JP6632559B2 - コロイド性ナノ粒子の析出によるディーゼル酸化触媒の製造 - Google Patents
コロイド性ナノ粒子の析出によるディーゼル酸化触媒の製造 Download PDFInfo
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- JP6632559B2 JP6632559B2 JP2017060524A JP2017060524A JP6632559B2 JP 6632559 B2 JP6632559 B2 JP 6632559B2 JP 2017060524 A JP2017060524 A JP 2017060524A JP 2017060524 A JP2017060524 A JP 2017060524A JP 6632559 B2 JP6632559 B2 JP 6632559B2
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- catalyst
- noble metal
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- exhaust gas
- combustion engine
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Description
(1)、金属前駆体の水溶液に保護剤を添加して混合物(M1)を得る工程と、
(2)前記混合物(M1)に還元剤を添加して混合物(M2)を得る工程と、
(3)前記混合物(M2)に担体材料を添加して混合物(M3)を得る工程と、
(4)前記混合物(M3)のpHを調節する工程と、
(5)前記混合物(M3)の固液相を分離する工程。
(1)、金属前駆体の水溶液に保護剤を添加して混合物(M1)を得る工程と、
(2)前記混合物(M1)に還元剤を添加して混合物(M2)を得る工程と、
(3)前記混合物(M2)に担体材料を添加して混合物(M3)を得る工程と、
(4)前記混合物(M3)のpHを調節する工程と、
(5)前記混合物(M3)の固液相を分離する工程。
結果として、改良された方法および減少したコストがもたらされる。
溶液1リットルにつき5.1*10-2モルのPtを含有している10.2gのH2PtCl6溶液が、400mlの水に希釈され、そして、溶液1mlにつき10mgのPVPを含有しているPVP溶液の適量が、Pt/PVP重量比率を1に等しくするために追加された。溶液を、1時間、室温で、空気中で攪拌させた後に、NaBH4が、室温で、溶液に追加された。NaBH4の量は、1/2のPt/NaBH4重量比率を有するように、選択された。獲得された混合物を、1時間、空気中で攪拌させた後、1%wt/wtの総金属添加量を達成するために、適量のアルミナ粉末が、溶液に追加され、そして重量の15%のHClを含有しているHCl溶液で、pHが2.4の値まで調節された。30分の攪拌後に、溶液は濾過され、固体粉末が回収された。
同じ方法および同じ量の試薬が、PVP添加を除いて、実施例1のように用いられた。ここでは、溶液1mgにつき10mgのPVPを含有しているPVP溶液の適量が、Pt/PVP重量比率を2に等しくするために追加された。
溶液1リットルにつき5.1*10-2モルのPtを含有している6.6gのH2PtCl6溶液が、110mgのK2PdCl4と共に400mlの水に希釈されたのを除き、同じ方法および同じ量の試薬が、実施例2のように用いられた。
溶液1リットルにつき5.1*10-2モルのPtを含有している6.6gのH2PtCl6溶液が、400mlの水に希釈され、そして、溶液1mlにつき10mgのPVPを含有しているPVP溶液の適量が、Pt/PVP重量比率を1に等しくするために追加された。溶液を、1時間、室温で、空気中で攪拌させた後に、NaBH4が、室温で、溶液に追加された。NaBH4の量は、1/2のPt/NaBH4重量比率を有するように、選択された。結果として生じた溶液は、30分間攪拌され、そして、110mgのK2PdCl4が、溶液に追加された。30分後に、NaBH4が、室温で、溶液に追加された。NaBH4の量は、1/2のPd/NaBH4重量比率を有するように、選択された。獲得された混合物を、1時間、空気中で攪拌させた後、1%wt/wtの総金属添加量を達成するために、適量のアルミナ粉末が、溶液に追加され、そして重量の15%のHClを含有しているHCl溶液で、pHが2.4の値まで調節された。30分の攪拌後に、溶液は濾過され、固体粉末が回収された。
同じ方法および同じ量の試薬が、H2PtCl6とK2PdCl4の添加の順序を逆にしたことを除いて、実施例4のように用いられた。
同じ方法および同じ量の試薬が、PVP添加を除いて、実施例1のように用いられた。ここでは、溶液1mgにつき10mgのPVPを含有しているPVP溶液の適量が、Pt/PVP重量比率を4に等しくするために追加された。
同じ方法および同じ量の試薬が、H2PtCl6、および、担体に対して2%wt/wtの貴金属を有する触媒を獲得するために選択された担体の量を除いて、実施例1のように用いられた。
同じ方法および同じ量の試薬が、H2PtCl6、K2PdCl4、および、担体に対して4%wt/wtの貴金属を有する触媒を獲得するために選択されたアルミナの量を除いて、実施例3のように用いられた。
〔比較例〕
図2を参照にすると、実施例1と同じ方法で調製され、12時間800℃で熱的に熟成した、アルミナ担体に沈澱した、担体物質に対して1%wt/wtのPtを備える試料のXRDスペクトルが示される。
〔比較例〕
図4を参照にすると、実施例3と同じ方法で調製され、12時間800℃で熱的に熟成した、アルミナ担体に沈澱した、担体物質に対して0.67%wt/wtのPtおよび0.33%wt/wtのPdを備える試料のXRDスペクトルが示される。
〔実施例と現状技術の例の比較〕
図6は、従来のディーゼルエンジンの排気ガスをシミュレートする実験室反応器で試験された、試料のガス活性を示す。使用された反応条件は、40mgの粉末が100mgのコーディエライト材料で希釈され、そして、混合物が250―500マイクロメートルの範囲で圧壊され、篩にかけられた、固定床管型反応器であった。総ガス流量は200mL/分で、そして、結果として生じる空間速度はモノリス試料が経験する1時間当たり15,000―20,000に相当した。粉末反応器試験で使用される気体組成は、CO2000ppm、NO100ppm、C3H6300ppm、C3H6300ppm、トルエン350ppm、O212%、H2O5%であった。特に明記しない限り、炭化水素(HC)濃度は、C1基準で報告される。
Claims (18)
- 触媒を基体上に含む、燃焼エンジンの排ガスの浄化用触媒複合体であって、
前記触媒は、貴金属成分、及び該貴金属成分用の担体材料を含み、及び
前記貴金属成分は、熱的な熟成において分散されるコロイドとしてもたらされたナノ粒子を前記担体材料上に含み、及び
前記触媒は、ディーゼル酸化触媒として有効であり、及び、
前記基体は、流通基体、又は壁流基体を含み、及び
前記貴金属成分としてプラチナ及びパラジウムを含み、及び酸化性雰囲気(空気に10%のH2O)で、前記触媒を800℃で12時間処理した後に、前記貴金属成分の粒子の36%以上が、22nm未満の平均直径を有していることを特徴とする燃焼エンジンの排ガスの浄化用触媒複合体。 - 前記貴金属成分が更に、ロジウム、金、銀、又はこれらの混合物を含み、及び前記担体材料が、酸化アルミニウム、酸化ケイ素、酸化セリウム、酸化ジルコニウム、酸化チタン、酸化マグネシウムの純物質またはこれらの混合物またはこれらの固溶体を含むことを特徴とする請求項1に記載の燃焼エンジンの排ガスの浄化用触媒複合体。
- 前記貴金属成分が、コロイドとして、及び保護剤使用下にもたらされたナノ粒子を含むことを特徴とする請求項1に記載の燃焼エンジンの排ガスの浄化用触媒複合体。
- 前記コロイドとして、及び保護剤使用下にもたらされたナノ粒子が、水性混合物中で還元及び保護剤と金属成分の前駆体の混合物のpH調整によって前記担体材料上に沈澱されることを特徴とする請求項3に記載の燃焼エンジンの排ガスの浄化用触媒複合体。
- 前記保護剤が、1個以上のアミノ、アミド、カルボキシル、アルデヒドまたはヒドロキシル基を有する可溶性ホモポリマーおよびコポリマー、ならびに、1個以上のアミノ、アミド、カルボキシル、アルデヒドまたはヒドロキシ基を有する有機分子、およびそれらの混合物から選択されることを特徴とする請求項3に記載の燃焼エンジンの排ガスの浄化用触媒複合体。
- 前記貴金属成分がプラチナ及びパラジウムを含み、及び酸化性雰囲気(空気に10%のH2O)で、前記触媒を800℃で12時間処理した後に、前記貴金属粒子の90%以上が、PtとPdの両方で構成されていることを特徴とする請求項1に記載の燃焼エンジンの排ガスの浄化用触媒複合体。
- 前記貴金属成分がプラチナ及びパラジウムを実質的に等しいモル比率で含み、及び酸化性雰囲気(空気に10%のH2O)で、前記触媒を800℃で12時間処理した後に、貴金属粒子の78%以上が0.8〜1.2の範囲のPt:Pdのモル割合で構成されることを特徴とする請求項1に記載の燃焼エンジンの排ガスの浄化用触媒複合体。
- 前記貴金属成分がプラチナ及びパラジウムを実質的に等しいモル比率で含み、及び酸化性雰囲気(空気に10%のH2O)で、前記触媒を800℃で12時間処理した後に、貴金属粒子の63%以上が0.9〜1.1の範囲のPt:Pdのモル割合で構成されることを特徴とする請求項1に記載の燃焼エンジンの排ガスの浄化用触媒複合体。
- 以下の工程;
(1)金属前駆体の水溶液に保護剤を添加して混合物(M1)を得る工程と、
(2)前記混合物(M1)に還元剤を添加して混合物(M2)を得る工程と、
(3)前記混合物(M2)に担体材料を添加して混合物(M3)を得る工程と、
(4)前記混合物(M3)のpHを調節し、担体材料上に金属粒子を含む触媒を形成する工程と、
(5)前記混合物(M3)の前記触媒と液相を分離する工程と、
(6)触媒を担体上に沈澱させる工程と、
を含み、
工程(2)で添加される前記還元剤は、アルカリ金属ホウ化水素、及びクエン酸アルカリ金属塩から成る群から選ばれ、及び
工程(3)で、前記担体材料は、液相中に懸濁されており、
工程(4)で、前記触媒は、液相中に懸濁されている、
ことを特徴とする請求項1に記載の燃焼エンジンの排ガスの浄化用触媒複合体を製造する方法。 - 前記保護剤が、1個以上のアミノ、アミド、カルボキシル、アルデヒドまたはヒドロキシル基を有する可溶性ホモポリマーおよびコポリマー、ならびに、1個以上のアミノ、アミド、カルボキシル、アルデヒドまたはヒドロキシ基を有する有機分子、及びこれらの混合物から選択される、ことを特徴とする請求項9に記載の方法。
- 前記金属前駆体が、プラチナ及びパラジウムの金属塩に加え、ロジウム、金、銀、又はこれらの混合物の金属塩から成る群から選ばれることを特徴とする請求項9に記載の方法。
- 前記担体材料が、酸化アルミニウム、酸化ケイ素、酸化セリウム、酸化ジルコニウム、酸化チタン、酸化マグネシウムの純物質またはこれらの混合物およびこれらの固溶体から成る群から選ばれることを特徴とする請求項9に記載の方法。
- 工程(5)で、混合物(M3)の前記触媒と前記液相が、濾過または前記溶媒の蒸発により分離されることを特徴とする請求項9に記載の方法。
- 金属としてプラチナ及びパラジウムを含み、及び酸化性雰囲気(空気に10%のH2O)で、前記触媒を800℃で12時間処理した後に、金属粒子の90%以上が、PtとPdの両方で構成されていることを特徴とする請求項9に記載の方法。
- ディーゼル排気を、請求項9に記載の方法によって得られた触媒複合体と接触させることを特徴とするディーゼル排気を酸化させる方法。
- 燃焼エンジンの排ガスの浄化用触媒であって、
プラチナ、パラジウム、又はこれらの混合物を含む貴金属成分、
酸化アルミニウムの粒子を含む貴金属成分用の担体材料、
を含み、
酸化性雰囲気(空気に10%のH2O)で、前記触媒を800℃で12時間処理した後に、前記貴金属成分の36%以上が、22nm未満の平均直径を有し、及び
ディーゼル酸化触媒として有効であることを特徴とする燃焼エンジンの排ガスの浄化用触媒。 - 前記貴金属成分が、コロイド的に、及び保護剤使用下にもたらされたナノ粒子を含むことを特徴とする請求項16に記載の燃焼エンジンの排ガスの浄化用触媒。
- プラチナ及びパラジウムが実質的に等しいモル比率であり、及び酸化性雰囲気(空気に10%のH2O)で、前記触媒を800℃で12時間処理した後に、貴金属粒子の78%以上が0.8〜1.2の範囲のPt:Pdのモル比率で構成されることを特徴とする請求項16に記載の燃焼エンジンの排ガスの浄化用触媒。
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KR20180019244A (ko) | 2018-02-23 |
JP2017159296A (ja) | 2017-09-14 |
WO2011017139A3 (en) | 2011-06-23 |
US9687818B2 (en) | 2017-06-27 |
US20110033353A1 (en) | 2011-02-10 |
EP2461905A4 (en) | 2013-02-20 |
EP2461905B1 (en) | 2017-06-28 |
KR20120040732A (ko) | 2012-04-27 |
ES2641241T3 (es) | 2017-11-08 |
JP6259186B2 (ja) | 2018-01-10 |
CN105944715A (zh) | 2016-09-21 |
PL2461905T3 (pl) | 2017-12-29 |
WO2011017139A2 (en) | 2011-02-10 |
KR102076112B1 (ko) | 2020-02-11 |
JP2013500862A (ja) | 2013-01-10 |
US20140044627A1 (en) | 2014-02-13 |
BR112012002614B1 (pt) | 2019-02-26 |
EP2461905A2 (en) | 2012-06-13 |
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