JP5235140B2 - 白金族ナノ粒子担持材料とその製造方法、白金族ナノ粒子の析出方法、触媒材料 - Google Patents
白金族ナノ粒子担持材料とその製造方法、白金族ナノ粒子の析出方法、触媒材料 Download PDFInfo
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- JP5235140B2 JP5235140B2 JP2009005113A JP2009005113A JP5235140B2 JP 5235140 B2 JP5235140 B2 JP 5235140B2 JP 2009005113 A JP2009005113 A JP 2009005113A JP 2009005113 A JP2009005113 A JP 2009005113A JP 5235140 B2 JP5235140 B2 JP 5235140B2
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- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical group [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 title claims description 93
- 239000002105 nanoparticle Substances 0.000 title claims description 60
- 239000000463 material Substances 0.000 title claims description 36
- 239000003054 catalyst Substances 0.000 title claims description 25
- 238000004519 manufacturing process Methods 0.000 title claims description 11
- 238000000151 deposition Methods 0.000 title claims description 6
- 241000894006 Bacteria Species 0.000 claims description 35
- 238000000034 method Methods 0.000 claims description 35
- 230000000813 microbial effect Effects 0.000 claims description 35
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 21
- -1 platinum group ion Chemical class 0.000 claims description 17
- 239000007789 gas Substances 0.000 claims description 16
- 229910052739 hydrogen Inorganic materials 0.000 claims description 15
- 239000001257 hydrogen Substances 0.000 claims description 15
- 244000005700 microbiome Species 0.000 claims description 10
- 239000007788 liquid Substances 0.000 claims description 8
- 241000863432 Shewanella putrefaciens Species 0.000 claims description 6
- 230000001603 reducing effect Effects 0.000 claims description 6
- 238000005372 isotope separation Methods 0.000 claims description 3
- 150000007524 organic acids Chemical class 0.000 claims description 3
- 229910052697 platinum Inorganic materials 0.000 description 26
- 239000000243 solution Substances 0.000 description 15
- 239000002245 particle Substances 0.000 description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 9
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 9
- YZCKVEUIGOORGS-OUBTZVSYSA-N Deuterium Chemical compound [2H] YZCKVEUIGOORGS-OUBTZVSYSA-N 0.000 description 8
- 229910052805 deuterium Inorganic materials 0.000 description 8
- 239000002609 medium Substances 0.000 description 8
- 239000005909 Kieselgur Substances 0.000 description 7
- 230000008569 process Effects 0.000 description 6
- 239000011780 sodium chloride Substances 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 5
- 238000002083 X-ray spectrum Methods 0.000 description 4
- 239000002253 acid Substances 0.000 description 4
- 150000002500 ions Chemical class 0.000 description 4
- 241001112696 Clostridia Species 0.000 description 3
- 241001135750 Geobacter Species 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 150000001720 carbohydrates Chemical class 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 238000009833 condensation Methods 0.000 description 3
- 230000005494 condensation Effects 0.000 description 3
- 238000000227 grinding Methods 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- 238000010298 pulverizing process Methods 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- 239000007790 solid phase Substances 0.000 description 3
- 239000012808 vapor phase Substances 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 2
- 241000863430 Shewanella Species 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 125000004429 atom Chemical group 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 239000012876 carrier material Substances 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000009388 chemical precipitation Methods 0.000 description 2
- 230000003247 decreasing effect Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000011261 inert gas Substances 0.000 description 2
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 239000002243 precursor Substances 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 238000003980 solgel method Methods 0.000 description 2
- JKMHFZQWWAIEOD-UHFFFAOYSA-N 2-[4-(2-hydroxyethyl)piperazin-1-yl]ethanesulfonic acid Chemical compound OCC[NH+]1CCN(CCS([O-])(=O)=O)CC1 JKMHFZQWWAIEOD-UHFFFAOYSA-N 0.000 description 1
- GUBGYTABKSRVRQ-XLOQQCSPSA-N Alpha-Lactose Chemical compound O[C@@H]1[C@@H](O)[C@@H](O)[C@@H](CO)O[C@H]1O[C@@H]1[C@@H](CO)O[C@H](O)[C@H](O)[C@H]1O GUBGYTABKSRVRQ-XLOQQCSPSA-N 0.000 description 1
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 1
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 1
- 239000007995 HEPES buffer Substances 0.000 description 1
- GUBGYTABKSRVRQ-QKKXKWKRSA-N Lactose Natural products OC[C@H]1O[C@@H](O[C@H]2[C@H](O)[C@@H](O)C(O)O[C@@H]2CO)[C@H](O)[C@@H](O)[C@H]1O GUBGYTABKSRVRQ-QKKXKWKRSA-N 0.000 description 1
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 description 1
- 241000519995 Stachys sylvatica Species 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 229940041514 candida albicans extract Drugs 0.000 description 1
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 description 1
- 230000010261 cell growth Effects 0.000 description 1
- 239000006285 cell suspension Substances 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000012937 correction Methods 0.000 description 1
- 238000012258 culturing Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000010894 electron beam technology Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 239000008103 glucose Substances 0.000 description 1
- 230000012010 growth Effects 0.000 description 1
- 239000001963 growth medium Substances 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 229910000037 hydrogen sulfide Inorganic materials 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000011534 incubation Methods 0.000 description 1
- 230000009878 intermolecular interaction Effects 0.000 description 1
- 230000016507 interphase Effects 0.000 description 1
- 229910052741 iridium Inorganic materials 0.000 description 1
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 description 1
- 235000014655 lactic acid Nutrition 0.000 description 1
- 239000004310 lactic acid Substances 0.000 description 1
- 239000008101 lactose Substances 0.000 description 1
- 239000010808 liquid waste Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 235000015097 nutrients Nutrition 0.000 description 1
- 229910052762 osmium Inorganic materials 0.000 description 1
- SYQBFIAQOQZEGI-UHFFFAOYSA-N osmium atom Chemical compound [Os] SYQBFIAQOQZEGI-UHFFFAOYSA-N 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000002285 radioactive effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 229910052703 rhodium Inorganic materials 0.000 description 1
- 239000010948 rhodium Substances 0.000 description 1
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 description 1
- 229910052707 ruthenium Inorganic materials 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 230000002269 spontaneous effect Effects 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000036962 time dependent Effects 0.000 description 1
- 238000009834 vaporization Methods 0.000 description 1
- 230000008016 vaporization Effects 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 239000012138 yeast extract Substances 0.000 description 1
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- Catalysts (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
- Other Surface Treatments For Metallic Materials (AREA)
Description
鉄還元菌としてジオバクター(Geobacter)菌やクロストリジア(Clostridia)菌のように酸素を遮断して培養する嫌気培養装置を必要とする菌ではなく、シェワネラ・ピュートリフェイシャンスのような好気性条件下で培養可能な菌を用いた。ポリペプトン10 g/L、酵母エキス2 g/L、NaCl 5 g/L及びMgSO4・7H2O 5 g/Lを含む培地を好気性培地とし、これをオートクレーブで120℃、20分間滅菌した。好気性培地200 cm3を容量500 cm3の三角フラスコにいれ、オートクレーブで滅菌した。この好気性培地に、鉄還元菌と、滅菌処理した栄養培養液を5 cm3加え、30℃、100 rpmで振とう培養した。細胞の成育が休止期に達したところで、培養液を3000 rpmで10分間遠心分離し、微生物を回収した。回収した微生物を20 mmol/dm3 HEPESおよび100 mmol/dm3 NaClを含む溶液(以下、HEPES-NaCl溶液という)(pH7)にて3回洗浄し、同溶液に懸濁させることにより、微生物細胞懸濁液を調製した。
白金族イオンとして白金酸(H2PtCl6)を用いた。上記HEPES-NaCl溶液とは別に準備したHEPES-NaCl溶液に0.5 mmol/dm3 H2PtCl6(Wako pure chemical Industries, Ltd)を加え、pHを7.0に調整したものを嫌気性培地とした。この嫌気性培地を孔径0.1 μmのフィルターでろ過滅菌し、容量20 cm3の滅菌済みバイアル瓶に10 cm3ずつ加えた。次いで、上記微生物細胞懸濁液を0.2 cm3ずつ加え、バイアル瓶をブチル栓とアルミキャップで密封した。さらに、高純度N2ガスで10分間脱気した後、H2-N2混合ガス(H2:4.8 vol%)でバイアル瓶の気相部を置換し、30℃で恒温培養した。
前記の方法で作製した、白金ナノ粒子が表面に析出した微生物細胞を含む溶液50cm3に珪藻土1gを加え、遠心分離装置で1750rpmで3時間混合振とうした。次に、溶液を孔径0.2μmのフィルターでろ過し、固相を回収した。図4は、濾紙上から回収した物質をSEMで観察撮影した写真である。中央の円柱状のものが担持材料として用いた珪藻土である。また、細長い楕円状のものが白金ナノ粒子を付着させた微生物細胞である。この図4より、Pt(0)粒子が表面に析出した微生物細胞が珪藻土に担持されたことが確認された。
前記の手法で作製した、固定担持材料に付着させた微生物細胞−白金ナノ粒子触媒(以下、触媒とする)をステンレス鋼製触媒カラムに充填した。また、実験装置内の圧力を103 Paに保った。供給したガスは、水素(H2)と重水素(D2)の混合ガスで、その割合(モル比)は、H2:D2= 2:1であった。このH2-D2混合ガスを流量0.1 cm3/min (線速度:3.8×10-2cm3/min)で供給し、触媒カラムを通過させた。触媒カラムから流出したガスの組成分析には、四重極型質量分析器(ANELVA、 M-400QA-M)を用いた。分析では、四重極型質量分析器内の圧力を10-4 Paに保ちながら流出ガスを該四重極型質量分析器へ導入した。そして、触媒カラムを通過した後の流出ガス中の水素・重水素と重水素・重水素の比(HD/D2存在比)を四重極型質量分析器で測定した。触媒作用が発現されれば、水素・重水素からなる水素ガス分子が検出される。なお、平衡を仮定すれば、その比は3.5となる。
Claims (6)
- 好気性条件下で培養した鉄還元菌の微生物細胞表面に白金族元素のナノ粒子を担持した白金族ナノ粒子担持微生物が、無機質担体に担持されていることを特徴とする白金族ナノ粒子担持材料。
- 鉄還元菌が、シュワネラ・ピュートリフェイシャンス(Shewanella putrefaciens)であることを特徴とする請求項1に記載の白金族ナノ粒子担持材料。
- 請求項1または2に記載の白金族ナノ粒子担持材料の製造方法であって、好気性条件下で培養した鉄還元菌の微生物細胞を、嫌気性条件下、電子供給源としての有機酸もしくは水素ガスを共存させた白金族イオン含有液に接触させて微生物細胞の表面に白金族ナノ粒子を析出させ、この白金族ナノ粒子を微生物細胞とともに無機質担体に担持させることを特徴とする白金族ナノ粒子担持材料の製造方法。
- 好気性条件下で培養した鉄還元菌の微生物細胞を、嫌気性条件下、電子供給源としての糖類もしくは水素ガスを共存させた白金族イオン含有液に接触させることにより、鉄還元菌の作用で白金族イオンを還元して微生物細胞の表面に白金族元素のナノ粒子を析出させることを特徴とする白金族ナノ粒子の析出方法。
- 鉄還元菌が、シェワネラ・ピュートリフェイシャンス(Shewanella putrefaciens)であることを特徴とする請求項4に記載の白金族ナノ粒子の析出方法。
- 請求項1または2に記載の白金族ナノ粒子担持材料からなる水素同位体分離用触媒材料。
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CN110577247A (zh) * | 2019-09-04 | 2019-12-17 | 中国石油大学(北京) | 负载有纳米单质铁的复合材料及其制备方法和应用 |
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JP2013005794A (ja) * | 2011-05-26 | 2013-01-10 | Osaka Prefecture Univ | 複合体およびその用途 |
JP6376660B2 (ja) | 2013-01-21 | 2018-08-22 | 三菱ケミカル株式会社 | 金属濃縮方法及び金属回収方法、並びに金属濃縮装置及び金属回収装置 |
JP6404823B2 (ja) * | 2013-10-02 | 2018-10-17 | 公立大学法人大阪府立大学 | 合金ナノ粒子の製造方法 |
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WO2008003522A1 (en) * | 2006-07-05 | 2008-01-10 | Janssen Pharmaceutica N.V. | Method for producing metal nanoparticles |
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CN110577247B (zh) * | 2019-09-04 | 2021-03-26 | 中国石油大学(北京) | 负载有纳米单质铁的复合材料及其制备方法和应用 |
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