JPWO2016136956A1 - 貴金属固溶体担持微粒子の製造方法 - Google Patents
貴金属固溶体担持微粒子の製造方法 Download PDFInfo
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- 229910000510 noble metal Inorganic materials 0.000 title claims abstract description 112
- 239000010419 fine particle Substances 0.000 title claims abstract description 47
- 239000007787 solid Substances 0.000 title claims abstract description 23
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 21
- 239000006104 solid solution Substances 0.000 claims abstract description 44
- 239000000243 solution Substances 0.000 claims abstract description 38
- 239000007788 liquid Substances 0.000 claims abstract description 37
- 150000002736 metal compounds Chemical class 0.000 claims abstract description 35
- 229910052703 rhodium Inorganic materials 0.000 claims abstract description 8
- 229910052763 palladium Inorganic materials 0.000 claims abstract description 5
- 229910052737 gold Inorganic materials 0.000 claims abstract description 4
- 239000002245 particle Substances 0.000 claims description 25
- 239000002904 solvent Substances 0.000 claims description 21
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 15
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 15
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 12
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 12
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- 239000002131 composite material Substances 0.000 claims description 4
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- 150000004681 metal hydrides Chemical class 0.000 claims description 4
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- 229910021393 carbon nanotube Inorganic materials 0.000 claims description 3
- 229910052878 cordierite Inorganic materials 0.000 claims description 3
- JSKIRARMQDRGJZ-UHFFFAOYSA-N dimagnesium dioxido-bis[(1-oxido-3-oxo-2,4,6,8,9-pentaoxa-1,3-disila-5,7-dialuminabicyclo[3.3.1]nonan-7-yl)oxy]silane Chemical compound [Mg++].[Mg++].[O-][Si]([O-])(O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2)O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2 JSKIRARMQDRGJZ-UHFFFAOYSA-N 0.000 claims description 3
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims description 3
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 claims description 3
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- QGLKJKCYBOYXKC-UHFFFAOYSA-N nonaoxidotritungsten Chemical compound O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 QGLKJKCYBOYXKC-UHFFFAOYSA-N 0.000 claims description 3
- XYJRXVWERLGGKC-UHFFFAOYSA-D pentacalcium;hydroxide;triphosphate Chemical compound [OH-].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O XYJRXVWERLGGKC-UHFFFAOYSA-D 0.000 claims description 3
- IYDGMDWEHDFVQI-UHFFFAOYSA-N phosphoric acid;trioxotungsten Chemical compound O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.OP(O)(O)=O IYDGMDWEHDFVQI-UHFFFAOYSA-N 0.000 claims description 3
- 238000009210 therapy by ultrasound Methods 0.000 claims description 3
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims description 3
- 229910001887 tin oxide Inorganic materials 0.000 claims description 3
- 238000011282 treatment Methods 0.000 claims description 3
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- ZZUFCTLCJUWOSV-UHFFFAOYSA-N furosemide Chemical compound C1=C(Cl)C(S(=O)(=O)N)=CC(C(O)=O)=C1NCC1=CC=CO1 ZZUFCTLCJUWOSV-UHFFFAOYSA-N 0.000 claims description 2
- 229910021645 metal ion Inorganic materials 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 2
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- 150000004696 coordination complex Chemical class 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 3
- 229910003771 Gold(I) chloride Inorganic materials 0.000 description 3
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- 238000002441 X-ray diffraction Methods 0.000 description 3
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- FDWREHZXQUYJFJ-UHFFFAOYSA-M gold monochloride Chemical compound [Cl-].[Au+] FDWREHZXQUYJFJ-UHFFFAOYSA-M 0.000 description 3
- 238000005191 phase separation Methods 0.000 description 3
- 238000001350 scanning transmission electron microscopy Methods 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 description 2
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- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 2
- 229910010082 LiAlH Inorganic materials 0.000 description 2
- 238000003917 TEM image Methods 0.000 description 2
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical compound CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 description 2
- HQABUPZFAYXKJW-UHFFFAOYSA-N butan-1-amine Chemical compound CCCCN HQABUPZFAYXKJW-UHFFFAOYSA-N 0.000 description 2
- 238000007872 degassing Methods 0.000 description 2
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- 150000004820 halides Chemical class 0.000 description 2
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- 150000002823 nitrates Chemical class 0.000 description 2
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- 238000006722 reduction reaction Methods 0.000 description 2
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- IYWJIYWFPADQAN-LNTINUHCSA-N (z)-4-hydroxypent-3-en-2-one;ruthenium Chemical compound [Ru].C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O IYWJIYWFPADQAN-LNTINUHCSA-N 0.000 description 1
- SBASXUCJHJRPEV-UHFFFAOYSA-N 2-(2-methoxyethoxy)ethanol Chemical compound COCCOCCO SBASXUCJHJRPEV-UHFFFAOYSA-N 0.000 description 1
- XNWFRZJHXBZDAG-UHFFFAOYSA-N 2-METHOXYETHANOL Chemical compound COCCO XNWFRZJHXBZDAG-UHFFFAOYSA-N 0.000 description 1
- ZNQVEEAIQZEUHB-UHFFFAOYSA-N 2-ethoxyethanol Chemical compound CCOCCO ZNQVEEAIQZEUHB-UHFFFAOYSA-N 0.000 description 1
- 101710134784 Agnoprotein Proteins 0.000 description 1
- 229910000873 Beta-alumina solid electrolyte Inorganic materials 0.000 description 1
- 229910001111 Fine metal Inorganic materials 0.000 description 1
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 150000001242 acetic acid derivatives Chemical class 0.000 description 1
- CUJRVFIICFDLGR-UHFFFAOYSA-N acetylacetonate Chemical compound CC(=O)[CH-]C(C)=O CUJRVFIICFDLGR-UHFFFAOYSA-N 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 229910000905 alloy phase Inorganic materials 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
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- 238000000354 decomposition reaction Methods 0.000 description 1
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- GDVKFRBCXAPAQJ-UHFFFAOYSA-A dialuminum;hexamagnesium;carbonate;hexadecahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Al+3].[Al+3].[O-]C([O-])=O GDVKFRBCXAPAQJ-UHFFFAOYSA-A 0.000 description 1
- XXJWXESWEXIICW-UHFFFAOYSA-N diethylene glycol monoethyl ether Chemical compound CCOCCOCCO XXJWXESWEXIICW-UHFFFAOYSA-N 0.000 description 1
- 229940075557 diethylene glycol monoethyl ether Drugs 0.000 description 1
- 229940105990 diglycerin Drugs 0.000 description 1
- GPLRAVKSCUXZTP-UHFFFAOYSA-N diglycerol Chemical compound OCC(O)COCC(O)CO GPLRAVKSCUXZTP-UHFFFAOYSA-N 0.000 description 1
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 description 1
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- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical class OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 description 1
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- 239000002798 polar solvent Substances 0.000 description 1
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- 229910052707 ruthenium Inorganic materials 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/92—Chemical or biological purification of waste gases of engine exhaust gases
- B01D53/94—Chemical or biological purification of waste gases of engine exhaust gases by catalytic processes
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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
- B01J23/40—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
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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
- B01J37/02—Impregnation, coating or precipitation
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- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/04—Mixing
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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
- B01J37/16—Reducing
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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
- 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
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Abstract
Description
本出願は、2015年2月28日に出願された、日本国特許出願第2015−039680号明細書(その開示全体が参照により本明細書中に援用される)に基づく優先権を主張する。
項1. 互いに相分離する2種の貴金属の化合物と担体を含む溶液を還元性液体に添加する工程を含み、前記2種の貴金属がPdとRu、AgとRh、AuとRhのいずれかである、PdRu、AgRh又はAuRhの固溶体を担体に担持してなる、貴金属固溶体担持微粒子の製造方法。
項2. 担体がアルミナ、ジルコニア、チタニア、セリア、シリカ、シリカアルミナ、カルシア、マグネシア、セリアジルコニア、ランタナ、ランタナアルミナ、酸化スズ、酸化タングステン、アルミノシリケート、アルミノホスフェート、ボロシリケート、リンタングステン酸、ヒドロキシアパタイト、ハイドロタルサイト、ペロブスカイト、コージェライト及びムライトの1種又はこれらの2種以上を含む複合酸化物、シリコンカーバイド、活性炭、カーボンブラック、アセチレンブラック、カーボンナノチューブ及びカーボンナノホーンからなる群から選ばれる、項1に記載の貴金属固溶体担持微粒子の製造方法。
項3. 還元性液体が、グリコール類、グリセリン、ポリグリセリン、アルキレングリコールモノアルキルエーテル及び金属水素化物の溶液からなる群から選ばれる、項1又は2に記載の貴金属固溶体担持微粒子の製造方法。
項4. 担体に担持された固溶体貴金属合金粒子の平均粒径が1〜100 nmである、項1〜3のいずれか1項に記載の貴金属固溶体担持微粒子の製造方法。
項5. 貴金属化合物と担体を溶媒中で混合し、濾過した担体を乾燥、或いは蒸発乾燥し、貴金属イオンが表面に付着した乾燥担体を直接もしくは溶媒に分散させて還元性液体に添加することを特徴とする、項1〜4のいずれか1項に記載の貴金属固溶体担持微粒子の製造方法。
項6. 貴金属化合物と担体を溶媒中で混合し、超音波処理又は脱気処理により担体表面の気泡を除去する工程をさらに含む、項5に記載の貴金属固溶体担持微粒子の製造方法。
Pd:Ru=5〜95モル%:95〜5モル%;好ましくは10〜90モル%:90〜10モル%;より好ましくは15〜85モル%:85〜15モル%、
Ag:Rh=5〜95モル%:95〜5モル%;好ましくは10〜90モル%:90〜10モル%;より好ましくは15〜85モル%:85〜15モル%、
Au:Rh=5〜95モル%:95〜5モル%;好ましくは10〜90モル%:90〜10モル%;より好ましくは15〜85モル%:85〜15モル%。
Au化合物:例えばAuCl3、HAuCl4、K[AuCl4]、Na[AuCl4]、K[Au(CN)2]、K[Au(CN)4]など;Rh化合物:例えばRh(NO3)2、Rh(NO3)3、RhCl2、RhCl3、Rh(CH3COO)3、Rh(CH3COO)2など;Ru化合物:例えばRuCl2、RuCl3、Ru(acac)3 (acacはアセチルアセトンである)、Ru(CH3COO)x (xは2〜3の数を示す)など;
Pd化合物:例えばH2PdCl4又はそのアルカリ金属塩、PdCl2、PdSO4、Pd(NO3)2など;Ag化合物:例えばAgNO3、Ag(CH3COO)など;
好ましい実施形態において、本発明の貴金属固溶体担持微粒子は、2種以上の貴金属化合物を溶媒に溶解して担体を加えた溶液を好ましくは撹拌、振盪もしくは超音波を加えながら還元性液体に加え、加熱して還元反応を進行させることで、得ることができる。還元性液体は、貴金属化合物と担体を含む溶液を加える前に所定の温度に加熱しておくことが好ましい。
10mlの水にK2PdCl4(0.048mmol)、RuCl3・nH2O (0.048mmol)、γ-Al2O3(990mg)を室温で加え、超音波処理によりK2PdCl4とRuCl3を溶解し、担体を含む貴金属化合物溶液(I)を調製した。
10mlの水にK2PdCl4(0.048mmol)、RuCl3・nH2O(0.048mmol)を室温で加え、超音波処理によりK2PdCl4とRuCl3を溶解し、貴金属化合物溶液(II)を調製した。
実施例1と比較例1で得られた微粒子におけるPdRu固溶体の担持量を、γ-Al2O3をバランス成分に設定して定量計算した。結果を図4に示す。定量は傾向X線分析(XRF)法を用いて行った。
Claims (6)
- 互いに相分離する2種の貴金属の化合物と担体を含む溶液を還元性液体に添加する工程を含み、前記2種の貴金属がPdとRu、AgとRh、AuとRhのいずれかである、PdRu、AgRh又はAuRhの固溶体を担体に担持してなる、貴金属固溶体担持微粒子の製造方法。
- 担体がアルミナ、ジルコニア、チタニア、セリア、シリカ、シリカアルミナ、カルシア、マグネシア、セリアジルコニア、ランタナ、ランタナアルミナ、酸化スズ、酸化タングステン、アルミノシリケート、アルミノホスフェート、ボロシリケート、リンタングステン酸、ヒドロキシアパタイト、ハイドロタルサイト、ペロブスカイト、コージェライト及びムライトの1種又はこれらの2種以上を含む複合酸化物、シリコンカーバイド、活性炭、カーボンブラック、アセチレンブラック、カーボンナノチューブ並びにカーボンナノホーンからなる群から選ばれる、請求項1に記載の貴金属固溶体担持微粒子の製造方法。
- 還元性液体が、グリコール類、グリセリン、ポリグリセリン、アルキレングリコールモノアルキルエーテル及び金属水素化物の溶液からなる群から選ばれる、請求項1又は2に記載の貴金属固溶体担持微粒子の製造方法。
- 担体に担持された固溶体貴金属合金粒子の平均粒径が1〜100 nmである、請求項1〜3のいずれか1項に記載の貴金属固溶体担持微粒子の製造方法。
- 貴金属化合物と担体を溶媒中で混合し、濾過した担体を乾燥、或いは蒸発乾燥し、貴金属イオンが表面に付着した乾燥担体を直接もしくは溶媒に分散させて還元性液体に添加することを特徴とする、請求項1〜4のいずれか1項に記載の貴金属固溶体担持微粒子の製造方法。
- 貴金属化合物と担体を溶媒中で混合し、超音波処理又は脱気処理により担体表面の気泡を除去する工程をさらに含む、請求項5に記載の貴金属固溶体担持微粒子の製造方法。
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