JP2009515680A - 極薄触媒酸化塗膜を有するディーゼル粉塵フィルター - Google Patents
極薄触媒酸化塗膜を有するディーゼル粉塵フィルター Download PDFInfo
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- JP2009515680A JP2009515680A JP2008540175A JP2008540175A JP2009515680A JP 2009515680 A JP2009515680 A JP 2009515680A JP 2008540175 A JP2008540175 A JP 2008540175A JP 2008540175 A JP2008540175 A JP 2008540175A JP 2009515680 A JP2009515680 A JP 2009515680A
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- exhaust gas
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- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 description 1
- 150000002926 oxygen Chemical class 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- MMKQUGHLEMYQSG-UHFFFAOYSA-N oxygen(2-);praseodymium(3+) Chemical compound [O-2].[O-2].[O-2].[Pr+3].[Pr+3] MMKQUGHLEMYQSG-UHFFFAOYSA-N 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- PIBWKRNGBLPSSY-UHFFFAOYSA-L palladium(II) chloride Chemical compound Cl[Pd]Cl PIBWKRNGBLPSSY-UHFFFAOYSA-L 0.000 description 1
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- 230000035515 penetration Effects 0.000 description 1
- 229910052670 petalite Inorganic materials 0.000 description 1
- 238000007750 plasma spraying Methods 0.000 description 1
- NFOHLBHARAZXFQ-UHFFFAOYSA-L platinum(2+);dihydroxide Chemical compound O[Pt]O NFOHLBHARAZXFQ-UHFFFAOYSA-L 0.000 description 1
- 125000005575 polycyclic aromatic hydrocarbon group Chemical group 0.000 description 1
- 229910003447 praseodymium oxide Inorganic materials 0.000 description 1
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- 238000001556 precipitation Methods 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 230000001172 regenerating effect Effects 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 230000000241 respiratory effect Effects 0.000 description 1
- 210000002345 respiratory system Anatomy 0.000 description 1
- 229910052707 ruthenium Inorganic materials 0.000 description 1
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- 238000000926 separation method Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- RAVDHKVWJUPFPT-UHFFFAOYSA-N silver;oxido(dioxo)vanadium Chemical compound [Ag+].[O-][V](=O)=O RAVDHKVWJUPFPT-UHFFFAOYSA-N 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
- 239000006104 solid solution Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 239000011975 tartaric acid Substances 0.000 description 1
- 235000002906 tartaric acid Nutrition 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 229910000314 transition metal oxide Inorganic materials 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- GPPXJZIENCGNKB-UHFFFAOYSA-N vanadium Chemical compound [V]#[V] GPPXJZIENCGNKB-UHFFFAOYSA-N 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 1
- 150000003754 zirconium Chemical class 0.000 description 1
- 229910052726 zirconium Chemical class 0.000 description 1
- DUNKXUFBGCUVQW-UHFFFAOYSA-J zirconium tetrachloride Chemical class Cl[Zr](Cl)(Cl)Cl DUNKXUFBGCUVQW-UHFFFAOYSA-J 0.000 description 1
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Abstract
【選択図】なし
Description
図2は、本発明の一実施様態における壁流型のモノリス流通セルの縦断面図である;
図3は、サブミクロン粒子を含む触媒極極塗膜の塗布の有無での壁流型の基板での圧力損失の比較を示すものである;
図4は、サブミクロンの被覆フィルター基板の走査型電子顕微鏡写真を示す;
図5は、各種の触媒極薄塗膜で被覆された壁流型の基板による、いろいろな温度での一酸化炭素の変換を比較したものを示す;
図6は、各種の触媒極薄塗膜で被覆された壁流型の基板による、いろいろな温度での一酸化炭素の変換を比較したものを示す;
図7は、各種の触媒極薄塗膜で被覆された壁流型の基板による、いろいろな温度での一酸化炭素の変換を比較したものを示す。
実施例1−試料Aの調整
直径1インチ×長さ3インチの長尺SiC製壁流型基板(58%空孔率、300セル/平方インチ、厚さ:12mil)を薄膜被覆して、試料Aを調整した。この壁流型基板を、90g/ft3のPt、0.6g/in3のシラロックス(R)Si/Al(約1.5%シリカ、98.5%アルミナ、サソルノースアメリカ製、米国)、0.3g/in3のサブミクロンCe/Zr複合物(約30%CeO2、平均結晶径:<0.5マイクロメータ、市販品)、及び0.05g/in3のZrO2を含む薄膜スラリーで被覆した。このSi/Al担体に、所望量のPtアミン塩を含浸させた。次いで、Pt/Si/Al粉末を粉砕して、90%の粒子の径が5マイクロメータ未満となるまで粒度を下げた。この粉砕の段階で、Ce/Zr複合物を添加した。この粉砕の段階で、追加のZr成分を酢酸ジルコニルゾルの形で、バインダーとして添加した。得られたスラリーのpHを酢酸で調整して、3.5〜4.5とした。極薄塗膜は、基板をスラリーに浸漬して塗布した。過剰のスラリーは、空気ナイフを用いてモノリスから吹き飛ばした。試料を、110℃で2時間乾燥し、次いで450℃の空気中のオーブンで1時間焼成した。次いで、試料Aを、空気と水蒸気のガス流中で700℃で4時間、熱的に養生させた。
直径1インチ×長さ3インチの長尺SiC製壁流型基板(58%空孔率、300セル/平方インチ、厚さ:12mil)を薄膜被覆して、試料Bを調整した。この壁流型の基板を、90g/ft3のPt、0.6g/in3のサブミクロンアルミナ(市販品)、0.3g/in3のサブミクロンCe/Zr複合物(約30%CeO2、平均結晶径:<0.5 マイクロメータ、市販品)、及び0.05g/in3のZrO2を含む薄膜スラリーで被覆した。このサブミクロンアルミナは、メーカー作成の水分散液であり、平均粒度は40ナノメーターであった。この薄膜スラリーは貴金属を含まず、極薄塗膜は、基板をスラリーに浸漬して塗布した。過剰のスラリーは空気ナイフを用いて吹き飛ばした。試料を、110℃で2時間乾燥し、次いで450℃の空気中のオーブンで1時間焼成した。得られた試料を次いで、Ptアミン塩溶液に浸漬し、必要量のPtを吸収させた。この試料を、再び450℃で1時間焼成した。次いで、試料Bを、空気と水蒸気のガス流中で700℃で4時間、熱的に養生させた。
直径1インチ×長さ3インチの長尺SiC製壁流型基板(58%空孔率、300セル/平方インチ、厚さ:12mil)を薄膜被覆して、試料Cを調整した。この壁流型の基板を、90g/ft33のPt、0.6g/in3のシラロックス(R)Si/Al(約1.5%シリカ、98.5%アルミナ、サソルノースアメリカ社製、米国)、0.3g/in3のサブミクロンアルミナ(市販品)、0.3g/in3のCe/Zr複合物(約30%CeO2、平均結晶径:約5マイクロメータs、市販品)と、0.05g/in3のZrO2を含む薄膜スラリーで被覆した。このサブミクロンアルミナは、メーカー作成の水分散液であり、単独でプレコートとして基板上に塗布した。このサブミクロンアルミナは次いで、450℃で1時間焼成した。第二のスラリーは、次のように調整した。Ptアミン塩をシラロックス(R)担体に含浸させ、所望の吸着量とした。次いで、Pt/シラロックス(R)Si/Al粉末を粉砕して、90%の粒子の径が5マイクロメータ未満となるまで粒度を下げた。この粉砕の段階で、Ce/Zr複合物を添加した。この粉砕の段階で、追加のZr成分を酢酸ジルコニルゾルの形で、バインダーとして添加した。得られたスラリーのpHを酢酸で調整して、3.5〜4.5とした。極薄塗膜は、基板をスラリーに浸漬して塗布した。過剰のスラリーは空気ナイフを用いて吹き飛ばした。試料を、110℃で2時間乾燥し、次いで450℃の空気中のオーブンで1時間焼成した。次いで、試料Cを、空気と水蒸気のガス流中で700℃で4時間、熱的に養生させた。
直径1インチ×長さ3インチの長尺SiC製壁流型基板(58%空孔率、300セル/平方インチ、厚さ:12mil)を薄膜被覆して、試料Dを調整した。この壁流型の基板を、90g/ft3のPt、0.6g/in3のサブミクロンアルミナ(市販品)、0.3g/in3のサブミクロンサイズのCeO2 (平均粒度:11ナノメーター、市販品)及び0.05g/in3のZrO2を含む薄膜スラリーで被覆した。このサブミクロンアルミナは、メーカー作成の水分散液であり、平均粒度は40ナノメーターであった。この薄膜スラリーは貴金属を含まず、極薄塗膜は、基板をスラリーに浸漬して塗布した。過剰のスラリーは空気ナイフを用いて吹き飛ばした。試料を、110℃で2時間乾燥し、次いで450℃の空気中のオーブンで1時間焼成した。得られた試料を次いで、Ptアミン塩溶液に浸漬し、必要量のPtを吸収させた。この試料を、再び450℃で1時間焼成した。次いで、試料Dを、空気と水蒸気のガス流中で700℃で4時間、熱的に養生させた。
直径1インチ×長さ3インチの長尺SiC製壁流型基板(58%空孔率、300セル/平方インチ、厚さ:12mil)を薄膜被覆して、試料Eを調整した。この壁流型の基板は、90g/ft3のPt、0.6g/in3のシラロックス(R)Si/Al (約1.5%シリカ、98.5%アルミナ、サソルノースアメリカ社製、米国)、0.3g/in3のサブミクロンCe/Zr複合物(約0% CeO2、平均結晶径:<0.5マイクロメータ、市販品)及び0.05g/in3 ZrO2を含む薄膜スラリーで被覆した。Ptアミン塩をシラロックス(R)担体に含浸させ、所望の吸着量とした。次いで、Pt/シラロックス(R)Si/Al粉末を粉砕して、90%の粒子の径が5マイクロメータ未満となるまで粒度を下げた。この粉砕の段階で、Ce/Zr複合物を添加した。この粉砕の段階で、追加のZr成分を酢酸ジルコニルゾルの形で、バインダーとして添加した。得られたスラリーのpHを酢酸で調整して、3.5〜4.5とした。極薄塗膜は、基板をスラリーに浸漬して塗布した。過剰のスラリーは空気ナイフを用いて吹き飛ばした。試料を、110℃で2時間乾燥し、次いで450℃の空気中のオーブンで1時間焼成した。次いで、試料Eを、空気と水蒸気のガス流中で700℃で4時間、熱的に養生させた。
直径1インチ×長さ3インチの長尺SiC製壁流型基板(58%空孔率、300セル/平方インチ、厚さ:12mil)を薄膜被覆して、試料Fを調整した。この壁流型の基板を。90g/ft3のPt、0.6g/in3のサブミクロンアルミナ(市販品)、0.3g/in3のサブミクロンサイズのCeO2 (平均の粒度:11ナノメーター、市販品)及び0.05g/in3のZrO2 を含む薄膜スラリーで被覆した。このサブミクロンアルミナは、メーカー作成の水分散液であり、平均粒度は40ナノメーターであった。この薄膜スラリーは、異なるスラリー成分を混合して作った。ついで、Ptアミン塩をスラリーに滴下して、Ptを固体状担体上に析出させた。極薄塗膜は、基板をスラリーに浸漬して塗布した。過剰のスラリーは空気ナイフを用いて吹き飛ばした。試料を、110℃で2時間乾燥し、次いで450℃の空気中のオーブンで1時間焼成した。次いで、試料Fを、空気と水蒸気のガス流中で700℃で4時間、熱的に養生させた。
直径1インチ×長さ3インチの長尺SiC製壁流型基板(58%空孔率、300セル/平方インチ、厚さ:12mil)を薄膜被覆して、試料Gを調整した。この壁流型の基板を、90 g/ft3のPt、0.6g/in3のサブミクロンアルミナ(市販品)、0.3g/in3のサブミクロンCe/Zr複合物(約30% CeO2、平均結晶径:<0.5マイクロメータ、市販品)及び0.05g/in3のZrO2を含む薄膜スラリーで被覆した。Ptアミン塩をサブミクロンアルミナに含浸させ、所望の吸着量とした。次いで、Pt/アルミナ粉末を粉砕して凝集物をつぶし、90%の粒子の径が5マイクロメータ未満となるまで粒度を下げた。この粉砕の段階で、Ce/Zr複合物を添加した。この粉砕の段階で、追加のZr成分を酢酸ジルコニルゾルの形で、バインダーとして添加した。得られたスラリーのpHを酢酸で調整して、3.5〜4.5とした。極薄塗膜は、基板をスラリーに浸漬して塗布した。過剰のスラリーは空気ナイフを用いて吹き飛ばした。試料は、110℃で2時間乾燥し、次いで空気中450℃の炉中で1時間焼成した。試料Gは、空気と水蒸気のガス流中で700℃で4時間、熱的に養生させた。
直径1インチ×長さ3インチの長尺SiC製壁流型基板(58%空孔率、300セル/平方インチ、厚さ:12mil)を薄膜被覆して、試料Hを調整した。この壁流型の基板を、90g/ft3のPt 0.9g/in3のサブミクロンアルミナ(粉末、平均結晶粒径:40ナノメーター、市販品)及び0.05g/in3のZrO2 を含む薄膜スラリーで被覆した。Ptアミン塩をサブミクロンアルミナに含浸させ、所望の吸着量とした。次いで、Pt/アルミナ粉末を粉砕して凝集物をつぶし、90%の粒子の径が5マイクロメータ未満となるまで粒度を下げた。この粉砕の段階で、Ce/Zr複合物を添加した。この粉砕の段階で、追加のZr成分を酢酸ジルコニルゾルの形で、バインダーとして添加した。得られたスラリーのpHを酢酸で調整して、3.5〜4.5とした。極薄塗膜は、基板をスラリーに浸漬して塗布した。過剰のスラリーは空気ナイフを用いて吹き飛ばした。試料を、110℃で2時間乾燥し、次いで450℃の空気中のオーブンで1時間焼成した。次いで、試料Hを、空気と水蒸気のガス流中で700℃で4時間、熱的に養生させた。
直径1.5インチ×長さ3インチの長尺のアルミニウムチタネート製壁流型基板(51%空孔率、300セル/平方インチ、厚さ:13mil)を薄膜被覆して、試料I〜試料Lを調整した。この壁流型の基板を、90g/ft3のPt、0.7g/in3のシラロックス(R)Si/Al(約1.5%シリカ、98.5%アルミナ、サソルノースアメリカ社製、米国)、及び0.035g/in3のZrO2を含む薄膜スラリーで被覆した。Ptアミン塩をシラロックス(R)担体に含浸させ、所望の吸着量とした。次いで、Pt/シラロックス(R)Si/Al粉末を粉砕して、粒度を下げた。最終的な粒度は、試料I、J、K及びLにおいて90%の粒子が、それぞれ2.0、5.5、3.6、8.5マイクロメータ未満となるようにした。この粉砕の段階で、Zr成分を酢酸ジルコニルゾルの形で、バインダーとして添加した。得られたスラリーのpHを酢酸で調整して、3.5〜4.5とした。極薄塗膜は、基板をスラリーに浸漬して塗布した。 過剰のスラリーは空気ナイフを用いて吹き飛ばした。試料を、110℃で2時間乾燥し、次いで450℃の空気中のオーブンで1時間焼成した。次いで、試料を、空気と水蒸気のガス流中で700℃で4時間、次いで空気と水蒸気のガス流中で800℃ 4時間、熱的に養生させた。
直径1.5インチ×長さ3インチの長尺のアルミニウムチタネート製壁流型基板(51%空孔率、300セル/平方インチ、厚さ:13mil)を薄膜被覆して、試料Mと試料Nを調整した。壁流型基板を、90g/ft3 Pt、0.7g/in3のサブミクロンアルミナ(粉末、平均結晶粒径:40ナノメーターs、市販品)及び0.035g/in3のZrO2を含む薄膜スラリーで被覆した。Ptアミン塩を、このアルミナ粉末に含浸させ、所望の吸着量とした。このPt/アルミナ粉末は、次いで粉砕して、凝集体をつぶした。最終の粒度は、試料MとNにおいて90%が、それぞれ5.5と4.7マイクロメータ未満である。この粉砕の段階で、Zr成分を酢酸ジルコニルゾルの形で、バインダーとして添加した。得られたスラリーのpHを酢酸で調整して、3.5〜4.5とした。極薄塗膜は、基板をスラリーに浸漬して塗布した。過剰のスラリーは空気ナイフを用いて吹き飛ばした。試料を、110℃で2時間乾燥し、次いで450℃の空気中のオーブンで1時間焼成した。次いで、試料を、空気と水蒸気のガス流中で700℃で4時間、次いで空気と水蒸気のガス流中で800℃ 4時間、熱的に養生させた。
試料Eと試料Gを、上述のように調整した。被覆壁流基板と非被覆壁流基板の圧力変化を測定した。図3に、極薄塗膜の形成前後での基板の圧力損失を示す。サブミクロン薄膜スラリー(試料G)を被覆した基板は、塗膜形成前の基板と比較して、圧損上昇は大きくはない。一方、従来のスラリー(試料E)を被覆した基板は、かなり大きな圧力損失を示した。
試料A〜試料Hを、上述のように調整した。
試料は、1000ppmのCO、167ppmのプロペン、10%のO2、10%の水を含むガスを供給しながら、流通反応系で試験した。この系には、COとHC、CO2の測定機が備わっており、これらを用いて触媒の変換効率を測定した。まず、触媒を90℃で供給ガスで飽和させる。90℃で安定化させた後、20℃/分で300℃まで温度を上げた。反応物と生成物の濃度を連続的に測定し、記録した。いろいろな時間でのCOまたはHCの変換率を、供給濃度(触媒通過前)と排出濃度(触媒通過後)間の相対差として計算した。
試料I〜試料Nを、前述の方法により調整した。
試料は、1000ppmのCO、167ppmのプロペン、10%のO2、10%の水を含むガスを供給しながら、流通反応系で試験した。この系には、COとHC、CO2の測定機が備わっており、これらを用いて触媒の変換効率を測定した。まず、触媒を90℃で供給ガスで飽和させる。90℃で安定化させた後、20℃/分で300℃まで温度を上げた。反応物と生成物の濃度を連続的に測定し、記録した。いろいろな時間でのCOまたはHCの変換率を、供給濃度(触媒通過前)と排出濃度(触媒通過後)間の相対差として計算した。
試料I〜試料Nを、上述のように調整した。
Claims (12)
- すすフィルターを有するディーゼルエンジン用排ガス処理システムであって、サブミクロン粒子を含む一種以上の極薄塗膜組成物がすすフィルター上に分散していることを特徴とする排ガス処理システム。
- 上記サブミクロン粒子の大きさが約0.01〜約0.5ミクロンの範囲にある請求項1に記載の排ガス処理システム。
- 上記サブミクロン粒子が、アルミナ酸化物、ジルコニア酸化物、酸化チタン、酸化マグネシウム、酸化ハフニウム、酸化ランタン、酸化イットリウム、酸化ケイ素、これらの混合物及び白金族金属を含む上記の塩基性金属酸化物からなる群から選ばれる一種以上の塩基性金属酸化物のサブミクロン粒子である請求項1に記載の排ガス処理システム。
- 上記サブミクロン粒子が、サブミクロンの、アルミナ、シリカ−アルミナ、または白金族金属を含む前記アルミナまたはシリカ−アルミナである請求項1に記載の排ガス処理システム。
- 上記サブミクロン粒子が、共形成サブミクロンセリア−ジルコニア複合物である請求項1に記載の排ガス処理システム。
- 上記極薄塗膜組成物が、更に一種以上のゼオライトを含む請求項1に記載の排ガス処理システム。
- 上記すすフィルターが、一種以上の上記極薄塗膜組成物で被覆された壁流型モノリスである請求項1に記載の排ガス処理システム。
- 上記壁流型のモノリスの空隙率が約40%〜約75%である請求項1に記載の排ガス処理システム。
- 上記極薄塗膜組成物が、さらに白金族金属を含み、前記白金が上記すすフィルターに0.01〜200g/ft3の量で含まれている請求項1に記載の排ガス処理システム。
- 上記白金金属基が、上記すすフィルターの上流領域及び下流領域のそれぞれに異なる濃度で局所的に被覆されている請求項1に記載の排ガス処理システム。
- 上記すすフィルターが、上記サブミクロン極薄塗膜組成物の少なくとも2層で積層被覆されている請求項1に記載の排ガス処理システム。
- ディーゼルエンジンの排ガス流を処理する方法であって、請求項1〜11のいずれか1項のすすフィルターを有するディーゼルエンジン用排ガス処理システムに記載されたサブミクロン粒子を含む一種以上の極薄塗膜組成物が分散しているすすフィルターを含む排ガス処理システムに上記排ガス流を通過させることを特徴とする方法。
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CN (2) | CN101365527A (ja) |
BR (1) | BRPI0618428B8 (ja) |
CA (1) | CA2629129C (ja) |
IN (1) | IN2008CH02893A (ja) |
MX (1) | MX2008006056A (ja) |
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JPWO2011108250A1 (ja) * | 2010-03-02 | 2013-06-20 | 日本板硝子株式会社 | 貴金属微粒子担持触媒およびその製造方法、ならびに浄化触媒 |
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JP5778129B2 (ja) * | 2010-03-02 | 2015-09-16 | 日本板硝子株式会社 | 貴金属微粒子担持触媒およびその製造方法、ならびに浄化触媒 |
JP2018187628A (ja) * | 2013-02-15 | 2018-11-29 | ジョンソン、マッセイ、パブリック、リミテッド、カンパニーJohnson Matthey Public Limited Company | 三元触媒で触媒化されたフィルターを含む火花点火式エンジン及び排気システム |
Also Published As
Publication number | Publication date |
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MY150086A (en) | 2013-11-29 |
US20070104623A1 (en) | 2007-05-10 |
BRPI0618428B1 (pt) | 2018-02-14 |
KR101346417B1 (ko) | 2014-01-02 |
IN2008CH02893A (ja) | 2009-03-06 |
JP2014140844A (ja) | 2014-08-07 |
MX2008006056A (es) | 2008-06-05 |
US8119075B2 (en) | 2012-02-21 |
EP1957185B1 (en) | 2014-03-12 |
CN104147925A (zh) | 2014-11-19 |
CN101365527A (zh) | 2009-02-11 |
JP5767770B2 (ja) | 2015-08-19 |
BRPI0618428B8 (pt) | 2018-03-13 |
WO2007058867A1 (en) | 2007-05-24 |
KR20080077977A (ko) | 2008-08-26 |
BRPI0618428A2 (pt) | 2011-08-30 |
ZA200804946B (en) | 2009-10-28 |
CA2629129A1 (en) | 2007-05-24 |
EP1957185A1 (en) | 2008-08-20 |
CN104147925B (zh) | 2017-01-18 |
CA2629129C (en) | 2014-05-06 |
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