JP2017159296A - 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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- JP2017159296A JP2017159296A JP2017060524A JP2017060524A JP2017159296A JP 2017159296 A JP2017159296 A JP 2017159296A JP 2017060524 A JP2017060524 A JP 2017060524A JP 2017060524 A JP2017060524 A JP 2017060524A JP 2017159296 A JP2017159296 A JP 2017159296A
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Abstract
【解決手段】少なくとも、混合物(M1)を提供するために金属前駆体の水溶液に保護剤を追加する段階、混合物(M2)を提供するために混合物(M1)に還元剤を追加する段階、混合物(M3)を提供するために混合物(M2)に担体物質を追加する段階、混合物(M3)のpHを調節する段階、混合物(M3)の固液相を分離する段階を含む、ディーゼル酸化触媒の製造方法に関し、さらに触媒そのもの、および、ディーゼル酸化触媒としての使用法。
【選択図】なし
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、空気よって攪拌させた後に、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、空気によって、攪拌させた後、1%wt/wtの総金属添加量と、重量の15%のHClを含有しているHCl溶液で、2.4の値まで調節されたpH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、空気よって攪拌させた後に、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、空気によって、攪拌させた後、1%wt/wtの総金属添加量と、重量の15%のHClを含有しているHCl溶液で、2.4の値まで調節されたpH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 (12)
- (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と、
を少なくとも含む、触媒の製造方法。 - 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およびそれらの混合物を有する有機分子から選択される、請求項1に記載の方法。
- 前記保護剤が、ポリ(ビニルアルコール)、ポリ(ビニルピロリドン)、ポリ(エチレンイミン)、ポリ(アクリル酸)、炭水化物またはクエン酸アルカリ金属塩から選択される、請求項1または2に記載の方法。
- 前記金属前駆体が、プラチナ、パラジウム、ロジウム、金および銀の金属塩またはこれら金属塩の混合物のから選択される、請求項1から3のいずれかに記載の方法。
- 前記還元剤が、アルカリ金属ホウ化水素、ヒドラジン、ホルムアルデヒド、クエン酸アルカリ金属塩、アミノボラン錯体、ガス状水素および一酸化炭素から選択される、請求項1から4のいずれかに記載の方法。
- 前記担体物質が、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み、或いはこれらの担体材料の混合物および/または固溶体から選択される、請求項1から5のいずれかに記載の方法。
- 工程(4)で、前記pHが、2から7の範囲の値に調節される、請求項1から6のいずれかに記載の方法。
- 工程(5)で、混合物(M3)の前記固液相が、濾過または前記溶媒の蒸発により分離される、請求項1から7のいずれかに記載の方法。
- 請求項1から8のいずれかの工程によって得られる触媒。
- 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、前記金属粒子の36%以上が、22nm以下の平均直径を有している、金属としてのプラチナおよびパラジウムを含む請求項9に記載の触媒。
- 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、前記金属粒子の90%以上が、PtとPdの両方で構成されている、金属としてのプラチナおよびパラジウムを含む請求項9または10に記載の触媒。
- ディーゼル酸化触媒として、請求項9から11のいずれかの触媒を使用する方法。
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KR102076112B1 (ko) | 2020-02-11 |
PL2461905T3 (pl) | 2017-12-29 |
JP2013500862A (ja) | 2013-01-10 |
ES2641241T3 (es) | 2017-11-08 |
KR20120040732A (ko) | 2012-04-27 |
EP2461905A4 (en) | 2013-02-20 |
WO2011017139A3 (en) | 2011-06-23 |
WO2011017139A2 (en) | 2011-02-10 |
CN105944715A (zh) | 2016-09-21 |
US20140044627A1 (en) | 2014-02-13 |
JP6259186B2 (ja) | 2018-01-10 |
CN102574106A (zh) | 2012-07-11 |
US9687818B2 (en) | 2017-06-27 |
BR112012002614B1 (pt) | 2019-02-26 |
US20110033353A1 (en) | 2011-02-10 |
JP6632559B2 (ja) | 2020-01-22 |
EP2461905B1 (en) | 2017-06-28 |
KR20180019244A (ko) | 2018-02-23 |
EP2461905A2 (en) | 2012-06-13 |
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