JP2015501719A - 触媒化基材モノリス - Google Patents
触媒化基材モノリス Download PDFInfo
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- JP2015501719A JP2015501719A JP2014545366A JP2014545366A JP2015501719A JP 2015501719 A JP2015501719 A JP 2015501719A JP 2014545366 A JP2014545366 A JP 2014545366A JP 2014545366 A JP2014545366 A JP 2014545366A JP 2015501719 A JP2015501719 A JP 2015501719A
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- substrate monolith
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- 239000000758 substrate Substances 0.000 title claims abstract description 176
- 230000003197 catalytic effect Effects 0.000 title description 12
- 239000003054 catalyst Substances 0.000 claims abstract description 181
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- 238000000576 coating method Methods 0.000 claims abstract description 90
- 239000011248 coating agent Substances 0.000 claims abstract description 84
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- 238000002485 combustion reaction Methods 0.000 claims abstract description 20
- 239000000463 material Substances 0.000 claims abstract description 15
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- 238000007254 oxidation reaction Methods 0.000 claims description 28
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 25
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- 238000001914 filtration Methods 0.000 claims description 23
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- JSKIRARMQDRGJZ-UHFFFAOYSA-N dimagnesium dioxido-bis[(1-oxido-3-oxo-2,4,6,8,9-pentaoxa-1,3-disila-5,7-dialuminabicyclo[3.3.1]nonan-7-yl)oxy]silane Chemical compound [Mg++].[Mg++].[O-][Si]([O-])(O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2)O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2 JSKIRARMQDRGJZ-UHFFFAOYSA-N 0.000 description 2
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- 150000003839 salts Chemical class 0.000 description 2
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- MGWGWNFMUOTEHG-UHFFFAOYSA-N 4-(3,5-dimethylphenyl)-1,3-thiazol-2-amine Chemical compound CC1=CC(C)=CC(C=2N=C(N)SC=2)=C1 MGWGWNFMUOTEHG-UHFFFAOYSA-N 0.000 description 1
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- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
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- JYIBXUUINYLWLR-UHFFFAOYSA-N aluminum;calcium;potassium;silicon;sodium;trihydrate Chemical compound O.O.O.[Na].[Al].[Si].[K].[Ca] JYIBXUUINYLWLR-UHFFFAOYSA-N 0.000 description 1
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- ZMIGMASIKSOYAM-UHFFFAOYSA-N cerium Chemical compound [Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce] ZMIGMASIKSOYAM-UHFFFAOYSA-N 0.000 description 1
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- AABBHSMFGKYLKE-SNAWJCMRSA-N propan-2-yl (e)-but-2-enoate Chemical group C\C=C\C(=O)OC(C)C AABBHSMFGKYLKE-SNAWJCMRSA-N 0.000 description 1
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Classifications
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- B01D53/9413—Processes characterised by a specific catalyst
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Abstract
Description
NO+1/2O2 → NO2 (1)、及び
BaO+2NO2+1/2O2 → Ba(NO3)2 (2)
であり、ここで、反応(1)では、一酸化窒素が白金上の活性酸化部位で酸素と反応して、NO2を形成する。反応(2)は、無機硝酸塩の形の貯蔵物質によるNO2の吸着を含む。
Ba(NO3)2→BaO+2NO+3/2O2又はBa(NO3)2
→BaO+2NO2+1/2O2 (3)、及び
NO+CO→1/2N2+CO2 (4)
(他の反応には、Ba(NO3)2+8H2→BaO+2NH3+5H2O、それに続くNH3+NOx→N2+yH2O又は2NH3+2O2+CO→N2+3H2O+CO2などが含まれる。)。
4NH3+4NO+O2→4N2+6H2O(即ち、1:1 NH3:NO)(5)
4NH3+2NO+2NO2→4N2+6H2O(即ち、1:1 NH3:NOx)(6)
8NH3+6NO2→7N2+12H2O(即ち、4:3 NH3:NOx)(7)
関連がある望ましくない、非選択的な副反応は、
2NH3+2NO2→N2O+3H2O+N2 (8)
である。
4NH3+5O2→4NO+6H2O (9)
市販されているベータゼオライトを撹拌しながらFe(NO3)3の水溶液に加えた。混合した後、結合剤及びレオロジー改質剤を加えて、ウォッシュコート組成物を形成した。
脱イオン水中における比較的高い粒度分布まで粉砕したアルミナ粒子、硝酸白金、結合剤及びレオロジー改質剤の混合物を含むウォッシュコート組成物を調製した。チタン酸アルミニウムウォールフローフィルターを、出願人/譲受人の国際公開2011/080525に開示されている方法及び装置を用いてウォッシュコート添加0.2g/in3から総計Pt添加が5gft−3の触媒組成物でコーティングした。ここでは、上流側まで配向させることが意図されている第1の端部におけるチャンネルを、それらの全長の75%で、硝酸白金及び微粒子アルミナを含むウォッシュコートにより、その意図されている上流端部からコーティングし;反対端における下流側に配向させることが意図されているチャンネルを、それらの全長の25%で、入口チャンネルと同じウォッシュコートでコーティングした。すなわち、この方法は、(i)ハニカムモノリス基材を実質的に垂直に保持するステップ;(ii)基材の下端でチャンネルの開口端から所定の容量の液体を基材に導入するステップ;(iii)基材内に導入した液体を密封維持するステップ;(iv)維持した液体を含有する基材を逆にするステップと;(v)逆にした基材の下端で基材のチャンネルの開口端に減圧を施して、基材のチャンネルに沿って液体を引き込むステップを含んでいた。触媒組成物を、第1の端部からフィルターチャンネル上にコーティングし、その後コーティングしたフィルターを乾燥させた。乾燥させた第1の端部からコーティングしたフィルターを、次に回転させ、この方法を繰り返してフィルターチャンネルに同じ触媒を第2の端部からコーティングし、続いて乾燥及びか焼した。
ガス接触の入口側に向かう配向が意図されたチャンネルの全チャンネル長の100%を、硝酸白金及びアルミナを含有するウォッシュコートでコーティングしてから、コーティングしたフィルターを乾燥させ;出口側に向かって配向させることが意図されたPtコーティングしたフィルターのチャンネルの全長の35%を、硝酸パラジウム及びアルミナを含有するウォッシュコートでコーティングしたこと以外は、比較例2と同じ方法を用いて、コーティングしたフィルターを調製した。得られた完全にコーティングしたフィルターを次いで乾燥させ、次いでか焼した。コーティングしたフィルター上へのPtの完全添加量は、5gft−3であり、コーティングしたフィルター上へのPdの完全添加量は、1.75gft−3であった。
出口側に向かう配向が意図されたチャンネルの全長の35%を、アルミナのみを含有するウォッシュコートでコーティングしたこと以外は、実施例3と同じ方法を用いて、コーティングしたフィルターを調製した。得られたコーティングしたフィルターを次いで乾燥させ、次いでか焼した。コーティングしたフィルターの入口チャンネル上へのPtの完全添加量は、5gft−3であった。
フィルターの出口チャンネルに塗布したウォッシュコートが硝酸白金に加えて硝酸パラジウムを含んでいたこと以外は、比較例2と同じ方法を用いて、コーティングしたフィルターを調製した。入口及び出口チャンネルにおけるウォッシュコート添加は、入口表面と出口表面の両方の上に5g/ft3Pt、1.25g/ft3Pd添加、すなわち全PGM添加が6.25g/ft3に達するように行った。
二層のウォッシュコートを出口チャンネルの25%全ゾーン長に塗布したこと以外は、比較例2と同じ方法を用いて、コーティングしたフィルターを調製した。第1の(又は下端)層では、ウォッシュコートは、硝酸白金及びアルミナを含有していた。コーティングしたフィルターを次いで乾燥及びか焼してから、硝酸パラジウム及びアルミナを含有した第2の(又は最上)層のウォッシュコートを塗布した。入口及び出口チャンネルにおけるウォッシュコート添加は、入口チャンネル及び出口チャンネル上への全総計添加の5g/ft3Pt、1.25g/ft3Pd添加、すなわち全PGM添加が6.25g/ft3に達するように行った。
フィルターの入口チャンネルと出口チャンネルの両方に塗布したウォッシュコートが硝酸白金に加えて硝酸パラジウムを含んでいたこと以外は、比較例2と同じ方法を用いて、コーティングしたフィルターを調製した。入口及び出口チャンネルにおけるウォッシュコート添加は、入口表面と出口表面の両方の上に5g/ft3Pt、5g/ft3Pd添加、すなわち全PGM添加が10g/ft3に達するように行った。
フィルターの入口チャンネルと出口チャンネルの両方に塗布したウォッシュコートが硝酸白金に加えて硝酸パラジウムを含んでいたこと以外は、比較例2と同じ方法を用いて、コーティングしたフィルターを調製した。入口及び出口チャンネルにおけるウォッシュコート添加は、入口表面と出口表面の両方の上に5g/ft3Pt、1g/ft3Pd添加、すなわち全PGM添加が6g/ft3に達するように行った。
図1に例示されている第1の合成触媒活性試験(SCAT)実験室用反応器で試験を行った。この反応器内では、実施例1のコーティングしたFe/ベータゼオライトSCR触媒のフレッシュなコアが、比較例2又は実施例3、4、5、6、7もしくは8の触媒化ウォールフローフィルターのいずれかのコアの下流の導管に配されている。触媒行程容積が30,000hr−1で合成ガス混合物を導管に通した。フィルター入口温度900℃で60分間、定常状態の温度で触媒化ウォールフローフィルター試料を加熱(又は「エージング」)するために炉を使用し、その間、入口SCR触媒の温度は300℃であった。フィルターとSCR触媒の間の温度降下をもたらすために、空気(熱交換器)又は水冷メカニズムを使用した。エージング中のガス混合物は、10%O2、6%H2O、6%CO2、100ppmCO、400ppmNO、100ppmClとしてのHC、残余N2であった。
市販されているアルミノシリケートCHAゼオライトを、Cu(NO3)2水溶液に撹拌しながら加えた。スラリーをろ過し、次いで洗浄及び乾燥させた。所望の金属添加を達成するまで、手順を繰り返すことができる。最終生成物をか焼した。混合後、結合剤及びレオロジー改質剤を加えて、ウォッシュコート組成物を形成した。
2種のディーゼル酸化触媒を以下のように調製した:
単層DOCを以下のように調製した。硝酸白金及び硝酸パラジウムをシリカ−アルミナのスラリーに加えた。ベータゼオライトを、質量でゼオライトとして固形分の<30%を含むようにスラリーに加えた。先の実施例1の方法を用いて、ウォッシュコートスラリーを400cpsiフロースルー基材上に投与した。投与した部分を乾燥させ、次いで500℃でか焼した。ウォッシュコート被膜中の全白金族元素添加量は、60gft−3であり、全Pt:Pd重量比は4:1であった。1インチ(2.54cm)直径×3インチ(7.62cm)長のコアを完成品から切断した。得られた部品は、「フレッシュ」、すなわちエージングしていない、と表す。
単層DOCを以下のように調製した。硝酸白金及び硝酸パラジウムをシリカ−アルミナのスラリーに加えた。ベータゼオライトを、質量でゼオライトとして固形分の<30%を含むようにスラリーに加えた。DOC Aで使用したのと同じ方法を用いて、ウォッシュコートスラリーを400cpsiフロースルー基材上に投与した。投与した部分を乾燥させ、次いで500℃でか焼した。単層DOC中の全PGM添加量は、120g/ft3であり、Pt:Pd重量比は2:1であった。1インチ(2.54cm)直径×3インチ(7.62cm)長のコアを完成品から切断した。得られた部品は、「フレッシュ」、すなわちエージングしていない、と表す。
図1に例示されている第1の合成触媒活性試験(SCAT)実験室用反応器で試験を行った。この反応器内では、実施例10のコーティングしたCu/CHAゼオライトSCR触媒のエージングしたコアが、ディーゼル酸化触媒(DOC)A又はB(実施例11に基づく)のいずれかのコアの下流の導管に配されている。毎分6リットルの速度で合成ガス混合物を導管に通した。触媒出口温度900℃で2時間、定常状態の温度でDOC試料を加熱(又は「エージング」)するために炉を使用した。SCR触媒をDOC試料の下流に配置し、水冷熱交換器ジャケットも適宜使用できるが、炉の出口及びSCR入口の間のチューブの長さを調節することによってエージングプロセス中に触媒温度300℃で保持した。温度は、適切に配置した熱電対(T1及びT2)を用いて決定した。エージング中に使用したガス混合物は、40%空気、50%N2、10%H2Oであった。
全体から見て、実施例7及び8ならびに比較例2に関連して図4に示した実施例9の結果は、1:1と5:1の間のPt:Pd重量比が、触媒を含有する白金族元素から下流のSCR触媒への白金族元素、主に白金の揮発によるNOx転化活性低下の問題を低減するのに有益であることを示唆している。
Claims (23)
- 第1のウォッシュコート被膜と第2のウォッシュコート被膜を含む、リーンバーン内燃機関から排出された排気ガスを処理するのに使用するための触媒化基材モノリスであって、第1のウォッシュコート被膜は、少なくとも1種の白金族元素(PGM)と該少なくとも1種のPGMのための少なくとも1種の担体材料とを含む触媒組成物を含み、該第1のウォッシュコート被膜中の少なくとも1種のPGMは、比較的高温を含む比較的極限の条件に第1のウォッシュコート被膜を曝したときに、揮発しやすく、第2のウォッシュコート被膜は、揮発したPGMをトラップするための少なくとも1種の金属酸化物を含み、第2のウォッシュコート被膜は、第1のウォッシュコート被膜と接触した排気ガスと接触するように配向されている、触媒化基材モノリス。
- 第1のウォッシュコート被膜中の少なくとも1種のPGMは白金を含む、請求項1に記載の触媒化基材モノリス。
- 第1のウォッシュコート被膜中の少なくとも1種のPGMは、白金とパラジウムの両方を含む、請求項1又は2に記載の触媒化基材モノリス。
- Pt:Pdの重量比が≦2である、請求項3に記載の触媒化基材モノリス。
- 第2のウォッシュコート被膜の少なくとも1種の金属酸化物が、安定化されていてもよいアルミナ、非晶質シリカ−アルミナ、安定化されていてもよいジルコニア、セリア、チタニア、安定化されていてもよいセリア−ジルコニア混合酸化物、及びそれらの任意の2種以上の混合物からなる群から選択される金属酸化物を含む、請求項1、2、3又は4に記載の触媒化基材モノリス。
- 第2のウォッシュコート被膜が、パラジウム、銀、金及びそれらの任意の2種以上の組合せからなる群から選択される少なくとも1種の金属を含む触媒組成物を含み、少なくとも1種の金属酸化物が、少なくとも1種の金属を支持している、請求項1から5のいずれか一項に記載の触媒化基材モノリス。
- 第2のウォッシュコート被膜は、白金及びパラジウムを含み、第2のウォッシュコート被膜中のPt:Pdの重量比が、第1のウォッシュコート被膜中のPt:Pdの重量比よりも低い、請求項1から6のいずれか一項に記載の触媒化基材モノリス。
- 第1のウォッシュコート被膜が、基材モノリスの第1のウォッシュコートゾーンに配され、第2のウォッシュコートが、基材モノリスの第2のウォッシュコートゾーンに配され、第1のウォッシュコートゾーンと第2のウォッシュコートゾーンとの間に実質的に重なりがない、請求項1から請求項7のいずれか一項に記載の触媒化基材モノリス。
- 第2のウォッシュコート被膜が、第1のウォッシュコート被膜の上の層に配されている、請求項1から7のいずれか一項に記載の触媒化基材モノリス。
- 基材モノリスが、フロースルー基材モノリスである、請求項1から9のいずれか一項に記載の触媒化基材モノリス。
- 基材モノリスが、入口表面及び出口表面を有するフィルタリング基材モノリスであり、入口表面が、多孔質構造によって出口表面から分離されている、請求項1から9のいずれか一項に記載の触媒化基材モノリス。
- フィルタリング基材モノリスが、ウォールフローフィルターである、請求項11に記載の触媒化基材モノリス。
- 第1のウォッシュコート被膜が、基材モノリスの第1のウォッシュコートゾーンに配され、第2のウォッシュコート被膜が、基材モノリスの第2のウォッシュコートゾーンに配され、第1のウォッシュコートゾーンと第2のウォッシュコートゾーンとの間に実質的に重なりがなく、第1のウォッシュコートゾーンは、フィルタリング基材モノリスの入口表面を含み、第2のウォッシュコートゾーンは、フィルタリング基材モノリスの出口表面を含み、多孔質構造は、第1のウォッシュコートゾーンと第2のウォッシュコートゾーンとの間の移行の境界を定める、請求項11又は12に記載の触媒化基材モノリス。
- 少なくとも第1のウォッシュコート被膜が、酸化触媒又はNOx吸収触媒を含む、請求項1から13のいずれか一項に記載の触媒化基材モノリス。
- 請求項1から14のいずれか一項に記載の第1の触媒化基材モノリスを含む、リーンバーン内燃機関のための排気システム。
- 選択接触還元(SCR)触媒を含む第2の触媒化基材モノリスを含み、第2の触媒化基材モノリスが、第1の触媒化基材モノリスから下流に配されている、請求項15に記載の排気システム。
- 第1の触媒化基材モノリスと第2の触媒化基材モノリスの間で排気ガス中に窒素還元剤を導入するための導入管を含む、請求項16に記載の排気システム。
- 第3の触媒化基材モノリスを含み、第1の触媒化基材モノリスが、請求項11、12又は13に記載のフィルタリング基材モノリスであり、第3の触媒化基材モノリスが、酸化触媒又はNOx吸収触媒を含むフロースルー基材モノリスであり、第3の触媒化基材モノリスが、第1の触媒化基材モノリスの上流に配されている、請求項15、16又は17に記載の排気システム。
- 第3の基材モノリスを含み、第3の基材モノリスが、フィルタリング基材モノリスであり、第3の基材モノリスが、第2の触媒化基材モノリスの下流に配されている、請求項15、16又は17に記載の排気システム。
- 第3の基材モノリスが酸化触媒を含む、請求項19に記載の排気システム。
- 請求項15から20のいずれか一項に記載の排気システムを含む、特に車両用の、リーンバーン内燃機関。
- 請求項21に記載のリーンバーン内燃機関を備えた車両。
- 白金族元素(PGM)を含む触媒組成物が比較的高温を含む比較的極限条件に曝されたときに、少なくとも1種の担体材料上に担持された少なくとも1種のPGMを含みかつ選択接触還元(SCR)触媒の上流の基材モノリス上に配された触媒組成物から揮発し得るPGMによって、リーンバーン内燃機関の排気システム中のSCR触媒が、作用を阻害されることを低減又は防止する方法であって、揮発したPGMを、少なくとも1種の金属酸化物を含むウォッシュコート被膜中にトラップすることを含み、ウォッシュコート被膜は、PGMを含む触媒組成物と同じ基材モノリス上に配されている、方法。
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KR20190039979A (ko) * | 2016-08-12 | 2019-04-16 | 존슨 맛쎄이 퍼블릭 리미티드 컴파니 | 휘발화된 백금을 위한 포획 영역을 갖는 압축 점화 엔진용 배기 시스템 |
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