CN113368851A - Method for preparing oxide-supported metal and application - Google Patents
Method for preparing oxide-supported metal and application Download PDFInfo
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- CN113368851A CN113368851A CN202110644829.5A CN202110644829A CN113368851A CN 113368851 A CN113368851 A CN 113368851A CN 202110644829 A CN202110644829 A CN 202110644829A CN 113368851 A CN113368851 A CN 113368851A
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- oxide
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- supported metal
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- 229910052751 metal Inorganic materials 0.000 title claims abstract description 105
- 239000002184 metal Substances 0.000 title claims abstract description 102
- 238000000034 method Methods 0.000 title claims abstract description 36
- 239000003054 catalyst Substances 0.000 claims abstract description 75
- 150000003839 salts Chemical class 0.000 claims abstract description 50
- 238000002360 preparation method Methods 0.000 claims abstract description 21
- 238000001354 calcination Methods 0.000 claims abstract description 7
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 18
- 238000006243 chemical reaction Methods 0.000 claims description 16
- 230000003197 catalytic effect Effects 0.000 claims description 14
- 229910052763 palladium Inorganic materials 0.000 claims description 13
- 229910052707 ruthenium Inorganic materials 0.000 claims description 13
- 229910052802 copper Inorganic materials 0.000 claims description 12
- 229910052759 nickel Inorganic materials 0.000 claims description 11
- 238000006555 catalytic reaction Methods 0.000 claims description 10
- 229910052742 iron Inorganic materials 0.000 claims description 9
- -1 alkali metal salt Chemical class 0.000 claims description 8
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 7
- 229910052737 gold Inorganic materials 0.000 claims description 7
- 229910052741 iridium Inorganic materials 0.000 claims description 7
- 229910052762 osmium Inorganic materials 0.000 claims description 7
- 229910052697 platinum Inorganic materials 0.000 claims description 7
- 229910052703 rhodium Inorganic materials 0.000 claims description 7
- 229910052709 silver Inorganic materials 0.000 claims description 7
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 claims description 6
- 238000001953 recrystallisation Methods 0.000 claims description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 claims description 3
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 claims description 3
- UBEWDCMIDFGDOO-UHFFFAOYSA-N cobalt(II,III) oxide Inorganic materials [O-2].[O-2].[O-2].[O-2].[Co+2].[Co+3].[Co+3] UBEWDCMIDFGDOO-UHFFFAOYSA-N 0.000 claims description 3
- 229910052681 coesite Inorganic materials 0.000 claims description 3
- 229910052593 corundum Inorganic materials 0.000 claims description 3
- 229910052906 cristobalite Inorganic materials 0.000 claims description 3
- 238000005984 hydrogenation reaction Methods 0.000 claims description 3
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 238000007254 oxidation reaction Methods 0.000 claims description 3
- 230000008569 process Effects 0.000 claims description 3
- 239000000377 silicon dioxide Substances 0.000 claims description 3
- 229910052682 stishovite Inorganic materials 0.000 claims description 3
- 229910052905 tridymite Inorganic materials 0.000 claims description 3
- 229910001845 yogo sapphire Inorganic materials 0.000 claims description 3
- 229910052684 Cerium Inorganic materials 0.000 claims description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 2
- 239000002253 acid Chemical class 0.000 claims description 2
- 229910052783 alkali metal Inorganic materials 0.000 claims description 2
- 229910052782 aluminium Inorganic materials 0.000 claims description 2
- 229910052786 argon Inorganic materials 0.000 claims description 2
- 150000005323 carbonate salts Chemical class 0.000 claims description 2
- 239000001307 helium Substances 0.000 claims description 2
- 229910052734 helium Inorganic materials 0.000 claims description 2
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 2
- 239000001257 hydrogen Substances 0.000 claims description 2
- 229910052739 hydrogen Inorganic materials 0.000 claims description 2
- 239000011261 inert gas Substances 0.000 claims description 2
- 229910052749 magnesium Inorganic materials 0.000 claims description 2
- 150000002823 nitrates Chemical class 0.000 claims description 2
- 238000000197 pyrolysis Methods 0.000 claims description 2
- 229910052710 silicon Inorganic materials 0.000 claims description 2
- RPACBEVZENYWOL-XFULWGLBSA-M sodium;(2r)-2-[6-(4-chlorophenoxy)hexyl]oxirane-2-carboxylate Chemical compound [Na+].C=1C=C(Cl)C=CC=1OCCCCCC[C@]1(C(=O)[O-])CO1 RPACBEVZENYWOL-XFULWGLBSA-M 0.000 claims description 2
- 150000003467 sulfuric acid derivatives Chemical class 0.000 claims description 2
- 229910052719 titanium Inorganic materials 0.000 claims description 2
- 229910052725 zinc Inorganic materials 0.000 claims description 2
- 229910052726 zirconium Inorganic materials 0.000 claims description 2
- 150000007513 acids Chemical class 0.000 claims 1
- 239000007789 gas Substances 0.000 claims 1
- 238000005406 washing Methods 0.000 abstract description 11
- 238000011068 loading method Methods 0.000 abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 8
- 238000000227 grinding Methods 0.000 abstract description 7
- 230000007547 defect Effects 0.000 abstract description 5
- 230000015572 biosynthetic process Effects 0.000 abstract description 3
- 238000007210 heterogeneous catalysis Methods 0.000 abstract description 3
- 238000002156 mixing Methods 0.000 abstract description 3
- 238000003786 synthesis reaction Methods 0.000 abstract description 3
- 238000005516 engineering process Methods 0.000 abstract description 2
- 230000001105 regulatory effect Effects 0.000 abstract 1
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 18
- 239000000203 mixture Substances 0.000 description 17
- KDLHZDBZIXYQEI-UHFFFAOYSA-N palladium Substances [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 17
- 230000000052 comparative effect Effects 0.000 description 15
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 description 11
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 11
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical compound [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 description 10
- 239000010949 copper Substances 0.000 description 9
- 239000001103 potassium chloride Substances 0.000 description 9
- 235000011164 potassium chloride Nutrition 0.000 description 9
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 8
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 8
- 238000005054 agglomeration Methods 0.000 description 8
- 230000002776 aggregation Effects 0.000 description 8
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 8
- 229910001928 zirconium oxide Inorganic materials 0.000 description 8
- 239000002082 metal nanoparticle Substances 0.000 description 7
- 238000009901 transfer hydrogenation reaction Methods 0.000 description 7
- 150000001299 aldehydes Chemical class 0.000 description 6
- 238000001704 evaporation Methods 0.000 description 6
- 230000008020 evaporation Effects 0.000 description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 6
- 239000007788 liquid Substances 0.000 description 6
- 239000000395 magnesium oxide Substances 0.000 description 6
- 238000013508 migration Methods 0.000 description 6
- 230000005012 migration Effects 0.000 description 6
- 229910000420 cerium oxide Inorganic materials 0.000 description 5
- 239000008367 deionised water Substances 0.000 description 5
- 229910021641 deionized water Inorganic materials 0.000 description 5
- 239000010931 gold Substances 0.000 description 5
- 239000007791 liquid phase Substances 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
- 239000002105 nanoparticle Substances 0.000 description 5
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 description 5
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Substances [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 5
- 239000010944 silver (metal) Substances 0.000 description 5
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 4
- HUMNYLRZRPPJDN-UHFFFAOYSA-N benzaldehyde Chemical compound O=CC1=CC=CC=C1 HUMNYLRZRPPJDN-UHFFFAOYSA-N 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- HYBBIBNJHNGZAN-UHFFFAOYSA-N furfural Chemical compound O=CC1=CC=CO1 HYBBIBNJHNGZAN-UHFFFAOYSA-N 0.000 description 4
- 230000003993 interaction Effects 0.000 description 4
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 4
- 229910044991 metal oxide Inorganic materials 0.000 description 4
- 150000004706 metal oxides Chemical class 0.000 description 4
- 239000000376 reactant Substances 0.000 description 4
- 230000035484 reaction time Effects 0.000 description 4
- 239000000758 substrate Substances 0.000 description 4
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 3
- 239000010941 cobalt Substances 0.000 description 3
- 229910017052 cobalt Inorganic materials 0.000 description 3
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- XPFVYQJUAUNWIW-UHFFFAOYSA-N furfuryl alcohol Chemical compound OCC1=CC=CO1 XPFVYQJUAUNWIW-UHFFFAOYSA-N 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 150000002739 metals Chemical class 0.000 description 3
- 239000002243 precursor Substances 0.000 description 3
- 238000006268 reductive amination reaction Methods 0.000 description 3
- YBCAZPLXEGKKFM-UHFFFAOYSA-K ruthenium(iii) chloride Chemical compound [Cl-].[Cl-].[Cl-].[Ru+3] YBCAZPLXEGKKFM-UHFFFAOYSA-K 0.000 description 3
- 238000009827 uniform distribution Methods 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000003837 high-temperature calcination Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- QNGNSVIICDLXHT-UHFFFAOYSA-N para-ethylbenzaldehyde Natural products CCC1=CC=C(C=O)C=C1 QNGNSVIICDLXHT-UHFFFAOYSA-N 0.000 description 2
- 230000002829 reductive effect Effects 0.000 description 2
- 239000011780 sodium chloride Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 239000007858 starting material Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000001308 synthesis method Methods 0.000 description 2
- 239000002028 Biomass Substances 0.000 description 1
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 238000005576 amination reaction Methods 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- GVPFVAHMJGGAJG-UHFFFAOYSA-L cobalt dichloride Chemical compound [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 150000004696 coordination complex Chemical class 0.000 description 1
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000004070 electrodeposition Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 238000005470 impregnation Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 229910017053 inorganic salt Inorganic materials 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 239000002923 metal particle Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 description 1
- 229910000069 nitrogen hydride Inorganic materials 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 239000010412 oxide-supported catalyst Substances 0.000 description 1
- PIBWKRNGBLPSSY-UHFFFAOYSA-L palladium(II) chloride Chemical compound Cl[Pd]Cl PIBWKRNGBLPSSY-UHFFFAOYSA-L 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 239000010457 zeolite Substances 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
Classifications
-
- 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
- B01J23/40—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals of the platinum group metals
- B01J23/46—Ruthenium, rhodium, osmium or iridium
- B01J23/462—Ruthenium
-
- 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
- B01J23/54—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/56—Platinum group metals
- B01J23/63—Platinum group metals with rare earths or actinides
-
- 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
- B01J23/74—Iron group metals
- B01J23/75—Cobalt
-
- 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
- B01J23/74—Iron group metals
- B01J23/755—Nickel
-
- 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
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/78—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with alkali- or alkaline earth 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/391—Physical properties of the active metal ingredient
- B01J35/393—Metal or metal oxide crystallite size
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/396—Distribution of the active metal ingredient
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
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- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Catalysts (AREA)
Abstract
The disclosure belongs to the technical field of catalyst preparation, and particularly relates to a method for preparing oxide supported metal and application thereof, wherein the preparation method comprises the following steps: grinding and mixing the oxide, the metal source and the salt, calcining in an inert atmosphere, and washing the product with water to obtain the oxide-supported metal catalyst. A series of oxide supported metal catalysts can be prepared by regulating the types of the oxide, the metal source and the salt. The method is simple in preparation, low in cost and universal, overcomes the defects that the existing synthesis technology of the oxide supported metal catalyst is complex and is difficult to prepare on a large scale, and the prepared catalyst is high in metal loading amount and uniform in loading, and has wide practical application prospects in the field of heterogeneous catalysis.
Description
Technical Field
The disclosure belongs to the technical field of catalyst preparation, and particularly relates to a method for preparing oxide supported metal and application thereof.
Background
The information in this background section is only for enhancement of understanding of the general background of the invention and is not necessarily to be construed as an admission or any form of suggestion that this information forms the prior art that is already known to a person of ordinary skill in the art.
The catalyst plays an important role in modern chemical industry, wherein the metal catalyst is widely applied to a plurality of fields such as environmental protection, energy catalysis and the like. In order to increase the atomic utilization of metal atoms, researchers have reduced the catalyst particle size to the nanometer or even atomic scale. In order to stabilize these nanoparticles, they are usually supported on supports with a high specific surface area, including oxides, carbon materials, ceramics, zeolites, etc., to form so-called supported metal catalysts, which constitute the main force of heterogeneous catalysis.
Among the various supported metal catalysts, metal catalysts based on oxide supports are of particular interest, since oxides generally exhibit special and variable properties, such as surface basicity and redox characteristics (particularly when reducible metals are involved), which lead to specific catalytic properties. In addition, the oxide surface has abundant defect sites (steps, corners, vacancies) and — OH groups can serve as anchor sites for a single metal atom. The strong interaction between the metal and the oxide enables the catalyst to have a stable chemical structure, and greatly influences the performance of the catalyst through a synergistic effect. The stability of the oxides at high temperatures is also an important starting point for increasing the mechanical and thermal stability of the metal catalysts.
The preparation of the oxide supported metal catalyst is a precondition for researching the structure and the catalytic performance of the oxide supported metal catalyst. Loading the metal precursor onto the surface of the oxide support is easy, but how to achieve uniform dispersion of the metal precursor and how to prevent migration agglomeration of metal atoms has certain challenges. Various methods have been developed for preparing oxide-supported metal catalysts, including impregnation, co-precipitation, ion exchange, deposition-precipitation, strong electrostatic adsorption, photochemical deposition, electrochemical deposition, and the like. These synthesis methods still have many problems, such as the synthesis methods are complicated, the precursors used are expensive, large-scale preparation is difficult, and the like, and the preparation methods are often effective only for one metal and lack a general strategy for preparing oxide-supported metal catalysts that is effective for a plurality of metals. In view of the superiority of the oxide supported metal catalyst in the field of catalysis, the development of a simple and universal preparation method of the oxide supported metal catalyst has important practical application significance.
Disclosure of Invention
In order to solve the problems in the prior art, the method for preparing the oxide supported metal and the application thereof are provided in the disclosure, the method is simple to prepare, low in cost and universal, the defects that the existing oxide supported metal catalyst is complex in synthesis technology and difficult to prepare in a large scale are overcome, and the prepared catalyst is high in metal loading amount, uniform in loading and wide in practical application prospect in the field of heterogeneous catalysis.
Specifically, the technical scheme of the present disclosure is as follows:
in a first aspect of the disclosure, a method of making an oxide supported metal, comprising the steps of:
the oxide, metal source and salt are ground and mixed evenly and calcined under inert atmosphere.
In a second aspect of the disclosure, the oxide supported metal catalyst prepared by the preparation method contains one metal and a plurality of metal catalytic active sites of Fe, Co, Ni, Cu, Pt, Pd, Au, Ag, Ru, Rh, Ir, and Os.
In a third aspect of the present disclosure, the use of the oxide-supported metal catalyst in a heterogeneously catalyzed reaction.
One or more technical schemes in the disclosure have the following beneficial effects:
(1) the method has universality and is suitable for oxide Fe2O3、Fe3O4、Co3O4、NiO、CuO、ZnO、MgO、Al2O3、ZrO2、CeO2、TiO2And SiO2All effective for supporting Fe, Co, Ni, Cu, Pt, Pd, Au, Ag, Ru, Rh, Ir and Os.
(2) The salt used in the method is a cheap industrial raw material, and compared with other methods, the method has the advantages of low cost and strong operability, can be used for synthesizing the oxide supported metal catalyst on a large scale, and solves the defects of complex synthesis and difficulty in large-scale preparation in other prior art.
(3) The catalyst prepared by the method has high metal loading amount, uniform loading, no obvious phenomena of agglomeration and migration of metal particles, and uniform and stable distribution of metal on the surface of the oxide carrier.
(4) The catalyst prepared by the method disclosed by the invention is suitable for various heterogeneous catalytic reactions and has a wide industrial application prospect.
Detailed Description
The disclosure is further illustrated with reference to specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present disclosure. The experimental procedures, in which specific conditions are not noted in the following examples, are generally carried out according to conventional conditions or according to conditions recommended by the manufacturers.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art. The reagents or starting materials used in the present invention can be purchased from conventional sources, and unless otherwise specified, the reagents or starting materials used in the present invention can be used in a conventional manner in the art or in accordance with the product specifications. In addition, any methods and materials similar or equivalent to those described herein can be used in the methods of the present invention. The preferred embodiments and materials described herein are intended to be exemplary only.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of example embodiments according to the present disclosure. As used herein, the singular forms "a", "an" and "the" are intended to include the plural forms as well, and it should be understood that when the terms "comprises" and/or "comprising" are used in this specification, they specify the presence of the stated features, steps, operations, and/or combinations thereof, unless the context clearly indicates otherwise.
At present, the method for preparing the metal oxide supported catalyst has no universality, is only suitable for one or two metals, and cannot realize that the same method is suitable for preparing a plurality of different metal oxide supported metal catalysts. In addition, the traditional method has complex preparation process, metal is easy to agglomerate and migrate on the surface of the oxide, the bonding force between the metal and the metal oxide is poor, the structure is unstable, the metal is easy to fall off in the reaction process, and the like.
In one embodiment of the present disclosure, a method of making an oxide supported metal, comprising the steps of: the oxide, metal source and salt are ground and mixed evenly and calcined under inert atmosphere.
And after calcination, washing the obtained product with water, and drying to obtain the oxide supported metal catalyst. The method is simple and high in applicability, the oxide, the metal source and the salt are directly ground and mixed, the inorganic salt is converted into a molten state at high temperature, the liquid phase environment provided by the method is beneficial to full contact between the oxide and the metal, and the problems that an oxide carrier and the metal are weak in binding force in the preparation process and the metal is easy to fall off on the surface of the carrier in a catalytic reaction in the traditional method are solved. The method for preparing the oxide-supported metal by using the assistance of the molten salt can improve the dispersion degree of the oxide, ensure that the metal can be completely dissolved in a system formed by the molten salt to be uniform, regulate and control the size of metal nanoparticles and effectively prevent the metal from agglomerating.
However, the conventional method is to perform high-temperature calcination in a muffle furnace to prepare an oxide-supported metal catalyst during the preparation of the oxide. The method has the serious defects that the metal cannot be uniformly and stably loaded on the surface of the oxide carrier, the metal is easy to agglomerate and migrate, and the bonding force between the metal and the oxide is poor and the metal is easy to fall off.
Furthermore, the salt-containing washing liquid is evaporated and recrystallized, and the salt is recycled, so that the method greatly reduces the production cost, effectively realizes the efficient utilization of the salt-containing solution, and is favorable for realizing large-scale popularization and production.
Further, the oxide is selected from oxides containing one or more elements of Fe, Co, Ni, Cu, Zn, Mg, Al, Zr, Ce, Ti and Si; preferably Fe2O3、Fe3O4、Co3O4、NiO、CuO、ZnO、MgO、Al2O3、ZrO2、CeO2、TiO2And SiO2。
Further, the metal source is selected from one or more of metal elements containing Fe, Co, Ni, Cu, Pt, Pd, Au, Ag, Ru, Rh, Ir and Os, and specifically is a metal salt, an acid or a metal complex corresponding to the metal elements.
Further, the salt is an alkali metal salt, preferably one or more of Li salt, Na salt, and K salt, and specifically, a halide salt, nitrate salt, sulfate salt, and carbonate salt corresponding thereto.
Further, the mass ratio of the oxide to the metal in the metal source is between 10:1 and 1000:1, preferably between 20:1 and 200: 1; or the mass ratio of the oxide to the salt is between 1:1 and 1:50, preferably between 1:2 and 1: 20. During the calcination, the reactants react uniformly and stably in the molten salt liquid phase system, however, if the amount of molten salt is too small, the molten salt cannot function as a liquid phase. When the amount of the salt is too large, the uniform and stable oxide-supported metal catalyst is not easy to obtain, because the excessive amount of the molten salt can reduce the migration rate among reactants, so that the reaction rate is reduced, and the uniform distribution of the metal on the oxide carrier is influenced; secondly, the overflow of the molten salt is caused due to the excessive amount of the molten salt, the overflowed molten salt cannot be used as a solvent, reactants cannot fully utilize the molten salt, and a stable and uniform liquid phase system is not provided; in addition, if the amounts of the oxide, the metal source and the salt are not controlled at a certain ratio, and the amount of the salt is controlled, the excessive molten salt promotes irregular migration of metal ions on the surface of the oxide, thereby causing agglomeration or the like on the surface of the oxide.
Further, the calcination temperature is between 122 and 1069 ℃, preferably between 300 and 900 ℃, and more preferably between 500 and 801 ℃; or the high-temperature pyrolysis time is 0.5-10 h, preferably 2-5 h; or the atmosphere of the inert gas is one or more of nitrogen, argon, helium and hydrogen. The calcination temperature needs to be controlled while the dosage ratio of each reactant is well controlled. During the high-temperature calcination process, the migration rate of ions is accelerated along with the increase of the temperature, so that the reaction is promoted, meanwhile, the evaporation of the molten salt is increased, and the holding time is generally determined by the reaction rate and the size and the shape of the product, so that the control of the specific reaction temperature and the reaction time plays an important role in forming uniform and stable oxide-supported metal.
In one embodiment of the disclosure, the oxide supported metal catalyst prepared by the preparation method contains one or more metal catalytic active sites of Fe, Co, Ni, Cu, Pt, Pd, Au, Ag, Ru, Rh, Ir, and Os. Based on the method, one metal of Fe, Co, Ni, Cu, Pt, Pd, Au, Ag, Ru, Rh, Ir and Os can be uniformly and stably loaded on the surface of the oxide carrier, the phenomena of metal migration, agglomeration and the like can not occur due to the high-efficiency control of the preparation method, in addition, the molten salt provides the optimal liquid phase environment for the loading of the metal by reasonably adjusting the preparation method, and the metal to be loaded and the surface of the oxide carrier form stronger bonding force, so that the metal cannot fall off in the catalytic reaction process due to the strong bonding force, and the catalytic stability of the catalyst is improved. In addition, the oxide supported metal catalyst obtained based on the method can expose more active sites, and the catalytic activity of the catalyst is improved.
In one embodiment of the present disclosure, the oxide-supported metal catalyst is used in a heterogeneous catalytic reaction. Further, the oxide supported metal catalyst is applied to a water vapor shift reaction, a CO preferential oxidation reaction, a selective hydrogenation reaction and a photoelectrocatalysis reaction.
In order to make the technical solutions of the present disclosure more clearly understood by those skilled in the art, the technical solutions of the present disclosure will be described in detail below with reference to specific embodiments.
Example 1
A zirconium oxide loaded ruthenium metal catalyst is prepared by the following specific steps:
uniformly mixing 1.0g of commercial zirconium oxide, 103.7mg of ruthenium chloride, 10.0g of lithium chloride and potassium chloride (mass ratio is 1:4) by grinding, placing the mixture in a small crucible, heating the mixture from room temperature 20 ℃ to 500 ℃ under Ar atmosphere, keeping the temperature at the rate of 2 ℃/min for 2h, cooling the mixture to room temperature, washing the obtained salt-containing mixture by using deionized water, and centrifuging the salt-containing mixture for three times, wherein a centrifugal lower-layer product is dried to obtain 1.04g of a target product, namely the zirconium oxide supported ruthenium metal catalyst, in particular to the zirconium oxide supported ruthenium catalyst. And the salt-containing washing liquid can recover lithium chloride and potassium chloride again through evaporation recrystallization operation.
Example 2
A cerium oxide supported palladium catalyst is prepared by the following specific steps:
uniformly mixing 1.0g of commercial cerium oxide, 20.0mg of potassium chloropalladite and 10.0g of sodium chloride by grinding, placing the mixture in a small crucible, heating the mixture from room temperature of 20 ℃ to 800 ℃ under the atmosphere of Ar at the heating rate of 5 ℃/min, keeping the temperature for 2h, cooling the mixture to the room temperature, washing the obtained salt-containing mixture by using deionized water, and centrifuging the mixture for three times, wherein a centrifugal lower-layer product is dried to obtain 0.97g of a target product, and the product is an oxide supported metal catalyst, in particular a cerium oxide supported palladium catalyst. And the salt-containing washing liquid can recover sodium chloride again through evaporation and recrystallization operations.
Example 3
A titanium oxide supported nickel metal catalyst is prepared by the following specific steps:
1.0g of commercial titanium oxide, 20.0mg of nickel chloride and 2.0g of potassium chloride were mixed homogeneously by grinding, the mixture was placed in a small crucible under N2Under the atmosphere, the temperature is raised from room temperature of 20 ℃ to 800 ℃, and the temperature raising rate is 5 ℃/miAnd n, keeping the temperature for 2 hours, cooling to room temperature, washing the obtained salt-containing mixture with deionized water, centrifuging for three times, drying a product at the lower layer of the centrifugation to obtain 0.96g of a target product, wherein the product is the titanium oxide supported nickel metal catalyst, and specifically the titanium oxide supported nickel catalyst. And the salt-containing washing liquid can recover the potassium chloride again through evaporation and recrystallization operations.
Example 4
An iron oxide supported cobalt metal catalyst is prepared by the following specific steps:
2.0g of iron oxide, 20.0mg of cobalt chloride and 2.0g of lithium chloride and potassium chloride (mass ratio 9:11) were mixed by grinding to homogeneity, the mixture was placed in a small crucible and heated under N2In the atmosphere, the temperature is raised from the room temperature of 20 ℃ to 600 ℃ at the temperature raising rate of 8 ℃/min, the temperature is kept for 2h, after the temperature is cooled to the room temperature, the obtained salt-containing mixture is washed by deionized water and centrifuged for three times, wherein a centrifuged lower-layer product is dried to obtain 1.95g of a target product, the product is the iron oxide supported cobalt metal catalyst, and cobalt metal nanoparticles are uniformly and stably distributed on the surface of the iron oxide without agglomeration imagination. And the salt-containing washing liquid can recover lithium chloride and potassium chloride again through evaporation recrystallization operation.
Example 5
A magnesium oxide loaded copper metal catalyst is prepared by the following specific steps:
1.5g of magnesium oxide, 5.0mg of copper chloride and 1.5g of potassium chloride are mixed homogeneously by grinding, the mixture is placed in a small crucible under N2In the atmosphere, the temperature is raised from the room temperature of 20 ℃ to 800 ℃ at the temperature raising rate of 8 ℃/min, the temperature is kept for 2h, after the temperature is cooled to the room temperature, the obtained salt-containing mixture is washed by deionized water and centrifuged for three times, wherein a centrifuged lower-layer product is dried to obtain 1.46g of a target product, the product is the magnesium oxide supported copper metal catalyst, and copper metal nanoparticles are uniformly and stably distributed on the surface of magnesium oxide without agglomeration imagination. And the salt-containing washing liquid can recover the potassium chloride again through evaporation and recrystallization operations.
Comparative example 1:
compared with example 1, the difference is that: zirconium oxide, lithium chloride and potassium chloride (mass ratio of 1:4) are uniformly mixed by grinding without adding ruthenium chloride, and the mixture is directly calcined at high temperature in Ar atmosphere to obtain the metal-free zirconium oxide catalyst.
Comparative example 2:
compared with example 1, the difference is that: the mass ratio of ruthenium chloride to zirconium oxide is 1:50, and the ruthenium metal nanoparticles of the catalyst are uniformly distributed on the surface of cerium oxide, but the distribution amount is small.
Comparative example 3:
compared with example 3, the difference is that: the mass ratio of cerium oxide to palladium chloride is 5:1, a large amount of agglomeration occurs on the surface of alumina by the palladium metal nanoparticles of the catalyst, and the palladium cannot be uniformly dispersed on the surface of the alumina.
Comparative example 4:
compared with example 3, the difference is that: the calcination temperature is 1300 ℃, partial agglomeration of palladium metal nanoparticles of the catalyst occurs on the surface of alumina, palladium cannot be uniformly dispersed on the surface of alumina, and the recovery rate of salt is low.
And (3) testing the performance of the catalyst:
(1) reductive amination reaction of aldehyde and ketone
The direct amination preparation of amine compounds from biomass-derived aldehyde and ketone compounds by using ammonia as a nitrogen source is one of the research hotspots in the field of organic chemistry in recent years. The performance of the catalyst (activity, selectivity and stability) is limited by the strong metal-support interaction (SMSI effect), which in turn depends on the size of the metal nanoparticles. Based on the catalysts of example 1 and comparative examples 1-2, the performance of the catalyst in catalyzing reductive amination of benzaldehyde to prepare amine compounds is tested, wherein the reaction substrate is 1mmol of benzaldehyde, the dosage of the catalyst is 10mg, and the catalytic reaction is performed at 3MPa H2、0.5MPa NH3The reaction time is 4h, and the substrate conversion rate and the selectivity of the amine compound are compared, and the reaction time is specifically shown in table 1:
| reductive amination catalyst | Conversion (%) | Selectivity (%) |
| Example 1 | 100 | 97.3 |
| Comparative example 1 | 100 | 79.5 |
| Comparative example 2 | 70.8 | 0 |
The results show that the catalyst prepared in example 1 successfully introduced ruthenium on the zirconia surface, providing active sites for catalytic reactions while increasing substrate conversion and product selectivity. This is a strong signal of the interaction force of the metal and the oxide support due to the uniform distribution of ruthenium nanoparticles on the zirconia surface. While the ruthenium nanoparticles on the surface of the zirconia in the comparative example 2 are less distributed, only a small amount of catalytic active sites are exposed, and the selectivity of the product is relatively poor.
(2) Catalytic transfer hydrogenation performance
Alpha, beta-unsaturated alcohol is an important fine chemical product, is usually prepared by selective hydrogenation of alpha, beta-unsaturated aldehyde, and is very key to realizing efficient preparation of the alpha, beta-unsaturated alcohol by developing a catalyst for catalyzing transfer hydrogenation of the alpha, beta-unsaturated aldehyde. Usually, the metal oxide catalyst containing acid-base sites shows good catalytic activity and selectivity in catalyzing the transfer hydrogenation reaction of alpha, beta-unsaturated aldehyde, and the catalytic activity can be further improved by introducing noble metals on the surface of an oxide carrier. Based on the zirconium oxide supported ruthenium metal catalyst prepared in example 1, the catalyst shows good activity and selectivity in catalyzing alpha, beta-unsaturated aldehyde to prepare alpha, beta-unsaturated alcohol. The performance of catalyzing furfural transfer hydrogenation to prepare furfuryl alcohol by using the catalyst contained in example 1 and comparative examples 1-4 was tested by using a reaction substrate of 1mmol of furfural, the catalyst amount of 80mg, a solvent of 10ml of isopropanol, the reaction temperature of 150 ℃ and the reaction time of 6h, and the specific results are shown in table 2:
| catalyst and process for preparing same | Conversion (%) | Selectivity (%) |
| Example 1 | 95.4 | 100 |
| Comparative example 1 | 32.5 | 100 |
| Comparative example 2 | 75.4 | 100 |
| Comparative example 3 | 80.1 | 83.7 |
| Comparative example 4 | 68.2 | 80.3 |
The result shows that the catalyst prepared in example 1 has more active sites exposed due to the uniform distribution of ruthenium nanoparticles on the surface of zirconia, so that the catalytic transfer hydrogenation activity is greatly improved, and the catalytic performance of the catalysts in comparative examples 1-4 is far worse than that of example 1. In addition, after the transfer hydrogenation catalyst in the embodiment 1 is recycled for 3 times, the ruthenium nanoparticles are still uniformly and stably loaded on the surface of the zirconia, while the zirconia surfaces in the comparative examples 3-4 are greatly changed, and the ruthenium metal falls off, so that the preparation method is proved to be capable of greatly improving the interaction force between the metal and the oxide carrier, and further improving the catalytic transfer hydrogenation performance.
Although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A method for preparing an oxide supported metal, comprising the steps of:
the oxide, metal source and salt are ground and mixed evenly and calcined under inert atmosphere.
2. A process for the preparation of an oxide supported metal as claimed in claim 1 wherein the salt-containing wash solution is subjected to evaporative recrystallisation and the recycled salt is recovered.
3. The method of claim 1, wherein the oxide is selected from the group consisting of oxides containing one or more elements selected from the group consisting of Fe, Co, Ni, Cu, Zn, Mg, Al, Zr, Ce, Ti, Si; preferably Fe2O3、Fe3O4、Co3O4、NiO、CuO、ZnO、MgO、Al2O3、ZrO2、CeO2、TiO2And SiO2。
4. The method according to claim 1, wherein the metal source is selected from one or more of the group consisting of Fe, Co, Ni, Cu, Pt, Pd, Au, Ag, Ru, Rh, Ir, and Os metal elements, and is selected from their corresponding metal salts, acids, and metal complexes.
5. The method according to claim 1, wherein the salt is an alkali metal salt, preferably one or more of a Li salt, a Na salt and a K salt, and more particularly, a halide salt, a nitrate salt, a sulfate salt and a carbonate salt thereof.
6. The method of claim 1, wherein the mass ratio of the oxide to the metal of the metal source is between 10:1 and 1000:1, preferably between 20:1 and 200: 1; or the mass ratio of the oxide to the salt is between 1:1 and 1:50, preferably between 1:2 and 1: 20.
7. The method of claim 1, wherein the calcination temperature is between 122 ℃ and 1069 ℃, preferably between 300 ℃ and 900 ℃, and more preferably between 500 ℃ and 801 ℃; or the high-temperature pyrolysis time is 0.5-10 h, preferably 2-5 h; or the atmosphere of the inert gas is one or more of nitrogen, argon, helium and hydrogen.
8. The oxide-supported metal catalyst prepared by the preparation method as set forth in any one of claims 1 to 7, wherein the oxide-supported metal catalyst contains one or more metal catalytic active sites selected from the group consisting of Fe, Co, Ni, Cu, Pt, Pd, Au, Ag, Ru, Rh, Ir and Os.
9. Use of the oxide-supported metal catalyst of claim 8 in a heterogeneously catalyzed reaction.
10. The use according to claim 9, wherein the oxide-supported metal catalyst is used in a water-gas shift reaction, a preferential oxidation reaction of CO, a selective oxidation reaction, a selective hydrogenation reaction, and a photoelectrocatalytic reaction.
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