JP2007204363A - 複合酸化物担体とその製造方法、低温シフト反応触媒とその製造方法、一酸化炭素の除去方法、燃料処理装置及び燃料電池システム - Google Patents
複合酸化物担体とその製造方法、低温シフト反応触媒とその製造方法、一酸化炭素の除去方法、燃料処理装置及び燃料電池システム Download PDFInfo
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- JP2007204363A JP2007204363A JP2007015362A JP2007015362A JP2007204363A JP 2007204363 A JP2007204363 A JP 2007204363A JP 2007015362 A JP2007015362 A JP 2007015362A JP 2007015362 A JP2007015362 A JP 2007015362A JP 2007204363 A JP2007204363 A JP 2007204363A
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- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
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- FJKROLUGYXJWQN-UHFFFAOYSA-N papa-hydroxy-benzoic acid Natural products OC(=O)C1=CC=C(O)C=C1 FJKROLUGYXJWQN-UHFFFAOYSA-N 0.000 description 1
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- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 1
- ULWHHBHJGPPBCO-UHFFFAOYSA-N propane-1,1-diol Chemical compound CCC(O)O ULWHHBHJGPPBCO-UHFFFAOYSA-N 0.000 description 1
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- 229920002258 tannic acid Polymers 0.000 description 1
- 239000011975 tartaric acid Substances 0.000 description 1
- 235000002906 tartaric acid Nutrition 0.000 description 1
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Abstract
【解決手段】セリアと、M1(Al、ZrまたはTi)の酸化物とを含み、セリウムとM1との原子比が1:4〜1:40である複合酸化物担体、該複合酸化物担体に遷移金属活性成分を初期含浸法を利用して担持させた低温シフト反応触媒、及びこれらの製造方法である。これにより、該複合酸化物担体を利用して製造した低温シフト反応触媒は、従来のWGS反応触媒に比べて一酸化炭素をさらに低い温度でさらに高転換率で除去することができる。
【選択図】図3
Description
アルミナ(Al2O3)前駆体、ジルコニア(ZrO2)前駆体、及びチタニア(TiO2)前駆体から選択された1種以上をアルコール系溶媒と酸溶液との混合物に溶解させて混合酸化物溶液を調製する段階と、前記各段階で製造された各溶液を混合及び加熱してゲル状の混合物を形成する段階と、前記ゲル状の混合物を焼成する段階と、を含む複合酸化物担体の製造方法が提供される。
(複合酸化物担体の製造)
Ce(NO3)3・6H2O 7.1gをエチレングリコール40.7g及びクエン酸34.4gの混合溶液に溶解させた。前記混合溶液(E1A溶液)とは別途に、Al(NO3)3・9H2O 24.6gをエチレングリコール162.8g及びクエン酸137.8gの混合溶液に溶解させた(E1B溶液)。
白金前駆体であるPt(NH3)4(NO3)2 0.405gを水5mlに溶解させた後、前記複合酸化物担体10gに一滴ずつ滴下しつつ混合した。滴下が完了した後、110℃のオーブンで16時間乾燥させ、その後に500℃で空気雰囲気のオーブンで4時間焼成して担持触媒を得た。
(複合酸化物担体の製造)
Ce(NO3)3・6H2O 4.0gをエチレングリコール23.0g及びクエン酸19.5gの混合溶液に溶解させた。前記混合溶液(E2A溶液)とは別途に、Al(NO3)3・9H2O 31.3gをエチレングリコール207.2g及びクエン酸175.38gの混合溶液に溶解させた(E2B溶液)。
白金前駆体であるPt(NH3)4(NO3)2 0.405gを水5mlに溶解させた後、前記複合酸化物担体10gに一滴ずつ滴下しつつ混合した。滴下が完了した後、110℃のオーブンで16時間乾燥させ、その後に500℃で空気雰囲気のオーブンで4時間焼成して担持触媒を得た。
(担体の製造)
水111.6gに商用γ−Al2O3(Aldrich社製)11.5gを入れて60℃に加熱した。ここにCe(NO3)3・6H2O 10.86gを入れて均一になるように約6時間混合した。前記混合溶液を70℃の温度に加熱しつつ減圧して水を除去した。その後、110℃のオーブンで16時間乾燥させ、500℃のオーブンで空気雰囲気で4時間焼成させた。セリウム:アルミニウムの原子比は1:9であった。
白金前駆体であるPt(NH3)4(NO3)2 0.405gを水100mlに溶解させた後、製造した担体10gを入れて混合した。温度を60℃に維持しながら6時間混合して均一にした。その後、前記混合溶液を70℃の温度に加熱しつつ減圧して水を除去した。その後、110℃のオーブンで16時間乾燥させ、500℃のオーブンで空気雰囲気で4時間焼成させた。
(担体の製造)
水217gに商用γ−Al2O3(Aldrich社製)20.4gを入れて60℃に加熱した。ここにCe(NO3)3・6H2O 43.4gを入れて均一になるように約6時間混合した。前記混合溶液を70℃の温度に加熱しつつ減圧して水を除去した。その後、110℃のオーブンで16時間乾燥させ、500℃のオーブンで空気雰囲気で4時間焼成させた。セリウム:アルミニウムの原子比は2:8であった。
前記で製造した担体を利用する点を除いては、比較例1と同じ方法で担持触媒を製造した。
白金前駆体であるPt(NH3)4(NO3)2 0.405gを水5mlに溶解させた後、前記比較例2で製造した担体10gに一滴ずつ滴下しつつ混合した。滴下が完了した後、110℃のオーブンで16時間乾燥させ、その後に500℃で空気雰囲気のオーブンで4時間焼成して担持触媒を得た。
商用担体であるγ−Al2O3(Aldrich社製)を使用した点を除いては、実施例1と同じ方法で担持触媒を製造した。
商用担体であるCeO2(Aldrich社製)を使用した点を除いては、実施例1と同じ方法で担持触媒を製造した。
白金前駆体であるPt(NH3)4(NO3)2 0.397と、セリウム前駆体であるCe(NO3)3・6H2O 2.53gとを水30gに溶解させた後、商用γ−Al2O3(Aldrich社製)10gを入れ、60℃に加熱しつつ1時間撹拌して均一に混合した。その後、1M濃度のNaOH水溶液をpHが9となるまで滴下した。約1時間撹拌してさらに混合した後、混合溶液をろ過及び洗浄して乾燥させた。その後、再び110℃のオーブンで約16時間乾燥させた後に、空気雰囲気のオーブンで500℃で4時間焼成した。
商用γ−Al2O3(Aldrich社製)10gを水25gに入れて60℃に加熱した。ここにCe(NO3)3・6H2O 2.53gをよく溶かした後、約1時間混合した後、1M濃度のNaOH水溶液をpHが9となるまで滴下した。約1時間撹拌してさらに混合した後、混合溶液をろ過及び洗浄して乾燥させた。その後、再び110℃のオーブンで約16時間乾燥させた後に、空気雰囲気のオーブンで500℃で4時間焼成した。その後、白金前駆体であるPt(NH3)4(NO3)2 0.405gを水5mlに溶解させた後、製造した担体10gに一滴ずつ滴下しつつ混合した。滴下が完了した後、110℃のオーブンで16時間乾燥させ、その後500℃で空気雰囲気のオーブンで4時間焼成して担持触媒を得た。
Claims (32)
- セリア(CeO2)と、
M1(M1は、アルミニウム(Al)、ジルコニウム(Zr)、及びチタン(Ti)から選択される1種以上の金属)の酸化物と、
を含み、
前記セリア中のセリウム(Ce)とM1との原子比が1:4〜1:40であることを特徴とする、複合酸化物担体。 - 前記複合酸化物担体の全体質量に対する前記セリアの質量含量が、3質量%〜20質量%であることを特徴とする、請求項1に記載の複合酸化物担体。
- 前記M1の酸化物が、アルミナ(Al2O3)であることを特徴とする、請求項1に記載の複合酸化物担体。
- 前記複合酸化物担体の表面積が、10m2/g〜1500m2/gであることを特徴とする、請求項1に記載の複合酸化物担体。
- セリア(CeO2)前駆体をアルコール系溶媒と酸溶液との混合物に溶解させてセリア溶液を調製する段階と、
アルミナ(Al2O3)前駆体、ジルコニア(ZrO2)前駆体、及びチタニア(TiO2)前駆体から選択された1種以上をアルコール系溶媒と酸溶液との混合物に溶解させて混合酸化物溶液を調製する段階と、
前記各段階で製造された各溶液を混合及び加熱してゲル状の混合物を形成する段階と、
前記ゲル状の混合物を焼成する段階と、
を含むことを特徴とする、複合酸化物担体の製造方法。 - 前記セリア前駆体が、Ce(NO3)3・6H2O、Ce(CH3CO2)3、Ce(CO3)3、CeCl3、(NH4)2Ce(NO3)6、(NH4)2Ce(SO4)4、Ce(OH)4、Ce2(C2O4)3、Ce(ClO4)3、またはCe2(SO4)3のうちから選択される1種以上であり、
前記アルミナ前駆体が、Al(NO3)3・9H2O、AlCl3、Al(OH)3、AlNH4(SO4)2・12H2O、Al((CH3)2CHO)3、Al(CH3CH(OH)CO2)2、Al(ClO4)3・9H2O、Al(C6H5O)3、Al2(SO4)3・18H2O、Al(CH3(CH2)3O)3、Al(C2H5CH(CH3)O)3Al、またはAl(C2H5O)3のうちから選択される1種以上であり、
前記ジルコニア前駆体が、ZrO(NO3)2、ZrCl4、Zr(OC(CH3)3)4、Zr(O(CH2)3CH3)4、(CH3CO2)Zr(OH)、ZrOCl2、Zr(SO4)2、またはZr(OCH2CH2CH3)4のうちから選択される1種以上であり、
前記チタニア前駆体が、Ti(NO3)4、TiOSO4、Ti(OCH2CH2CH3)4、Ti(OCH(CH3)2)4、Ti(OC2H5)4、Ti(OCH3)4、TiCl3、Ti(O(CH2)3CH3)4、またはTi(OC(CH3)3)4のうちから選択される1種以上であることを特徴とする、請求項5に記載の複合酸化物担体の製造方法。 - 前記焼成が、400℃〜700℃で行われることを特徴とする、請求項5に記載の複合酸化物担体の製造方法。
- 前記セリア溶液において、セリア前駆体と、酸溶液と、アルコール系溶媒との質量比が、1:2:10〜1:20:80であることを特徴とする、請求項5に記載の複合酸化物担体の製造方法。
- 前記混合酸化物溶液において、アルミナ前駆体、ジルコニア前駆体、及びチタニア前駆体から選択された1種以上と、酸溶液と、アルコール系溶媒との質量比が、1:2:10〜1:20:80であることを特徴とする、請求項5に記載の複合酸化物担体の製造方法。
- 前記アルコール系溶媒は、炭素数1〜10の1価アルコールまたは炭素数1〜10の2価アルコールであることを特徴とする、請求項5に記載の複合酸化物担体の製造方法。
- 前記セリア溶液及び前記混合酸化物溶液を混合及び加熱してゲル状の混合物を形成する段階が、100℃〜200℃で行われることを特徴とする、請求項5に記載の複合酸化物担体の製造方法。
- 前記セリア前駆体中のセリウムと、アルミナ前駆体、ジルコニア前駆体、及びチタニア前駆体から選択された1種以上の前駆体中の金属成分との原子比が、1:4〜1:40であることを特徴とする、請求項5に記載の複合酸化物担体の製造方法。
- (a)セリア(CeO2)と、M1(M1は、アルミニウム(Al)、ジルコニウム(Zr)、及びチタン(Ti)から選択される1種以上の金属)の酸化物とを含み、前記セリア中のセリウム(Ce)とM1との原子比が1:4〜1:40である複合酸化物担体と、
(b)前記複合酸化物担体に担持された遷移金属活性成分と、
を含むことを特徴とする、低温シフト反応触媒。 - 前記遷移金属活性成分の含量が、前記低温シフト反応触媒の全体質量に対して1質量%〜10質量%であることを特徴とする、請求項13に記載の低温シフト反応触媒。
- 前記遷移金属活性成分の分散度が60%以上であることを特徴とする、請求項13に記載の低温シフト反応触媒。
- 前記遷移金属活性成分が、白金(Pt)、または、パラジウム(Pd)、ニッケル(Ni)、コバルト(Co)、ルテニウム(Ru)、レニウム(Re)、ロジウム(Rh)、オシウム(Os)、チタン(Ti)、バナジウム(V)、クロム(Cr)、マンガン(Mn)、鉄(Fe)、銅(Cu)、セリウム(Ce)もしくは亜鉛(Zn)と白金との合金であることを特徴とする、請求項13に記載の低温シフト反応触媒。
- 前記複合酸化物担体の全体質量に対する前記セリアの質量含量が、3質量%〜20質量%であることを特徴とする、請求項13に記載の低温シフト反応触媒。
- 前記M1の酸化物が、アルミナ(Al2O3)であることを特徴とする、請求項13に記載の低温シフト反応触媒。
- 前記複合酸化物担体の表面積が、10m2/g〜1500m2/gであることを特徴とする、請求項13に記載の低温シフト反応触媒。
- セリア(CeO2)前駆体をアルコール系溶媒と酸溶液との混合物に溶解させてセリア溶液を調製する段階と、
アルミナ(Al2O3)前駆体、ジルコニア(ZrO2)前駆体、及びチタニア(TiO2)前駆体から選択された1種以上をアルコール系溶媒と酸溶液との混合物に溶解させて混合酸化物溶液を調製する段階と、
前記各段階で製造された各溶液を混合及び加熱してゲル状の混合物を形成する段階と、
前記ゲル状の混合物を焼成して複合酸化物担体を製造する段階と、
前記複合酸化物担体に初期含浸法を利用して、遷移金属活性成分を含浸させる段階と、
前記含浸された結果物を焼成する段階と、
を含むことを特徴とする、低温シフト反応触媒の製造方法。 - 前記含浸された結果物の焼成が、300℃〜700℃の温度で行われることを特徴とする、請求項20に記載の低温シフト反応触媒の製造方法。
- 前記セリア前駆体が、Ce(NO3)3・6H2O、Ce(CH3CO2)3、Ce(CO3)3、CeCl3、(NH4)2Ce(NO3)6、(NH4)2Ce(SO4)4、Ce(OH)4、Ce2(C2O4)3、Ce(ClO4)3、またはCe2(SO4)3のうちから選択される1種以上であり、
前記アルミナ前駆体が、Al(NO3)3・9H2O、AlCl3、Al(OH)3、AlNH4(SO4)2・12H2O、Al((CH3)2CHO)3、Al(CH3CH(OH)CO2)2、Al(ClO4)3・9H2O、Al(C6H5O)3、Al2(SO4)3・18H2O、Al(CH3(CH2)3O)3、Al(C2H5CH(CH3)O)3Al、またはAl(C2H5O)3のうちから選択される1種以上であり、
前記ジルコニア前駆体が、ZrO(NO3)2、ZrCl4、Zr(OC(CH3)3)4、Zr(O(CH2)3CH3)4、(CH3CO2)Zr(OH)、ZrOCl2、Zr(SO4)2、またはZr(OCH2CH2CH3)4のうちから選択される1種以上であり、
前記チタニア前駆体が、Ti(NO3)4、TiOSO4、Ti(OCH2CH2CH3)4、Ti(OCH(CH3)2)4、Ti(OC2H5)4、Ti(OCH3)4、TiCl3、Ti(O(CH2)3CH3)4、またはTi(OC(CH3)3)4のうちから選択される1種以上であることを特徴とする、請求項20に記載の低温シフト反応触媒の製造方法。 - 前記ゲル状の混合物の焼成が、400℃〜700℃で行われることを特徴とする、請求項20に記載の低温シフト反応触媒の製造方法。
- 前記セリア溶液において、セリア前駆体、酸溶液及びアルコール系溶媒の質量比が1:2:10〜1:20:80であることを特徴とする、請求項20に記載の低温シフト反応触媒の製造方法。
- 前記混合酸化物溶液において、アルミナ前駆体、ジルコニア前駆体、及びチタニア前駆体から選択された1種以上と、酸溶液と、アルコール系溶媒との質量比が、1:2:10〜1:20:80であることを特徴とする、請求項20に記載の低温シフト反応触媒の製造方法。
- 前記アルコール系溶媒が、炭素数1〜10の1価アルコールまたは炭素数1〜10の2価アルコールであることを特徴とする、請求項20に記載の低温シフト反応触媒の製造方法。
- 前記セリア溶液及び前記混合酸化物溶液を混合及び加熱してゲル状の混合物を形成する段階が、100℃〜200℃で行われることを特徴とする、請求項20に記載の低温シフト反応触媒の製造方法。
- 前記セリア前駆体中のセリウムと、アルミナ前駆体、ジルコニア前駆体、及びチタニア前駆体から選択された1種以上の前駆体中の金属成分との原子比が、1:4〜1:40であることを特徴とする、請求項20に記載の低温シフト反応触媒の製造方法。
- 請求項13〜請求項19のうちいずれか一項に記載の低温シフト反応触媒を、一酸化炭素を含む気体と接触させる段階を含むことを特徴とする、一酸化炭素の除去方法。
- 前記接触が、200℃〜280℃の温度で行われることを特徴とする、請求項29に記載の一酸化炭素の除去方法。
- 請求項1〜請求項4のうちいずれか一項に記載の複合酸化物担体を含む、燃料処理装置。
- 請求項1〜請求項4のうちいずれか一項に記載の複合酸化物担体を含む、燃料電池システム。
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JP2002542015A (ja) * | 1999-04-19 | 2002-12-10 | エンゲルハード・コーポレーシヨン | セリアと白金族金属を含んで成る触媒組成物 |
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- 2006-12-06 US US11/634,108 patent/US20070179053A1/en not_active Abandoned
- 2006-12-19 CN CN200610171738XA patent/CN101204672B/zh not_active Expired - Fee Related
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JP2009117365A (ja) * | 2007-11-07 | 2009-05-28 | Korea Inst Of Science & Technology | 電極活物質の製造方法及びその方法で製造された電極活物質を含むリチウム電池 |
JP2010064036A (ja) * | 2008-09-12 | 2010-03-25 | Japan Energy Corp | 低い温度での水素製造に適した水素製造用改質触媒、及び該触媒を用いた水素製造方法 |
JP2011083685A (ja) * | 2009-10-14 | 2011-04-28 | Jx Nippon Oil & Energy Corp | 水素製造用改質触媒及びその製造方法、並びに該触媒を用いた水素製造方法 |
JP2011167595A (ja) * | 2010-02-16 | 2011-09-01 | Jx Nippon Oil & Energy Corp | 水素製造用改質触媒及びその製造方法、並びに該触媒を用いた水素製造方法 |
WO2019131176A1 (ja) * | 2017-12-28 | 2019-07-04 | ユミコア日本触媒株式会社 | 水素製造用触媒及びこれを用いた排ガス浄化用触媒 |
JP6544880B1 (ja) * | 2017-12-28 | 2019-07-17 | ユミコア日本触媒株式会社 | 水素製造用触媒及びこれを用いた排ガス浄化用触媒 |
US11446638B2 (en) | 2017-12-28 | 2022-09-20 | Umicore Shokubai Japan Co., Ltd | Hydrogen-producing catalyst and exhaust gas purifying catalyst using same |
Also Published As
Publication number | Publication date |
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US20070179053A1 (en) | 2007-08-02 |
CN101204672A (zh) | 2008-06-25 |
JP4662955B2 (ja) | 2011-03-30 |
CN101204672B (zh) | 2012-05-23 |
KR100723392B1 (ko) | 2007-05-30 |
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