JP5137401B2 - Nsr及びscr触媒を有する放出ガス処理システム - Google Patents
Nsr及びscr触媒を有する放出ガス処理システム Download PDFInfo
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- JP5137401B2 JP5137401B2 JP2006538478A JP2006538478A JP5137401B2 JP 5137401 B2 JP5137401 B2 JP 5137401B2 JP 2006538478 A JP2006538478 A JP 2006538478A JP 2006538478 A JP2006538478 A JP 2006538478A JP 5137401 B2 JP5137401 B2 JP 5137401B2
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Description
NO+1/2O2 →NO2 (1)
NOxの硝酸塩としての貯蔵
2NO2+MCO3+1/2O2→M(NO3)2+CO2 (2)
NOxの放出
M(NO3)2+2CO→MCO3+NO2+NO+CO2 (3)
NOxのN2 への還元
NO2+CO→NO+CO2 (4)
2NO+2CO→N2+2CO2 (5)
式2及び3において、Mは2価の金属カチオンを表す。Mは式が再バランスを必要とする場合には1または3価の金属化合物であってもよい。
2NO+5CO+3H2O→2NH3+5CO2 (6)
このNSR触媒の性質は、それ自体有毒な成分であるNH3が排気ガスの大気放出に先立って無毒な種へ転化されねばならないことを要求する。
(a)NOxを含んでなる排気ガスを、白金族金属成分及び少なくとも0.0061g/mlのNOx吸収剤を耐火性金属酸化物上に分散させて含んでなるNOx貯蔵還元(NSR)触媒と可燃性成分の希薄な期間接触させて、排気ガスからのNOxの一部を吸収させ、そしてこのNOxの一部を未処理のNSR触媒中に流通させ、
(b)排気ガス流の空気/燃料比を周期的に変えて可燃性成分の濃厚な期間中に可燃性成分の濃厚なガス流を供給し、
(c)この可燃性成分の濃厚なガス流をNSR触媒と接触させて、吸収されたNOxをNH3に還元し、そして
(d)続いてこのNH3と排気ガス中の未処理のNOxの混合物をSCR触媒と接触させてN2を生成させる、
ことを含む。
定義
次の術語は、本明細書の目的のために、それぞれ以下に示す意味を有する。
本発明のシステムで使用されるNSR触媒組成物は、耐火性金属酸化物担体上に分散されたNOx吸収剤及び白金族金属成分を含む。更にNSR組成物は、随時他の成分、例えば濃厚な運転期間中に生成するNH3 の量に著しく影響する酸素貯蔵成分及び鉄成分を含む。そのような組成物は、引用により本明細書に包含される2003年1月31日付けの出願米国特許願第10/355779号に開示されているものと同様である。そのようなNSR組成物は100−600℃の排気ガス温度、より特定的には150−450℃の排気ガス温度において良好なNOx貯蔵/NOx還元活性を示す。更にそのようなNSR触媒組成物は際立った熱安定性と硫黄化合物を適度な条件下に除去する能力を示す。
放出ガス処理システムは多くの公知のSCR触媒を用いて、NSR触媒の下流でNOxを処理することができる。例えば卑金属(例えば銅、鉄)で交換されたゼオライト組成物またはバナジアに基づく組成物(例えばV2O5/WO3/TiO2/SiO2)を用いてSCR触媒を生成させることができる。このSCR触媒は自己支持性触媒粒子の形でまたはSCR触媒組成物のハニカムモノリス形であってよい。しかしながら本発明の好適な具体例において、NSR触媒組成物はウォッシュコ−トとしてまたはウォッシュコ−トの組み合わせとしてセラミックまたは金属基材、好ましくはハニカム流通基材上に配置される。
好ましくは、NSR及びSCR触媒組成物のそれぞれは基材上に配置される。この基材は触媒の製造に典型的に使用される材料のいずれであってよく、好ましくはセラミックまたは金属ハニカム構造を含んでなる。通路が全体にわたって流体の流れに対し開かれている(ハニカム流通基材として言及)いずれか適当な基材、例えば基材の入口または出口面から全体に延びる細い平行なガス流通路を有する種類のモノリス型基材が使用しうる。流体の入口から流体の出口まで本質的に真っ直ぐな通路を有する通路は、通路を流れるガスが触媒物質と接触するように、触媒物質がウォッシュコ−トとして被覆されている壁によって規制される。モノリス型基材の流通路は、いかなる適当な断面積及び形、例えば台形、長方形、正方形、シヌソイド形、6角形、楕円形、円形などであってよい薄壁路である。そのような構造は断面積平方インチ当たり約60−約300もしくはそれ以上のガス入口開口(即ちセル)を含み得る。
図1Aに示すような放出ガス処理システムは単独で使用でき、随時そのシステムは図1Bのシステム10Bで示されるように、NSR触媒2の上流に及び/またはSCR触媒3の下流(4Bとして)にジ−ゼル酸化(DOC)触媒4Aを含むことができる。DOC組成物は技術的によく知られており、卑金属(例えばセリア)及び/または白金族金属を触媒試剤として含んでなってよい。
触媒A
基材はコ−ディエライトからなった。底部層は白金75g/0.028m 3 、BaO 0.0256g/ml 、ZrO2 0.00305g/ml、及びCeO2被覆のAl2O3からなる担体0.111g/mlからなった。この担体は初期湿式技術で製造し、CeO2 10重量%をAl2 O3の表面上に配置せしめた。担体材料を、アミン可溶化水酸化白金を含浸させて、所望の装填を達成した。次いで粒子の90%が10ミクロン以下の粒径(即ちd90<10μ)を有して、それにより高固体スラリ−が得られるように、粉末を水の存在下にミル処理した。このミル処理中、水に溶解した酢酸バリウム及び酢酸ジルコニルも添加した。
触媒Bは次のように製造した2層触媒複合物である。基材はコ−ディエライトであった。底部層は白金75g/0.028m 3 、BaO 0.0256g/ml、ZrO2 0.00305g/ml、及びTiO2被覆のAl2O3からなる担体0.111g/mlからなった。この担体を化学的蒸着法で製造し、TiO2 10重量%をAl2O3の表面上に堆積せしめた。この担体材料に、アミン可溶化水酸化白金を含浸させて、所望の装填を達成した。次いで粒子の90%が10ミクロン以下の粒径(即ちd90<10μ)を有して、それにより高固体スラリ−が得られるように、粉末を水の存在下にミル処理した。このミル処理中、水に溶解した酢酸バリウム及び酢酸ジルコニルの溶液も添加した。
触媒Cは単層触媒複合物であり、即ち1つの層だけをコ−ディエライト基材上に付着させた。単一層は、触媒Aに対する層で上述したのと同一の方法で製造した。この単一層は白金150g/0.028m 3、BaO 0.0244g/ml、Fe2O3 0.0122g/ml、及びAl2O3担体0.146g/mlからなった。複合物は硝酸鉄、酢酸バリウム及びアミン可溶化水酸化白金を用いて、担体に連続含浸させて製造した。
触媒の希薄なエ−ジングは、触媒を入口温度700℃で4時間、時間空間速度30,000時−1下に空気/水蒸気(水蒸気10%)流に露呈することにより行った。
本実施例では、NOx転化、NH3及びN2生成を、濃厚なパルス(即ち濃厚なガス流)におけるCO濃度の関数として決定した。先ず一連の配置において触媒Aを上流基材として及び下流の基材としてモノリス基材を通流するブランク流を有するシステムを用いてこれらの決定を行った。このシステムはここでは「システムI]と言及する。
本実施例において、NOx転化率、NH3及びN2生成を、濃厚な供給物タイミング(timing)の関数として決定した。先ずこの決定は、システムI及びシステムIIの両方を用いて行った。システムI及びシステムIIは、実施例2に記述してある。
本実施例において、NOx転化率、NH3 及びN2 生成を、化学量論点附近の濃厚な供給物を用いて決定した。この決定は、実施例2に記述してあるシステムI及びシステムIIの両方を用いて行った。
本実施例において、NH3 生成を、3つのNSR触媒、触媒A、B及びC、間で同一の条件下に比較した。性能試験は希薄な及び濃厚な供給物を、希薄な期間50秒及び濃厚な期間5秒で交互にして行なった。希薄な供給物はO2 10%、H2O 10%、CO2 5%、及びNO500ppmからなった。濃厚な供給物は、O2 1%、H2O 10%、CO2 5%、NO 500ppm、及びCO4%からなった。濃厚な供給物に対するλは約0.94であった。システムは、200、250、300、350、及び450℃でGHSV30,000時−1で評価した。性能が一定の温度で安定化するや、10分間データを取った。NO及びNO2 濃度(及びそれゆえにNOx濃度)及びNH3生成をフ−リエ変換赤外分光法(FTIR)で決定した。触媒の下流のNOx濃度を、システムの上流のそれと比較した。NOx濃度の相対的消失、NH3及びN2の生成をパ−セントで表し、データ捕収期間を通して1/秒で計算した。
Claims (14)
- NOx吸収剤を少なくとも0.0061g/ml(0.1g/in3)の濃度で且つ白金族金属成分を耐火性金属酸化物担体上に分散させて含んでなるNOx貯蔵還元(NSR)触媒,及び
該NSR触媒の下流に配置されたSCR触媒、
を含んでなり、但し該NSR触媒がセリウム及びプラセオジムの酸化物1つまたはそれ以上からの酸素貯蔵成分を更に含んでなり、酸素貯蔵成分が0.0305g/ml(0.5g/in3)未満であり、白金族金属成分がロジウムを含んでなる、排気ガス流のための放出ガス処理システム。 - NSR触媒の白金族金属成分が白金、パラジウム、ロジウム成分及びそれらの混合物からなる群から選択される、請求項1の放出ガス処理システム。
- 酸素貯蔵成分がセリアである、請求項1の放出ガス処理システム。
- NOx吸収剤がリチウム、ナトリウム、カリウム、セシウム、マグネシウム、カルシウム、ストロンチウム、バリウム、ランタン、及びネオジムの酸化物から選択される少なくとも1つの金属酸化物である、請求項1の放出ガス処理システム。
- SCR触媒がゼオライト成分、V2O5、WO3及びTiO2からなる群から選択される少なくとも1つの成分を含んでなる、請求項1の放出ガス処理システム。
- SCR触媒が鉄及び銅からなる群から選択されたイオンでイオン交換されたゼオライトを含んでなる、請求項1の放出ガス処理システム。
- NSR触媒成分が基材上に配置された少なくとも2つの触媒層を含んでなる、請求項1の放出ガス処理システム。
- NSR触媒成分が基材上に堆積された単一の触媒層である、請求項1の放出ガス処理システム。
- 上流ジ−ゼル酸化触媒をNSR触媒の上流に及び/または下流酸化触媒をSCR触媒の下流に更に含んでなる、請求項1の放出ガス処理システム。
- すすフィルターがNSRの上流にまたはNSR触媒とSCR触媒の間に配置されている、請求項1の放出ガス処理システム。
- NSR触媒及びSCR触媒の少なくとも1つがすすフィルター上に配置されている請求項1の放出ガス処理システム。
- 上流ジ−ゼル酸化触媒がNSR触媒の上流のすすフィルター上に配置され及び/または下流酸化触媒がSCR触媒の下流のすすフィルター上に配置されている、請求項11の放出ガス処理システム。
- すすフィルターが入口端、出口端、及び入口端から出口端まで延び且つ開放された入口と閉鎖された出口を有する入口チャンネル及び開放された出口と閉鎖された入口を有する出口チャンネルを含んでなる交互のチャンネルを持つ入口チャンネル側及び出口チャンネル側を含んでなる複数の通路を規定する内壁を含んでなる壁流フィルターであり、こゝでNSR触媒が入口チャンネル側に配置され、SCR触媒が出口チャンネル側に配置され、且つNSR触媒が開放された入口から閉鎖された出口へ向かう距離の少なくとも一部分に対して入口端から延び、そしてSCR触媒が開放された出口から閉鎖された出口へ向かう距離の少なくとも一部分に対して出口端から延びる、請求項12の放出ガス処理システム。
- (a)NOxを含んでなる排気ガスを、ロジウムを含んで成る白金族金属成分及びアルカリ土類金属酸化物からなる群から選択される少なくとも0.0061g/ml(0.1g/in3)のNOx吸収剤を耐火性金属酸化物担体上に分散させて含んでなるNOx貯蔵還元(NSR)触媒と可燃性成分の希薄な期間接触させて、排気ガスからのNOxの一部をアルカリ土類金属硝酸塩の形で吸収させ、そしてこのNOxの一部を未処理のNSR触媒中に流通させ、
(b)排気ガス流の空気/燃料比を周期的に変えて可燃性成分の濃厚な期間中可燃性成分の濃厚なガス流を供給し、
(c)この可燃性成分の濃厚なガス流をNSR触媒と接触させて、吸収されたNOxをNH3へ還元し、そして
(d)続いてこのNH3と排気ガス中の未処理のNOxの混合物をSCR触媒と接触させてN2を生成させ、但し該NSR及びSCRの少なくとも1つがセリウム及びプラセオジムの酸化物1つまたはそれ以上からの酸素貯蔵成分を更に含んでなり、酸素貯蔵成分が0.0305g/ml(0.5g/in3)未満である、
ジ−ゼルエンジンまたは可燃性成分の希薄な燃焼のガソリンエンジンからの排気ガス中のNOxをN2へ転化する方法。
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- 2004-11-04 EP EP04800722.3A patent/EP1687514B1/en active Active
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US7919051B2 (en) | 2011-04-05 |
EP1687514B1 (en) | 2019-05-08 |
US7490464B2 (en) | 2009-02-17 |
KR101165864B1 (ko) | 2012-07-13 |
KR20060107757A (ko) | 2006-10-16 |
WO2005047663A2 (en) | 2005-05-26 |
WO2005047663A3 (en) | 2005-06-23 |
JP5464620B2 (ja) | 2014-04-09 |
PL1687514T3 (pl) | 2019-10-31 |
US20070269353A1 (en) | 2007-11-22 |
EP1687514A2 (en) | 2006-08-09 |
US20050129601A1 (en) | 2005-06-16 |
JP2013039566A (ja) | 2013-02-28 |
JP2007527314A (ja) | 2007-09-27 |
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