JP7314357B2 - 白金族金属ナノ粒子を含むディーゼル酸化触媒 - Google Patents
白金族金属ナノ粒子を含むディーゼル酸化触媒 Download PDFInfo
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- JP7314357B2 JP7314357B2 JP2022080335A JP2022080335A JP7314357B2 JP 7314357 B2 JP7314357 B2 JP 7314357B2 JP 2022080335 A JP2022080335 A JP 2022080335A JP 2022080335 A JP2022080335 A JP 2022080335A JP 7314357 B2 JP7314357 B2 JP 7314357B2
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Description
DOC組成物は、還元ナノ粒子形態のPGM構成成分(例えば、PGMの少なくとも約90%は、還元形態にある)を含み、1種または複数の多孔質の耐熱性酸化物支持体を一般にさらに含む。本明細書で使用する場合、「白金族金属」または「PGM」とは、白金(Pt)、パラジウム(Pd)、ルテニウム(Ru)、ロジウム(Rh)、オスミウム(Os)、イリジウム(Ir)およびそれらの混合物を含めた、白金族金属またはその酸化物を指す。ある特定の実施形態では、白金族金属は、約1:10~約10:1の質量比、さらに一般には、約1.5:1以上、約2:1以上、または約5:1以上の白金対パラジウム比などの、白金とパラジウムの組合せを含む。PGM構成成分(例えば、Pt、Pdまたはそれらの組合せ)の濃度は、様々となり得るが、所与の組成物中、多孔質の耐熱性酸化物支持材料(例えば、耐熱性酸化物支持体に対して、約1質量%~約6質量%)の質量に対して、通常、約0.1質量%~約10質量%になろう。
1つまたは複数の実施形態によれば、DOC組成物を支持するために使用される基材は、車両用触媒を製造するために、通常、使用される任意の材料から構成され得、金属製またはセラミック製のハニカム構造を、通常、含むであろう。基材は、通常、DOCウォッシュコート組成物が施用されて付着し、これにより、触媒組成物の担体として作用する、複数の壁表面をもたらす。
本開示によれば、DOC触媒組成物は、PGMナノ粒子(PGMNP)のコロイド状分散液を耐熱性酸化物支持材料と会合させることにより、一般に製造される。このようなコロイド状分散液は、一部の実施形態では、a)1種または複数の白金族金属ナノ粒子(PGMNP)の複数、b)分散媒体、c)安定化剤、およびd)還元剤を含むことができ、これは、本明細書の以下により詳細に開示される。
上で言及される通り、DOC組成物は、一部の実施形態では、独立して製造されて、基材上にコーティングされる。DOC組成物は、水と混合して(乾燥形態にある場合)、触媒基材をコーティングするためのスラリーを形成することができる。スラリーは、触媒粒子に加え、結合剤、炭化水素(HC)貯蔵構成成分(例えば、ゼオライト)、会合性増粘剤、および/または界面活性剤(陰イオン性、陽イオン性、非イオン性または両性界面活性剤を含む)を任意に含有することができる。一部の実施形態では、スラリーのpHは、例えば、約3~約5の酸性pHに調節することができる。
本発明はまた、本明細書に記載されているDOC組成物または物品を組み込んだ排出物処理システムを提供する。本発明のDOC組成物は、ディーゼル排気ガス排出物の処理のための1種または複数の追加の構成成分を含む、一体型排出物処理システムで、通常、使用される。したがって、用語「排気流」、「エンジン排気流」、「排気ガス流」などは、エンジン放出、および本明細書に記載されている1種または複数の他の触媒システム構成成分の下流での放出を指す。
400個のセル密度を有するコーディエライト基材を、酸性(p=4.5)の1.5%のSiO2-Al2O3支持材料のスラリーによりコーティングして、1.0g/in3のウォッシュコート使用量を実現した。110℃/2時間で乾燥し、450℃/1時間で焼成した後、コーティングされている基材を必要なPt量およびコーティングされている基材が吸収する水の量に基づいて算出した所定の濃度を有するPt(NH3)4(OH)2溶液に浸漬した。過剰の液体をコーティングされている基材から吹いて除去し、湿潤試料をホットエアガンを用いて迅速に乾燥し、次に、空気中、450℃で1時間、焼成した。最終的なPt使用量は、20g/ft3であった。得られた材料は、図6Aに示されている通り、0~1nmのPt粒子が大多数であること、および粒子サイズのバイモーダル分布であることを示している。
実施例5Aと同様に、1.0g/in3のSi-Al2O3材料でコーティングした基材を製造した。コーティング済み試料を、実施例1のコロイド状Ptナノ粒子分散液に浸漬した。過剰の液体をコーティングされている基材から吹いて除去し、湿潤試料をホットガンを用いて迅速に乾燥し、次に、空気中、450℃で1時間、焼成した。最終的なPt使用量は、20g/ft3であった。図6B中に示されている通り、得られた材料は、1~3nmのPt粒子を含む。
実施例5Aおよび5Bの比較材料および本発明の材料を、100℃~500℃までのNOライトオフ試験前に、NOライトオフガス混合物中(NO500ppm;CO100ppm;C3H610ppm;10%O2、7%H2O;5%CO2;SV 50K/時)、500℃で1時間、処理した。図7に示される通り、実施例5Bのコーティング済み基材は、実施例5Aのコーティング済み基材よりも、NOのNO2への転化率がかなり高いことを示した。次に、どちらのコーティング済み基材にも、空気中、10%流で、550℃/50時間、水熱エージングを施し、上のように試験した。図8に示されている通り、水熱エージング後、実施例5Aのコーティング済み基材(非コロイド状のPt錯体溶液を使用して製造)は、非常に大きなPt粒子(例えば、粒子サイズは最大約100nm、図8A)であることを示している一方、実施例5Bのコーティング済み基材(コロイド状Ptナノ粒子分散液を使用して製造)は、大きな粒子はより少ないことを示した。しかし、図8Bの、最大約80nmまでの粒子サイズを有する粒子が依然として観察された。実施例5Aおよび5Bの比較材料および本発明の材料のどちらも、エージング時にかなり焼結する。実施例5Bの本発明の材料は、全体的に、それほど焼結していないことを示している。
ドープした1.5%のSiO2-Al2O3材料を希釈Ptアミン錯体溶液にインシピエントウエットネス(incipient wetness)含浸し、得られた材料を脱イオン(DI)水に加えて、スラリー懸濁液を形成した。スラリー懸濁液のpHを希HNO3によって4~5に調節した。このスラリーをD90=12~15μmまでミル粉砕し、1.5%のSiO2-Al2O3材料の2.5質量%の使用量で、アルミナ結合剤材料を加えた。次に、このスラリーを400/4ハニカム基材に、30~45%の固体含有率でコーティングした。乾燥後、触媒コーティング基材を、空気中、450℃で1時間、焼成した。得られたウォッシュコート使用量は、1.037g/in3であり、Pt使用量は、20g/ft3であった。
ドープした1.5%のSiO2-Al2O3材料をDI水に加えて、スラリー懸濁液を形成させて、スラリー懸濁液のpHを希HNO3により4~5に調節した。このスラリーをD90=12~15μmまでミル粉砕し、実施例6Aと同じPt使用量、次いで、1.5%SiO2-Al2O3材料が2.5質量%となる使用量のアルミナ結合剤材料を生じるよう、ミル粉砕したスラリーに実施例1のコロイド状Pt溶液の量を加えた。次に、このスラリーを400/4ハニカム基材上にコーティングし、実施例8Aに記載されている通り、焼成した。代替として、任意のミル粉砕前に、ドープした1.5%SiO2-Al2O3支持材料をコロイド状Ptの希釈溶液に直接、加えることができた。この改変は、高いPt使用量において、およびコロイド状前駆体中のPt濃度が低い場合、特に有用である。
実施例6Aおよび6Bのコーティング済みハニカム基材は、550℃で100時間、連続的にディーゼルエンジンでエージングし、Euro6のキャリブレーションを行ったエンジンのエンジンアウト条件(模倣世界統一試験サイクル(WHTC)の平均温度、225℃)を模倣した、過渡ディーゼルラボリアクター(transient diesel lab reactor)で評価した。実施例6Aおよび6Bのコーティング済み基材を用いて達成されたNOのNO2転化率、図10に比較している。実施例6Bのコーティング済み基材(コロイド状Pt分散液を使用して製造)は、実施例6Aのコーティング済み基材(非コロイド状Pt錯体溶液を使用して製造)よりも7%高いNO転化率を示す。
ドープした14%のSiO2-TiO2材料を希釈Ptアミン錯体溶液にインシピエントウエットネス含浸し、次に、DI水に加えて、スラリー懸濁液を形成した。スラリー懸濁液のpHを、希HNO3によって4~5に調節した。このスラリーをD90=12~15μmになるまでミル粉砕し、14%のSiO2TiO2材料が2.5質量%の使用量となるシリカ結合剤材料を加えた。次に、このスラリーを400/4ハニカム基材に、25~30%の固体含有率でコーティングした。乾燥後、触媒コーティング基材を、空気中、450℃で1時間、焼成した。得られたウォッシュコート使用量は、0.774g/in3であり、Pt使用量は、10g/ft3であった。
実施例1の希釈コロイド状Pt溶液(所望のPt使用量を達成するよう希釈した)に、ドープした14%のSiO2-TiO2材料を加えて、スラリー懸濁液を形成させて、このスラリー懸濁液のpHを希HNO3により4~5に調節した。このスラリーをD90=12~15μmまでミル粉砕し、14%のSiO2-TiO2材料が2.5質量%となる使用量で、シリカ結合剤材料を加えた。次に、このスラリーを400/4ハニカム基材上に25~29%の固体含有率でコーティングし、実施例7Aに記載されている通り、焼成した。得られたウォッシュコート使用量は、0.774g/in3であり、Pt使用量は、10g/ft3であった。
実施例7Aおよび7Bのコーティング済み基材を、550℃で100時間、連続的にディーゼルエンジンでエージングし、実施例5Aおよび5Bと同じ試験条件下で、NOライトオフについて評価した。図11に示されている通り、実施例7Bのコーティング済み基材(コロイド状Pt分散液を使用して製造)は、実施例7A(非コロイド状Pt錯体溶液を使用して製造)よりもかなり多量にNO2を生成することを示した。
ドープした1.5%のSiO2-Al2O3材料を希釈Ptアミン錯体溶液にインシピエントウエットネス含浸し、得られた材料をDI水に加えて、スラリー懸濁液を形成した。スラリー懸濁液のpHは、希HNO3によって4~5に調節した。スラリーをミル粉砕して、D90=4~5μmにし、次に、200/12コーディエライトフィルター基材上に15~20%の固体含有率でコーティングした。暖かい空気を用いて迅速に乾燥した後、触媒コーティング基材を、空気中、450℃で1時間、焼成した。得られたウォッシュコート使用量は、0.15g/in3であり、Pt使用量は、5g/ft3であった。
ドープした1.5%のSiO2-Al2O3材料をDI水に加えて、スラリー懸濁液を形成し、スラリー懸濁液のpHを希HNO3により4~5に調節した。このスラリーをミル粉砕して、D90=4~5μmにし、実施例1のコロイド状Pt分散液を加え(所望のPt使用量に基づいて決定した量で)、次に、このスラリーを200/12コーディエライトフィルター基材上にコーティングし、このコーティング済み基材を実施例8Aに記載されている通り焼成した。得られたウォッシュコート使用量は、0.15g/in3であり、Pt使用量は、5g/ft3であった。
実施例8Aおよび8Bのコーティング済み基材は、10%流を含有する空気中、550℃で50時間、連続的にエージングし、実施例6Aおよび6Bについて記載されている世界統一試験サイクル(WHTC)により、ディーゼル車両シミュレータで評価した。実施例8Aおよび8Bの触媒コーティング基材のNOのNO2への転化率が、図12に比較されており、この図は、実施例8Bの触媒コーティング基材(コロイド状Pt分散液を使用して製造)を使用して達成されたNO転化率は、実施例8Aの触媒コーティング基材(非コロイド状Pt錯体溶液を使用して製造)を使用して達成されたものよりも3%高いことを示している。
Claims (34)
- ディーゼル酸化触媒組成物であって、
Pt、Pd、Au、Ag、Ru、Rh、Ir、Os、それらの合金およびそれらの混合物からなる群から選択される、複数の白金族金属ナノ粒子であって、該白金族金属の90%以上が、完全還元形態にあり、該ナノ粒子は、1~10nmの平均粒子サイズを有しており、該ナノ粒子の少なくとも90%が、平均粒子サイズの+/-2nmとなる粒子サイズを有する、白金族金属ナノ粒子と、
耐熱性金属酸化物材料と
を含み、及び
ハロゲン化物、アルカリ金属、アルカリ土類金属、硫黄化合物およびホウ素化合物の含有量が、ディーゼル酸化触媒組成物の質量に基づいて0.05%未満であり、
前記耐熱性金属酸化物材料が、SiO 2 をドープしたZrO 2 を含む、ディーゼル酸化触媒組成物。 - ナノ粒子の少なくとも90%が、平均粒子サイズの+/-1nmとなる粒子サイズを有する、請求項1に記載のディーゼル酸化触媒組成物。
- ナノ粒子の少なくとも95%が、平均粒子サイズの+/-2nmとなる粒子サイズを有する、請求項1に記載のディーゼル酸化触媒組成物。
- ナノ粒子の少なくとも95%が、平均粒子サイズの+/-1nmとなる粒子サイズを有する、請求項1に記載のディーゼル酸化触媒組成物。
- ナノ粒子の平均粒子サイズが、2~3nmである、請求項1に記載のディーゼル酸化触媒組成物。
- ナノ粒子の平均粒子サイズが、3~5nmである、請求項1に記載のディーゼル酸化触媒組成物。
- ナノ粒子の平均粒子サイズが、5~7nmである、請求項1に記載のディーゼル酸化触媒組成物。
- ナノ粒子の平均粒子サイズが、7~9nmである、請求項1に記載のディーゼル酸化触媒組成物。
- ディーゼル酸化触媒組成物の合計質量に基づいて、ホウ素の含有量が10ppm未満であり、およびナトリウムの含有量が10ppm未満である、請求項1に記載のディーゼル酸化触媒組成物。
- 白金族金属ナノ粒子が白金を含む、請求項1に記載のディーゼル酸化触媒組成物。
- 耐熱性金属酸化物が、1~30%のSiO2をドープしたZrO2を含む、請求項1に記載のディーゼル酸化触媒組成物。
- 請求項1~11のいずれか一項に記載のディーゼル酸化触媒組成物を含むコーティングがその上に配置されている基材を含む、ディーゼル酸化触媒物品。
- 耐熱性金属酸化物材料が、基材を覆う層として存在し、かつ基材とコーティングとの間に配置されている、請求項12に記載のディーゼル酸化触媒物品。
- ディーゼルエンジンからの排気流を処理する方法であって、請求項12に記載のディーゼル酸化触媒物品に排気流を通過させて、NOが該触媒物品内部で酸化されるようする工程を含む、方法。
- 請求項1~11のいずれか一項に記載のディーゼル酸化触媒組成物を含むコーティングがその上に配置されている基材を含む、触媒添加煤フィルター物品。
- 請求項1~14の何れか1項に記載のディーゼル酸化触媒組成物を作製する方法であって、SiO 2 をドープしたZrO 2 を含む耐熱性金属酸化物スラリー、および白金族金属ナノ粒子を含むコロイド状分散液を基材に施用する工程を含む、方法。
- ディーゼル酸化触媒組成物が、ディーゼル酸化触媒物品または触媒添加煤フィルター物品に使用される、請求項16に記載の方法。
- 施用工程後に、コーティングされた基材を焼成する工程をさらに含む、請求項16に記載の方法。
- 水中の耐熱性金属酸化物スラリーおよびコロイド状分散液を含むウォッシュコートスラリーを形成する工程と、耐熱性金属酸化物スラリーおよびコロイド状分散液を、ウォッシュコートの形態にある基材に施用する工程とをさらに含む、請求項16に記載の方法。
- 基材に耐熱性金属酸化物スラリーを施用する工程と、
基材上の耐熱性金属酸化物コーティングを焼成する工程と、
その後に、焼成済み耐熱性金属酸化物コーティングの上にコロイド状分散液を施用する工程と
を含む、請求項16に記載の方法。 - 白金族金属ナノ粒子が白金を含む、請求項16に記載の方法。
- ナノ粒子の少なくとも90%が、平均粒子サイズの+/-1nmとなる粒子サイズを有する、請求項16に記載の方法。
- ナノ粒子の少なくとも95%が、平均粒子サイズの+/-2nmとなる粒子サイズを有する、請求項16に記載の方法。
- ナノ粒子の少なくとも95%が、平均粒子サイズの+/-1nmとなる粒子サイズを有する、請求項16に記載の方法。
- ナノ粒子の平均粒子サイズが、2~3nmである、請求項16に記載の方法。
- ナノ粒子の平均粒子サイズが、3~5nmである、請求項16に記載の方法。
- ナノ粒子の平均粒子サイズが、5~7nmである、請求項16に記載の方法。
- ナノ粒子の平均粒子サイズが、7~9nmである、請求項16に記載の方法。
- 前記コロイド状分散液の合計質量に基づいて、該コロイド状分散液のホウ素の含有量が10ppm未満であり、およびナトリウムの含有量が10ppm未満である、請求項16に記載の方法。
- 触媒物品に550~600℃で加熱処理を施すことにより該物品をエージングする工程であって、エージング後のPGM粒子の少なくとも50%が、1~50nmの直径を有する、エージングする工程をさらに含む、請求項16に記載の方法。
- 触媒物品に550~600℃で加熱処理を施すことにより前記触媒物品をエージングする工程であって、エージング後のPGM粒子の少なくとも75%が、1~50nmの直径を有する、エージングする工程をさらに含む、請求項16に記載の方法。
- 触媒物品に550~600℃で加熱処理を施すことにより前記触媒物品をエージングする工程であって、エージング後のPGM粒子の少なくとも50%が、1~25nmの直径を有する、エージングする工程をさらに含む、請求項16に記載の方法。
- a)分散媒体および水溶性ポリマー懸濁安定化剤の存在下、Pt、Pd、Au、Ag、Ru、Rh、Ir、Osおよびそれらの合金の塩から選択される白金族金属前駆体の溶液であって、白金族金属前駆体が、ハロゲン化物、アルカリ金属、アルカリ土類金属、硫黄化合物およびホウ素化合物を実質的に含まない、溶液を製造する工程と、
b)この溶液を還元剤と一緒にして、白金族金属ナノ粒子のコロイド状分散液を得る工程であって、ナノ粒子濃度が、コロイド状分散液の総質量の少なくとも2質量%であり、コロイド状分散液中の白金族金属の少なくとも90%が完全還元形態にある工程と
を含む方法により、白金族金属ナノ粒子を製造することをさらに含む、請求項16に記載の方法。 - 排気ガス流を処理するための排出物処理システムであって、
排気ガス流を生成するディーゼルエンジンと、
排気ガス流と流体連通して配置されており、かつ排気流中の一酸化炭素および炭化水素ガスを酸化して処理済み排気ガス流を形成するようになされている、請求項12に記載の第1の触媒物品と、
第1の触媒物品の下流にあり、かつ処理済み排気ガス流と流体連通している少なくとも1つの追加の触媒物品であり、アンモニア酸化、微粒子ろ過、NOx貯蔵、NOx捕捉、NOxの選択的触媒還元またはそれらの組合せを行うようになされている、少なくとも1つの追加の触媒物品と
を含む、排出物処理システム。
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