JP2014516912A - 音波処理によるパラジウム系金属酸化物の合成 - Google Patents
音波処理によるパラジウム系金属酸化物の合成 Download PDFInfo
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- 238000000527 sonication Methods 0.000 title claims abstract description 57
- 229910052763 palladium Inorganic materials 0.000 title claims abstract description 20
- 229910044991 metal oxide Inorganic materials 0.000 title claims description 64
- 150000004706 metal oxides Chemical class 0.000 title claims description 63
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 title abstract description 136
- 230000015572 biosynthetic process Effects 0.000 title description 3
- 238000003786 synthesis reaction Methods 0.000 title description 3
- 238000000034 method Methods 0.000 claims abstract description 69
- 239000002243 precursor Substances 0.000 claims abstract description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910052723 transition metal Inorganic materials 0.000 claims abstract description 6
- -1 transition metal salt Chemical class 0.000 claims abstract description 4
- 229910052751 metal Inorganic materials 0.000 claims description 50
- 239000002184 metal Substances 0.000 claims description 50
- 239000002245 particle Substances 0.000 claims description 41
- 239000000203 mixture Substances 0.000 claims description 35
- 150000003839 salts Chemical class 0.000 claims description 29
- 229910052760 oxygen Inorganic materials 0.000 claims description 15
- 229910052802 copper Inorganic materials 0.000 claims description 13
- 229910052748 manganese Inorganic materials 0.000 claims description 13
- WVDDGKGOMKODPV-UHFFFAOYSA-N Benzyl alcohol Chemical compound OCC1=CC=CC=C1 WVDDGKGOMKODPV-UHFFFAOYSA-N 0.000 claims description 12
- 229910052742 iron Inorganic materials 0.000 claims description 11
- 229910052799 carbon Inorganic materials 0.000 claims description 10
- 229910052717 sulfur Inorganic materials 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical group CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 229910052759 nickel Inorganic materials 0.000 claims description 8
- 230000003647 oxidation Effects 0.000 claims description 8
- 238000007254 oxidation reaction Methods 0.000 claims description 8
- 229910002651 NO3 Inorganic materials 0.000 claims description 7
- 229910052782 aluminium Inorganic materials 0.000 claims description 7
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 7
- 229910052793 cadmium Inorganic materials 0.000 claims description 7
- 229910052804 chromium Inorganic materials 0.000 claims description 7
- 229910052737 gold Inorganic materials 0.000 claims description 7
- 229910052735 hafnium Inorganic materials 0.000 claims description 7
- 229910052741 iridium Inorganic materials 0.000 claims description 7
- 229910052750 molybdenum Inorganic materials 0.000 claims description 7
- 229910052758 niobium Inorganic materials 0.000 claims description 7
- 229910052762 osmium Inorganic materials 0.000 claims description 7
- 239000001301 oxygen Substances 0.000 claims description 7
- 229910052697 platinum Inorganic materials 0.000 claims description 7
- 229910052702 rhenium Inorganic materials 0.000 claims description 7
- 229910052703 rhodium Inorganic materials 0.000 claims description 7
- 229910052707 ruthenium Inorganic materials 0.000 claims description 7
- 229910052709 silver Inorganic materials 0.000 claims description 7
- 229910052715 tantalum Inorganic materials 0.000 claims description 7
- 229910052713 technetium Inorganic materials 0.000 claims description 7
- 229910052719 titanium Inorganic materials 0.000 claims description 7
- 229910052721 tungsten Inorganic materials 0.000 claims description 7
- 229910052720 vanadium Inorganic materials 0.000 claims description 7
- 229910052725 zinc Inorganic materials 0.000 claims description 7
- 229910052726 zirconium Inorganic materials 0.000 claims description 7
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 6
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 5
- 239000003638 chemical reducing agent Substances 0.000 claims description 5
- 239000007789 gas Substances 0.000 claims description 5
- 238000004519 manufacturing process Methods 0.000 claims description 5
- 229910021645 metal ion Inorganic materials 0.000 claims description 5
- 150000003624 transition metals Chemical class 0.000 claims description 5
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 claims description 4
- 235000019445 benzyl alcohol Nutrition 0.000 claims description 4
- 229910052753 mercury Inorganic materials 0.000 claims description 4
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 3
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 3
- 150000002500 ions Chemical class 0.000 claims description 2
- 150000002739 metals Chemical class 0.000 claims description 2
- 239000002002 slurry Substances 0.000 abstract description 11
- 239000011541 reaction mixture Substances 0.000 abstract description 6
- 229910000314 transition metal oxide Inorganic materials 0.000 abstract description 3
- 238000002474 experimental method Methods 0.000 description 11
- 238000005516 engineering process Methods 0.000 description 9
- 239000000523 sample Substances 0.000 description 9
- 239000010949 copper Substances 0.000 description 8
- 239000000126 substance Substances 0.000 description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- HUMNYLRZRPPJDN-UHFFFAOYSA-N benzaldehyde Chemical compound O=CC1=CC=CC=C1 HUMNYLRZRPPJDN-UHFFFAOYSA-N 0.000 description 6
- 238000000634 powder X-ray diffraction Methods 0.000 description 6
- 238000001878 scanning electron micrograph Methods 0.000 description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 5
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 5
- 150000002940 palladium Chemical class 0.000 description 5
- 238000002360 preparation method Methods 0.000 description 5
- 239000003054 catalyst Substances 0.000 description 4
- OPQARKPSCNTWTJ-UHFFFAOYSA-L copper(ii) acetate Chemical compound [Cu+2].CC([O-])=O.CC([O-])=O OPQARKPSCNTWTJ-UHFFFAOYSA-L 0.000 description 4
- 238000009826 distribution Methods 0.000 description 4
- 238000012986 modification Methods 0.000 description 4
- 230000004048 modification Effects 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- YJVFFLUZDVXJQI-UHFFFAOYSA-L palladium(ii) acetate Chemical compound [Pd+2].CC([O-])=O.CC([O-])=O YJVFFLUZDVXJQI-UHFFFAOYSA-L 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- IOVCWXUNBOPUCH-UHFFFAOYSA-M Nitrite anion Chemical compound [O-]N=O IOVCWXUNBOPUCH-UHFFFAOYSA-M 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- QNGNSVIICDLXHT-UHFFFAOYSA-N para-ethylbenzaldehyde Natural products CCC1=CC=C(C=O)C=C1 QNGNSVIICDLXHT-UHFFFAOYSA-N 0.000 description 3
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 3
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 3
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- 239000011701 zinc Substances 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 230000014509 gene expression Effects 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000010335 hydrothermal treatment Methods 0.000 description 2
- 239000010410 layer Substances 0.000 description 2
- 239000012044 organic layer Substances 0.000 description 2
- 229920001223 polyethylene glycol Polymers 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- 238000000611 regression analysis Methods 0.000 description 2
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- 101100172879 Caenorhabditis elegans sec-5 gene Proteins 0.000 description 1
- 229910002480 Cu-O Inorganic materials 0.000 description 1
- XFXPMWWXUTWYJX-UHFFFAOYSA-N Cyanide Chemical compound N#[C-] XFXPMWWXUTWYJX-UHFFFAOYSA-N 0.000 description 1
- YZCKVEUIGOORGS-OUBTZVSYSA-N Deuterium Chemical compound [2H] YZCKVEUIGOORGS-OUBTZVSYSA-N 0.000 description 1
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- 239000003570 air Substances 0.000 description 1
- 125000003158 alcohol group Chemical group 0.000 description 1
- 150000001299 aldehydes Chemical class 0.000 description 1
- 239000000908 ammonium hydroxide Substances 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 150000001879 copper Chemical class 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 239000000412 dendrimer Substances 0.000 description 1
- 229920000736 dendritic polymer Polymers 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000002149 energy-dispersive X-ray emission spectroscopy Methods 0.000 description 1
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000013401 experimental design Methods 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical compound I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 238000003780 insertion Methods 0.000 description 1
- 230000037431 insertion Effects 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000002808 molecular sieve Substances 0.000 description 1
- PZKNFJIOIKQCPA-UHFFFAOYSA-N oxalic acid palladium Chemical compound [Pd].OC(=O)C(O)=O PZKNFJIOIKQCPA-UHFFFAOYSA-N 0.000 description 1
- HBEQXAKJSGXAIQ-UHFFFAOYSA-N oxopalladium Chemical compound [Pd]=O HBEQXAKJSGXAIQ-UHFFFAOYSA-N 0.000 description 1
- 229910003445 palladium oxide Inorganic materials 0.000 description 1
- LWHYKTAISUZRAD-UHFFFAOYSA-L palladium(2+);carbonate Chemical compound [Pd+2].[O-]C([O-])=O LWHYKTAISUZRAD-UHFFFAOYSA-L 0.000 description 1
- PIBWKRNGBLPSSY-UHFFFAOYSA-L palladium(II) chloride Chemical compound Cl[Pd]Cl PIBWKRNGBLPSSY-UHFFFAOYSA-L 0.000 description 1
- 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 description 1
- INIOZDBICVTGEO-UHFFFAOYSA-L palladium(ii) bromide Chemical compound Br[Pd]Br INIOZDBICVTGEO-UHFFFAOYSA-L 0.000 description 1
- GPNDARIEYHPYAY-UHFFFAOYSA-N palladium(ii) nitrate Chemical compound [Pd+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O GPNDARIEYHPYAY-UHFFFAOYSA-N 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 1
- 239000011949 solid catalyst Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/20—Catalysts, in general, characterised by their form or physical properties characterised by their non-solid state
- B01J35/23—Catalysts, in general, characterised by their form or physical properties characterised by their non-solid state in a colloidal state
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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
- B01J23/38—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
- B01J23/60—Platinum group metals with zinc, cadmium or mercury
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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
- B01J23/38—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
- B01J23/64—Platinum group metals with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- 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
- B01J23/64—Platinum group metals with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/656—Manganese, technetium or rhenium
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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
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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
- B01J23/8906—Iron and noble metals
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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
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- 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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- 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
- B01J37/34—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
- B01J37/341—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation
- B01J37/343—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation of ultrasonic wave energy
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/90—Carbides
- C01B32/907—Oxycarbides; Sulfocarbides; Mixture of carbides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G55/00—Compounds of ruthenium, rhodium, palladium, osmium, iridium, or platinum
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G55/00—Compounds of ruthenium, rhodium, palladium, osmium, iridium, or platinum
- C01G55/002—Compounds containing, besides ruthenium, rhodium, palladium, osmium, iridium, or platinum, two or more other elements, with the exception of oxygen or hydrogen
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- Engineering & Computer Science (AREA)
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- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Optics & Photonics (AREA)
- Health & Medical Sciences (AREA)
- Plasma & Fusion (AREA)
- Toxicology (AREA)
- Catalysts (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
Description
本出願は、2011年6月16日に出願したインド特許出願番号第2042/CHE/2011の優先権を主張するものであり、その内容は参照により本明細書に組み込まれる。
水(70mL)中で酢酸パラジウムをエタノール(20mL)により還元し、続いて溶媒を蒸発させて100℃未満の高温において空気中で乾燥させることにより、パラジウム金属(0.106g、1mmol)をミクロン径の粉末状に調製した。Pd金属粉末を水(70mL)中に分散してPd−水スラリーを形成し、酢酸銅(0.20g、1mmol)を混合物に加えた。約10分にわたりスラリーを磁気的に撹拌し、次いで以下に記載の音極(sonotrode)を使用して超音波処理装置内で音波処理してスラリーに直接的に照射して黒色粒子のスラリーを形成した。
アルコール還元法によりパラジウム金属を形成するための前駆体としてパラジウム塩を使用してPd系酸化物を直接調製した。例えば、酢酸パラジウム(0.224g、1mmol)及び酢酸銅(0.200g、1mmol)を、エチルアルコール−水(20mL:70mL)の混合物を含有する100mLのガラス容器中に移した。実施例1に記載したように混合物を音波処理した。
また、18%〜35%の振幅、5秒/1秒〜5秒/4秒のオン/オフ期間、15分〜60分の音波処理期間、及び30℃〜45℃の循環槽温度を用いて音波処理を行った実験計画(DOE)の原則を使用して、Pd系金属酸化物も形成した。以下の音波処理条件、即ち期間:60(分)、振幅割合:25(%)、オン/オフ期間:5秒/1秒、温度:35℃において、最小の粒径350nmを得た。音波処理の周波数を20kHzに固定した。DOEの原則に基づき、反応パラメータによる粒径の変化を調べた。表2は、反応混合物が1mmolの酢酸銅及び1mmolの酢酸パラジウムである場合の様々な音波処理条件に関して得られた粒径を示す。
粒径=5.39−0.0190[期間]+0.0216[振幅]−0.038[オン/オフ]−0.0893[温度]
電圧20.0kV、プローブ電流1.00nA、エネルギー範囲0〜20keVのJEOL6380機械を使用してSEM−EDX分析を実行した。
d=nλ/2Sinθ
(式中、λは使用した放射線(CuKα)の波長であり、θはピーク位置に関する回折角である)。
約80重量%のPVP(Pd金属の重量に基づく)を添加して混合触媒[PVP−Pd−Cu−OC]を生成した以外は実施例1の方法に従ってパラジウム酸化物系触媒を合成した。アルコールからアルデヒドを合成するための、具体的にはベンジルアルコールからベンズアルデヒドへの液相触媒酸化のための酸化触媒として、混合触媒[PVP−Pd−Cu−OC]を調べた。過酸化水素、空気、又は酸素を使用して緩和な条件、即ち大気圧及び30℃において酸化を実行した。表16は、実験5及び6の音波処理を含む、調査した様々な条件を示す。ベンジルアルコールの30%以下の変換を達成した。
カラムの詳細:10%OV17SSカラム、内径1/8インチ、長さ4m
注入器温度:300℃、検出器温度:300℃
オーブン温度(温度プログラミング):
開始温度:175℃
加熱速度:20℃/分
最終温度&保持期間:275℃、5分
ガス圧:窒素3.6bar、水素2bar、空気1bar
超音波プローブを使用する直接的音波分解の代わりに、反応混合物を含有する容器を超音波槽中で同時に連続的かつ間接的に音波処理した(Mark MU2500、120W、30〜36kHz、容量2.5L)以外は、実施例1に示される方法に従ってPd−Cu−O−Cを調製した。温度制御は非等温であった。各反応混合物は、水90mL中にPd及び酢酸銅を含有した。水槽ポンプを使用して反応混合物中に空気をバブリングした。行った16例の実験に関する条件を以下の表17に記載する。
特定の実施形態が例示及び記載されているが、特許請求の範囲で定義された、そのより広い態様における技術から逸脱することなく当業者によって本明細書において変更及び修正が可能であることを理解しなくてはならない。
Claims (26)
- Pd(0)又はその前駆体と、水と、式M1(n+)(式中、M1は酸化状態がn+であるPd以外の任意の金属であり、nは2又は3である)の金属イオンを含む第1の金属塩とを含む混合物を音波分解し、Pd、M1及び酸素を含むPd系金属酸化物を生成することを含む製造方法。
- 前記混合物が、式M2(n+)(式中、M2は酸化状態がn+であるPd以外の任意の金属であり、nは2又は3であり、M1及びM2は異なる金属である)の金属イオンを含む第2の金属塩を更に含み、前記Pd系金属酸化物がM2を更に含む、請求項1に記載の方法。
- M1がPd以外の遷移金属であり、M2がPd以外の遷移金属である、請求項1又は2に記載の方法。
- M1がAl、Ti、V、Cr、Mn、Fe、Co、Ni、Cu、Zn、Zr、Nb、Mo、Tc、Ru、Rh、Ag、Cd、Hf、Ta、W、Re、Os、Ir、Pt、Au又はHgであり、
M2がAl、Ti、V、Cr、Mn、Fe、Co、Ni、Cu、Zn、Zr、Nb、Mo、Tc、Ru、Rh、Ag、Cd、Hf、Ta、W、Re、Os、Ir、Pt、Au又はHgである、請求項1又は2に記載の方法。 - M1がCu、Co、Mn又はFeであり、M2がCu、Co、Mn又はFeである、請求項1又は2に記載の方法。
- 前記第1の金属塩、前記第2の金属塩、又は前記第1及び第2の金属塩のそれぞれが酢酸塩、硫酸塩、炭酸塩、シュウ酸塩、塩化物又は硝酸塩である、請求項1に記載の方法。
- 前記混合物がPd(2+)イオンと、Pd(2+)をPd(0)に還元することができる還元剤とを含む、請求項1に記載の方法。
- 前記還元剤がエタノール又はベンジルアルコールである、請求項7に記載の方法。
- 前記混合物がPd(0)を含む、請求項1に記載の方法。
- 前記混合物が硝酸アニオンを含まず、かつ前記混合物が亜硝酸アニオンを含まない、請求項1に記載の方法。
- 前記音波分解することが直接的音波分解、間接的音波分解、又は直接的音波分解及び間接的音波分解の両方を含む、請求項1に記載の方法。
- 前記音波分解することが1秒〜10秒にわたる音波処理後に続く1秒〜10秒にわたる非音波処理の1回又は複数回のサイクルを含む、請求項1に記載の方法。
- 前記音波分解することが15分〜120分にわたって行われる、請求項1に記載の方法。
- 前記音波分解することが約15kHz〜約25kHzの周波数で行われる、請求項1に記載の方法。
- 音波分解中に前記混合物を気体に散布することを更に含む請求項1に記載の方法。
- 前記音波分解することが約10℃〜約100℃の範囲の温度で行われる、請求項1に記載の方法。
- 前記Pd系金属酸化物が約20nm〜約2000nmの粒径を有する、請求項1に記載の方法。
- 前記Pd(0)又はその前駆体の前記Pd含有量がM1の金属含有量に対して約0.1重量%〜約99.9重量%である、請求項1に記載の方法。
- 前記Pd(0)又はその前駆体の前記Pd含有量がM1及びM2の金属含有量に対して約0.1重量%〜約99.9重量%である、請求項2に記載の方法。
- 前記Pd(0)又はその前駆体の前記Pd含有量がAl、Ti、V、Cr、Mn、Fe、Co、Ni、Cu、Zn、Zr、Nb、Mo、Tc、Ru、Rh、Ag、Cd、Hf、Ta、W、Re、Os、Ir、Pt、Au及びHgから成る群から選択されるM1の金属含有量に対して約0.1重量%〜約99.9重量%である、請求項1に記載の方法。
- 前記Pd(0)又はその前駆体の前記Pd含有量がM1及びM2の金属含有量に対して約0.1重量%〜約99.9重量%であり、M2がAl、Ti、V、Cr、Mn、Fe、Co、Ni、Cu、Zn、Zr、Nb、Mo、Tc、Ru、Rh、Ag、Cd、Hf、Ta、W、Re、Os、Ir、Pt、Au及びHgから成る群から選択される、請求項2に記載の方法。
- M1がCu、Mn、Co又はFeである、請求項20に記載の方法。
- 前記Pd系金属酸化物がC、O、S、又はこれらの内の任意の2つ以上の組み合わせを更に含む、請求項1から22のいずれか一項に記載の方法。
- 前記Pd系金属酸化物が、
約0.25重量%〜約70重量%のPd、
約0.1重量%〜約60重量%のM1、
0重量%〜約35重量%のC、
約5重量%〜約60重量%のO、及び
0重量%〜約30重量%のSを含む、請求項1から22のいずれか一項に記載の方法。 - 前記Pd系金属酸化物が0.1重量%〜約60重量%のM2を更に含む、請求項23に記載の方法。
- 請求項1〜25のいずれか一項に記載の方法で調製されるPd系金属酸化物。
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