; the inert gas is argon or nitrogen; the concentration range of the metal A in the solvent is 0.1-20 mg/ml.
Further, the adding speed of the reducing agent in the step (2) is 1.5-15 mg/min.
Further, the low-platinum hollow polyhedral nano-structured catalyst obtained in the step (3) is collected by means of magnet absorption or centrifugation.
Furthermore, the reaction temperature of the preparation steps (1), (2) and (3) is 20-60 ℃, and the reaction time is 0.05-3 h.
Compared with the prior art, the invention has the beneficial effects that:
(1) the method for preparing the low-platinum hollow polyhedral nano-structured catalyst has the advantages of simple and efficient synthesis mode, simple and convenient operation, green and environment-friendly synthesis process, greatly reduces the usage amount of noble metal platinum, can realize large-scale production and preparation of the catalyst, and can effectively reduce the industrial cost of the catalyst;
(2) the invention provides a preparation method of a low-platinum hollow polyhedral nano-structured catalyst with controllable structure, morphology and components, wherein the particle size range of the prepared hollow polyhedral nano-structured low-platinum material is 20-200 nm;
(3) the low-platinum hollow polyhedral nano-structured catalyst provided by the invention effectively utilizes the high utilization rate of platinum with a hollow nano-structure, so that the prepared low-platinum hollow polyhedral nano-structured catalyst has excellent electrocatalytic activity, stability and corrosion resistance, and can meet the application of the catalyst in various energy conversion processes;
(4) the catalyst prepared by the invention has high catalytic performance for the cathode reduction reaction of methanol and oxygen, the activity of unit mass of platinum is 2-20 times that of a commercial Pt/C catalyst, and the catalyst has good stability.
Drawings
FIG. 1 is a TEM image of a low platinum hollow polyhedral nanostructured catalyst (H-PtCo) prepared in example 1.
FIG. 2 is the XRD pattern of the supported low platinum hollow polyhedral nano-structured catalyst (H-PtCo/C) prepared in example 1
FIG. 3 shows the reaction of H-PtCo/C prepared in example 1 and a commercial catalyst at room temperature, 0.1M HClO4Medium oxygen reduction polarization curve.
FIG. 4 shows the reaction conditions of the H-PtCo/C catalyst prepared in example 1 at room temperature, 1M KOH +0.5M CH3Graph of oxidation performance in OH for methanol.
Detailed Description
In order to better understand the technical content of the invention, specific examples are provided below to further illustrate the invention.
The experimental methods used in the examples of the present invention are all conventional methods unless otherwise specified.
The materials, reagents and the like used in the examples of the present invention can be obtained commercially without specific description.
Example 1: H-PtCo low-platinum hollow polyhedral nanostructured catalyst
(1) Preparation of platinum Metal precursor solution
And (3) adding 30ml of ultrapure water into a two-neck flask in a fume hood, then adding 90mg of chloroplatinic acid and 15mg of polyvinylpyrrolidone, introducing argon for protection, and continuing ultrasonic oscillation treatment for 30 minutes to obtain a platinum metal precursor solution.
(2) Preparation of polyhedral Co nanoparticle solution
50ml of deionized water was added to a two-necked flask in a fume hood, followed by 30mg of CoCl2And 50mg of polyvinylpyrrolidone. And (4) continuously performing ultrasonic oscillation treatment, and continuously introducing argon. After 30 minutes, 30mg of NaBH was added dropwise in a two-necked flask4(NaBH4The adding speed is 5mg/min), and after 10 minutes of reaction, the polyhedral Co nanoparticle solution is obtained.
(3) Preparation of low-platinum hollow polyhedral nanostructured catalyst
And (3) dropwise adding 15ml of the Co nano particle solution prepared in the step (2) into the platinum metal precursor solution prepared in the step (1), keeping the argon atmosphere, and continuously carrying out ultrasonic oscillation treatment. After reacting for 30 minutes, stopping gas supply and ultrasonic oscillation treatment, collecting a sample through a magnet, and centrifugally washing the sample for 5 times by using pure water and ethanol to obtain the low-platinum hollow polyhedral nano-structured catalyst (H-PtCo).
(4) Preparation of supported low-platinum hollow polyhedral nano-structured catalyst
Weighing 10mg of low-platinum hollow polyhedral nano-structured catalyst and 40mg of carbon powder (XC-72R), putting into a 25ml beaker, adding 10ml of ethanol, performing ultrasonic treatment for 60min, putting into an oven, drying at 50 ℃ for 12H, and drying to obtain the supported low-platinum hollow polyhedral nano-structured catalyst (H-PtCo/C).
(5) Structural morphology characterization and performance test of catalyst
(A) Structural morphology and element characterization of the catalyst:
the image of the low platinum hollow polyhedral nanostructured catalyst (fig. 1) was observed by Transmission Electron Microscopy (TEM), and the particle size of the low platinum hollow polyhedral nanostructured low catalyst prepared in this example was about 100 nm. And as is apparent from the figure, the prepared catalyst material presents a distinct cubic nanostructure.
The elemental composition information of the low platinum hollow polyhedral nanostructured catalyst was characterized by X-ray diffraction (XRD) (fig. 2). As can be seen from fig. 2, the prepared material exhibited significant XRD diffraction peak information of platinum element.
(B) And (3) testing the catalytic performance of cathode oxygen reduction:
using a three-electrode system, 0.1M HClO saturated in oxygen4In the above, cyclic voltammetric scans were performed at a sweep rate of 5mV/s and an electrode rotation rate of 1600r/min, and the results are shown in FIG. 3.
(C) Testing the catalytic performance of methanol anodic oxidation:
using a three-electrode system at 1M KOH +0.5M CH3The catalytic activity of the catalyst for anodic oxidation of methanol was determined by cyclic voltammetric scanning at a sweep rate of 50mV/s in OH solution, and the results are shown in FIG. 4.
The catalysts prepared in this example were 2.8 times and 1.7 times as active for oxygen reduction and methanol oxidation, respectively, as commercial Pt/C catalysts.
The catalyst of the present invention was tested for cathodic oxygen reduction, anodic methanol oxidation and catalyst stability in the same manner as above except as otherwise specified.
Example 2H-PtNi hollow polyhedral nanostructured Low catalyst
The preparation and testing procedures were exactly the same as in example 1 except that nickel chloride was used instead of cobalt chloride, and the catalyst prepared in this example had an oxygen reduction performance 3.3 times higher than that of the commercial Pt/C catalyst.
Example 3H-PtCu hollow polyhedral nanostructured Low catalyst
The preparation and testing procedures were exactly the same as in example 1 except that nickel chloride was used instead of cobalt chloride, and the catalyst prepared in this example had 1.3 times the oxygen reduction performance of the commercial Pt/C catalyst.
Example 4H-PtAg hollow polyhedral nanostructured Low catalyst
The procedure was as in example 1 except that the following procedure was different from example 1.
(2) Preparation of Ag nanoparticles for seed
In a fume hood, willThe flask was placed in a water bath, and then 30ml of ethylene glycol and 10mg of AgNO were added in order3And 15mg of polyacrylonitrile, the temperature was raised to 60 ℃. And after reacting for 60 minutes, taking out the Ag nano particle solution for later use.
The catalyst prepared in this example had 1.5 times the oxygen reduction performance of the commercial Pt/C catalyst.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (7)
1. A preparation method of a low-platinum hollow polyhedral nano-structured catalyst is characterized by comprising the following steps: the method comprises the following steps:
(1) preparing a platinum metal precursor solution: dissolving platinum metal salt and a surfactant in a first solvent, then introducing inert gas, and reacting to obtain a platinum metal precursor solution.
(2) Preparing a polyhedral A metal nanoparticle solution: dissolving A metal salt and a surfactant in a first solvent, then introducing inert gas, adding a reducing agent after reaction, and continuing the reaction to obtain the polyhedral A metal nanoparticle solution.
(3) Preparing a low-platinum hollow polyhedral nanostructured catalyst: and adding the polyhedral A metal nanoparticle solution into a platinum metal precursor solution, keeping the inert gas atmosphere, and reacting to obtain the low-platinum hollow polyhedral nanostructured catalyst.
2. The method of claim 1, wherein the method comprises the steps of: the platinum metal salt in the step (1) is acetylacetone platinum, chloroplatinic acid, potassium chloroplatinate or diamine tetrachloroplatinate; the surfactant is one or more of dodecyl trimethyl ammonium chloride, hexadecyl trimethyl ammonium bromide and polyvinylpyrrolidone; the first solvent is deionized water, alcohols, a mixture of the alcohols and ketone, a mixture of the alcohols and ester, oleylamine, octadecene or oleic acid; the inert gas is argon or nitrogen; the concentration range of the platinum metal salt in the precursor solution is 0.05-10 mg/mL.
3. The method of claim 1, wherein the method comprises the steps of: the metal salt A in the step (2) is ferric chloride, ferric nitrate, ferric acetate, ferric acetylacetonate, cobalt chloride, cobalt nitrate, cobalt acetate, cobalt acetylacetonate, nickel chloride, nickel nitrate, nickel acetate, nickel acetylacetonate, copper chloride, copper nitrate, copper acetylacetonate, palladium chloride, palladium nitrate, palladium acetate, palladium acetylacetonate; the surfactant is one or more of dodecyl trimethyl ammonium chloride, hexadecyl trimethyl ammonium bromide and polyvinylpyrrolidone; the reducing agent is sodium borohydride, citric acid, ascorbic acid or sodium citrate; the first solvent and the first solvent in the step (1) are the same solvent; the inert gas is argon or nitrogen; the concentration range of the metal A in the solvent is 0.1-20 mg/ml.
4. The method of claim 1, wherein the method comprises the steps of: the adding speed of the reducing agent in the step (2) is 1.5-15 mg/min.
5. The method of claim 1, wherein the method comprises the steps of: and (4) collecting the low-platinum hollow polyhedral nano-structured catalyst obtained in the step (3) in a magnet absorption or centrifugation mode.
6. The method of claim 1, wherein the method comprises the steps of: the reaction temperature of the preparation steps (1), (2) and (3) is 20-60 ℃, and the reaction time is 0.05-3 h.
7. The low platinum hollow polyhedral nanostructured catalyst of claim 1, wherein: the prepared catalyst can be applied to high-efficiency catalytic oxygen reduction reaction and methanol oxidation reaction.
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