JPWO2020130078A1 - 金属、金属酸化物が担持された複合体の製造方法 - Google Patents
金属、金属酸化物が担持された複合体の製造方法 Download PDFInfo
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- JPWO2020130078A1 JPWO2020130078A1 JP2020561510A JP2020561510A JPWO2020130078A1 JP WO2020130078 A1 JPWO2020130078 A1 JP WO2020130078A1 JP 2020561510 A JP2020561510 A JP 2020561510A JP 2020561510 A JP2020561510 A JP 2020561510A JP WO2020130078 A1 JPWO2020130078 A1 JP WO2020130078A1
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- Prior art keywords
- carrier
- metal
- supported
- liquid phase
- reducing agent
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Links
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- 239000002184 metal Substances 0.000 title claims abstract description 58
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- 238000004519 manufacturing process Methods 0.000 title claims description 5
- 239000007791 liquid phase Substances 0.000 claims abstract description 54
- 239000000203 mixture Substances 0.000 claims abstract description 52
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 51
- -1 alcohol compound Chemical class 0.000 claims abstract description 45
- 238000000034 method Methods 0.000 claims abstract description 38
- 150000001768 cations Chemical class 0.000 claims abstract description 27
- 230000009467 reduction Effects 0.000 claims abstract description 27
- 238000002360 preparation method Methods 0.000 claims abstract description 26
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- 150000001875 compounds Chemical class 0.000 claims abstract description 13
- 239000002131 composite material Substances 0.000 claims abstract description 8
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 8
- 230000001603 reducing effect Effects 0.000 claims abstract description 8
- 229910052802 copper Inorganic materials 0.000 claims abstract description 7
- 229910052737 gold Inorganic materials 0.000 claims abstract description 7
- 229910052707 ruthenium Inorganic materials 0.000 claims abstract description 6
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- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 60
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims description 15
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- 239000010948 rhodium Substances 0.000 description 4
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- 150000001298 alcohols Chemical class 0.000 description 3
- 238000006356 dehydrogenation reaction Methods 0.000 description 3
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- 238000001035 drying Methods 0.000 description 3
- 239000000835 fiber Substances 0.000 description 3
- KGRJUMGAEQQVFK-UHFFFAOYSA-L platinum(2+);dibromide Chemical compound Br[Pt]Br KGRJUMGAEQQVFK-UHFFFAOYSA-L 0.000 description 3
- 239000010944 silver (metal) Substances 0.000 description 3
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 2
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- 229910026551 ZrC Inorganic materials 0.000 description 2
- OTCHGXYCWNXDOA-UHFFFAOYSA-N [C].[Zr] Chemical compound [C].[Zr] OTCHGXYCWNXDOA-UHFFFAOYSA-N 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- ODWXUNBKCRECNW-UHFFFAOYSA-M bromocopper(1+) Chemical compound Br[Cu+] ODWXUNBKCRECNW-UHFFFAOYSA-M 0.000 description 2
- 230000005587 bubbling Effects 0.000 description 2
- WXANAQMHYPHTGY-UHFFFAOYSA-N cerium;ethyne Chemical compound [Ce].[C-]#[C] WXANAQMHYPHTGY-UHFFFAOYSA-N 0.000 description 2
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 description 2
- OPQARKPSCNTWTJ-UHFFFAOYSA-L copper(ii) acetate Chemical compound [Cu+2].CC([O-])=O.CC([O-])=O OPQARKPSCNTWTJ-UHFFFAOYSA-L 0.000 description 2
- 239000007772 electrode material Substances 0.000 description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 238000011068 loading method Methods 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 150000004767 nitrides Chemical class 0.000 description 2
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 239000010936 titanium Substances 0.000 description 2
- 238000011282 treatment Methods 0.000 description 2
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- PIGFYZPCRLYGLF-UHFFFAOYSA-N Aluminum nitride Chemical compound [Al]#N PIGFYZPCRLYGLF-UHFFFAOYSA-N 0.000 description 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 1
- 229910001369 Brass Inorganic materials 0.000 description 1
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- 229920000049 Carbon (fiber) Polymers 0.000 description 1
- 229910021594 Copper(II) fluoride Inorganic materials 0.000 description 1
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 description 1
- 229910003771 Gold(I) chloride Inorganic materials 0.000 description 1
- 229910003767 Gold(III) bromide Inorganic materials 0.000 description 1
- 229910003803 Gold(III) chloride Inorganic materials 0.000 description 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 1
- NNWPJQJICQTQOJ-UHFFFAOYSA-N O.[Na+].[Na+].[Na+].[O-]P([O-])[O-] Chemical compound O.[Na+].[Na+].[Na+].[O-]P([O-])[O-] NNWPJQJICQTQOJ-UHFFFAOYSA-N 0.000 description 1
- 229910052581 Si3N4 Inorganic materials 0.000 description 1
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- NRTOMJZYCJJWKI-UHFFFAOYSA-N Titanium nitride Chemical compound [Ti]#N NRTOMJZYCJJWKI-UHFFFAOYSA-N 0.000 description 1
- AQQVTZBWWYVEGR-UHFFFAOYSA-N [NH4+].[O-][PH2]=O Chemical compound [NH4+].[O-][PH2]=O AQQVTZBWWYVEGR-UHFFFAOYSA-N 0.000 description 1
- KTVZJASWYJPWEV-UHFFFAOYSA-M [PH2]([O-])=O.[Li+] Chemical compound [PH2]([O-])=O.[Li+] KTVZJASWYJPWEV-UHFFFAOYSA-M 0.000 description 1
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- BCZWPKDRLPGFFZ-UHFFFAOYSA-N azanylidynecerium Chemical compound [Ce]#N BCZWPKDRLPGFFZ-UHFFFAOYSA-N 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000010951 brass Substances 0.000 description 1
- 150000001649 bromium compounds Chemical class 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
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- 239000004917 carbon fiber Substances 0.000 description 1
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- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 description 1
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 description 1
- 150000001805 chlorine compounds Chemical class 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 229910001431 copper ion Inorganic materials 0.000 description 1
- RFKZUAOAYVHBOY-UHFFFAOYSA-M copper(1+);acetate Chemical compound [Cu+].CC([O-])=O RFKZUAOAYVHBOY-UHFFFAOYSA-M 0.000 description 1
- 229910000009 copper(II) carbonate Inorganic materials 0.000 description 1
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 description 1
- 229910000366 copper(II) sulfate Inorganic materials 0.000 description 1
- GWFAVIIMQDUCRA-UHFFFAOYSA-L copper(ii) fluoride Chemical compound [F-].[F-].[Cu+2] GWFAVIIMQDUCRA-UHFFFAOYSA-L 0.000 description 1
- GEZOTWYUIKXWOA-UHFFFAOYSA-L copper;carbonate Chemical compound [Cu+2].[O-]C([O-])=O GEZOTWYUIKXWOA-UHFFFAOYSA-L 0.000 description 1
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- 239000011646 cupric carbonate Substances 0.000 description 1
- FWBOFUGDKHMVPI-UHFFFAOYSA-K dicopper;2-oxidopropane-1,2,3-tricarboxylate Chemical compound [Cu+2].[Cu+2].[O-]C(=O)CC([O-])(C([O-])=O)CC([O-])=O FWBOFUGDKHMVPI-UHFFFAOYSA-K 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- HTXDPTMKBJXEOW-UHFFFAOYSA-N dioxoiridium Chemical compound O=[Ir]=O HTXDPTMKBJXEOW-UHFFFAOYSA-N 0.000 description 1
- 239000002612 dispersion medium Substances 0.000 description 1
- 150000002222 fluorine compounds Chemical class 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 235000011187 glycerol Nutrition 0.000 description 1
- FDWREHZXQUYJFJ-UHFFFAOYSA-M gold monochloride Chemical compound [Cl-].[Au+] FDWREHZXQUYJFJ-UHFFFAOYSA-M 0.000 description 1
- OVWPJGBVJCTEBJ-UHFFFAOYSA-K gold tribromide Chemical compound Br[Au](Br)Br OVWPJGBVJCTEBJ-UHFFFAOYSA-K 0.000 description 1
- RJHLTVSLYWWTEF-UHFFFAOYSA-K gold trichloride Chemical compound Cl[Au](Cl)Cl RJHLTVSLYWWTEF-UHFFFAOYSA-K 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 150000004679 hydroxides Chemical class 0.000 description 1
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 description 1
- 229910000457 iridium oxide Inorganic materials 0.000 description 1
- 229910001383 lithium hypophosphite Inorganic materials 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 238000011866 long-term treatment Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 150000002823 nitrates Chemical class 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- HBEQXAKJSGXAIQ-UHFFFAOYSA-N oxopalladium Chemical compound [Pd]=O HBEQXAKJSGXAIQ-UHFFFAOYSA-N 0.000 description 1
- SJLOMQIUPFZJAN-UHFFFAOYSA-N oxorhodium Chemical compound [Rh]=O SJLOMQIUPFZJAN-UHFFFAOYSA-N 0.000 description 1
- 229910003445 palladium oxide Inorganic materials 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- ACVYVLVWPXVTIT-UHFFFAOYSA-M phosphinate Chemical compound [O-][PH2]=O ACVYVLVWPXVTIT-UHFFFAOYSA-M 0.000 description 1
- 229910000073 phosphorus hydride Inorganic materials 0.000 description 1
- 229910001380 potassium hypophosphite Inorganic materials 0.000 description 1
- CRGPNLUFHHUKCM-UHFFFAOYSA-M potassium phosphinate Chemical compound [K+].[O-]P=O CRGPNLUFHHUKCM-UHFFFAOYSA-M 0.000 description 1
- XTFKWYDMKGAZKK-UHFFFAOYSA-N potassium;gold(1+);dicyanide Chemical compound [K+].[Au+].N#[C-].N#[C-] XTFKWYDMKGAZKK-UHFFFAOYSA-N 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- WUAPFZMCVAUBPE-UHFFFAOYSA-N rhenium atom Chemical compound [Re] WUAPFZMCVAUBPE-UHFFFAOYSA-N 0.000 description 1
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 description 1
- 229910003450 rhodium oxide Inorganic materials 0.000 description 1
- 229910001925 ruthenium oxide Inorganic materials 0.000 description 1
- WOCIAKWEIIZHES-UHFFFAOYSA-N ruthenium(iv) oxide Chemical compound O=[Ru]=O WOCIAKWEIIZHES-UHFFFAOYSA-N 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- LFAGQMCIGQNPJG-UHFFFAOYSA-N silver cyanide Chemical compound [Ag+].N#[C-] LFAGQMCIGQNPJG-UHFFFAOYSA-N 0.000 description 1
- 229910001961 silver nitrate Inorganic materials 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 1
- SDVHRXOTTYYKRY-UHFFFAOYSA-J tetrasodium;dioxido-oxo-phosphonato-$l^{5}-phosphane Chemical compound [Na+].[Na+].[Na+].[Na+].[O-]P([O-])(=O)P([O-])([O-])=O SDVHRXOTTYYKRY-UHFFFAOYSA-J 0.000 description 1
- 150000003568 thioethers Chemical class 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- ZVWKZXLXHLZXLS-UHFFFAOYSA-N zirconium nitride Chemical compound [Zr]#N ZVWKZXLXHLZXLS-UHFFFAOYSA-N 0.000 description 1
Images
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/88—Processes of manufacture
- H01M4/8825—Methods for deposition of the catalytic active composition
- H01M4/8842—Coating using a catalyst salt precursor in solution followed by evaporation and reduction of the precursor
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
- C25B1/01—Products
- C25B1/02—Hydrogen or oxygen
- C25B1/04—Hydrogen or oxygen by electrolysis of water
-
- 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
- B01J23/42—Platinum
-
- 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
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/48—Silver or gold
- B01J23/52—Gold
-
- 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
- B01J23/72—Copper
-
- 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
- B01J37/16—Reducing
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
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Abstract
Description
一方、液相還元法ではアルコール化合物も使用される。アルコール化合物は温和な還元剤なので取り扱いが容易である。しかし、アルコール化合物を還元剤とした場合には、100℃超の高温で長時間の処理によって還元反応を起こさせる必要がある。高温、長時間の処理は、経済的、時間的コストの増大に繋がる。
アルコール化合物と、ホスフィン酸またはその塩と、担体と、Au、Ag、Cu、Ptのうち少なくともいずれか1つの陽イオンの供給源化合物と、を少なくとも含有する液相混合物を調製する調製工程と、
前記液相混合物中にて前記陽イオンを還元する還元工程と、
を少なくとも含む、
前記還元された陽イオンに由来する金属単体、または、金属酸化物、もしくはその両方を前記担体に担持させて複合体を製造する技術が提供される。
H2PO2 − + H2O → H2PO3 − + 2H・ ・・・(式1)
この原子状の水素が還元種であり、これによって金属陽イオンを還元する。ホスフィン酸イオンを低温加熱するのみでは、この脱水素化反応が起こりにくく、還元剤として機能しない。ここでアルコールが共存すると、ホスフィン酸イオンの脱水素化反応が促進され、低温下でも還元剤として十分に機能する。
調製工程では、第1の還元剤としてのアルコール化合物と、第2の還元剤としてのホスフィン酸またはその塩と、生じた金属単体などを担持させる対象である担体と、還元対象である所定金属の陽イオンの供給源となる化合物と、を添加し混合する。添加順序に特に制限はない。図1の例では、担体、陽イオン供給源化合物、アルコール化合物、ホスフィン酸またはその塩の順に配合する。
調製工程S101において調製された前記液相混合物は、次の還元工程S102に供される。この還元工程において、供給源化合物に由来する所定金属の陽イオンが、アルコール化合物とホスフィン酸または塩とによって還元される。この還元によって、金属単体若しくは金属酸化物またはその両方として、液相混合物中の担体上に析出、若しくは担持の一方、または両方が生じる。よって還元工程は析出工程、担持工程とも表現できる。
還元工程S102によって、所望の粒径の金属単体、若しくは、金属酸化物、またはその両方を担体に担持させて複合体が得られた後、前記の容器または装置にエタノール等の洗浄溶剤を添加し、均一攪拌することで生成した複合体が洗浄される(S103)。このとき必要に応じて、複合体が所定の還元温度から室温(15℃〜30℃)程度まで冷却されても良い。また、この工程は複数回行うこととしても良い。なお、複合体の洗浄が必要ない場合には、この工程を行わなくともよい。
洗浄工程S103が完了すると、得られた複合体が所定の温度(60℃〜90℃)にまで加熱され、常圧条件下または減圧条件下にて乾燥させられる(S104)。
金属陽イオンの供給源として硝酸銅(II)を使用し、担体としてカーボン粒子を使用し、ホスフィン酸塩としてホスフィン酸ナトリウム・1水和物を使用した。0.5gの担体の入ったフラスコに、表1に示す種類、量(mL)のアルコール化合物または水を添加した。その後、表1に示す量のホスフィン酸ナトリウムを配合した。最後に0.795gの硝酸銅を配合し、均一になるよう混合して液相混合物を得た。担体に担持させる銅単体の目標担持量(所望量)は、担体重量を100重量%とした場合の50重量%である。ホスフィン酸ナトリウムは、この目標担持量に対して化学量論的に算出した(例えば、化学量論的に10倍量の時には4.5gのホスフィン酸ナトリウムを配合した)。なお、金属単体を担持させるため、この実施例では、液相混合物に対して窒素ガスバブリングを行い、溶存酸素を予め除去した。
それぞれの液相混合物を表1に示す温度(℃)まで加熱して0.5時間に亘って、金属イオンの還元および担体上への金属担持を行った。
反応終了後、製造された複合体を取り出し、これを適量のエタノールで数回洗浄した。
担持された金属単体の担持量、金属単体粒子の平均粒径をSEMによって評価した(図2参照)。図2において白く光って見える部分が金属単体である。図2に示すように、評価が「○」のものは極めて粒径の小さい(平均粒径が1nm以上100nm未満となる)金属粒子であって、且つ、当該金属粒子が担体均一に担持できている状態を示す。評価が「×」のものは金属単体が担持できていない。評価が「△」のものは金属粒子を担持できているが、粒子がナノ粒子の凝集体であったり、平均粒径100nm以上となるミクロンあるいはサブミクロンオーダーの大きい粒子であったり、不均一に担持されていたりする。
Claims (5)
- 第1の還元剤としてのアルコール化合物と、第2の還元剤としてのホスフィン酸またはその塩と、担体と、Au、Ag、Cu、Pt、Rh、Ru、Re、Pd、Irを含む群より選ばれる1種以上の陽イオンの供給源化合物と、を少なくとも含有する液相混合物を調製する調製工程と、
前記液相混合物中にて前記陽イオンを還元する還元工程と、
を少なくとも含む、
前記還元された陽イオンに由来する金属単体、若しくは、金属酸化物、またはその両方を前記担体に担持させた複合体の製造方法。 - 前記液相混合物に占める水の含有割合が、液相混合物全量基準で1質量%以下であることを特徴とする請求項1に記載の方法。
- 前記アルコール化合物の一部または全部が、エチレングリコールおよびプロピレングリコールからなる群より選択される少なくとも1種であることを特徴とする請求項1または2に記載の方法。
- 前記還元工程が100℃未満の温度にて行われることを特徴とする請求項1〜3のいずれか1項に記載の方法。
- 前記ホスフィン酸またはその塩の含有量が、担体に担持させる所定金属の単体、酸化物またはその両方の量に対して化学量論的に1倍以上であることを特徴とする請求項1〜4のいずれか1項に記載の方法。
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