JP2005514551A - ディーゼルエンジンの排気から粒子状物質を除去するための排気系および方法 - Google Patents
ディーゼルエンジンの排気から粒子状物質を除去するための排気系および方法 Download PDFInfo
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- JP2005514551A JP2005514551A JP2003556648A JP2003556648A JP2005514551A JP 2005514551 A JP2005514551 A JP 2005514551A JP 2003556648 A JP2003556648 A JP 2003556648A JP 2003556648 A JP2003556648 A JP 2003556648A JP 2005514551 A JP2005514551 A JP 2005514551A
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- JP
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- Prior art keywords
- zeolite
- exhaust system
- soot filter
- soot
- exhaust
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
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Images
Classifications
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F01—MACHINES OR ENGINES IN GENERAL; ENGINE PLANTS IN GENERAL; STEAM ENGINES
- F01N—GAS-FLOW SILENCERS OR EXHAUST APPARATUS FOR MACHINES OR ENGINES IN GENERAL; GAS-FLOW SILENCERS OR EXHAUST APPARATUS FOR INTERNAL COMBUSTION ENGINES
- F01N3/00—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust
- F01N3/08—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for rendering innocuous
- F01N3/0807—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for rendering innocuous by using absorbents or adsorbents
- F01N3/0828—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for rendering innocuous by using absorbents or adsorbents characterised by the absorbed or adsorbed substances
- F01N3/0835—Hydrocarbons
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F01—MACHINES OR ENGINES IN GENERAL; ENGINE PLANTS IN GENERAL; STEAM ENGINES
- F01N—GAS-FLOW SILENCERS OR EXHAUST APPARATUS FOR MACHINES OR ENGINES IN GENERAL; GAS-FLOW SILENCERS OR EXHAUST APPARATUS FOR INTERNAL COMBUSTION ENGINES
- F01N3/00—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust
- F01N3/08—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for rendering innocuous
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/92—Chemical or biological purification of waste gases of engine exhaust gases
- B01D53/94—Chemical or biological purification of waste gases of engine exhaust gases by catalytic processes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/92—Chemical or biological purification of waste gases of engine exhaust gases
- B01D53/94—Chemical or biological purification of waste gases of engine exhaust gases by catalytic processes
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Abstract
Description
本明細書の目的に対し下記の言葉はそれぞれ下記に示す意味をもつものとする。
実施例1
下記の一般的な方法を用いて低温NO2捕捉材料をつくった。約300gの水の中で交換すべき金属を含んだ金属塩の溶液をつくり、対応するゼオライトに予め定められた量の金属が与えられるようにした。次いで100gのアンモニウム形のゼオライトをこの金属塩溶液に加え、周囲条件下で2時間撹拌した。2時間後予め定められた量の水酸化アンモニウム溶液を加えて溶液(pH約8〜9)中の過剰の金属を沈澱させた。次いで交換されたゼオライトを濾過して取り出し、約500mLの水で洗滌した。次いで約10gのアルミナを結合剤として用い濾液をスラリにした。
実施例2
ここでゼオライト・捕捉材料に対する試験条件を一般的に説明する。直径が0.5インチ、長さが1インチのハニカム形の担体を石英の反応器の中にきっちりと詰め込み、この中に通常は室温において全流量約1〜15L/分でガス供給流を導入し、約30,000〜45,000/時間のGHSVを得た。供給流のガスの組成は典型的には250ppmのNO2、トルエンまたはプロピレンとしての1000ppmのCl、20ppmのSO2、1.5%の水、5%のO2を含み、残りはN2であった。水の濃度は使用した方法に依存し、各実施例で示すことにする。1.5%の水を得るために室温に保った1Lの容器の中に空気を泡立たせて通し、完全に飽和させた(湿度100%)。供給流中の10%の水蒸気は注入ポンプを用いて得た。出口ガス流中のNOxの検出はケミルミネッセンス法を用いて行った。供給されたNOxの量に関してNO2の消失率を測定した。((NOxin−NOxout/NOxin)×100)。
実施例3
EST−10は珪酸チタン型のモレキュラー・シーブであり、その製造法は米国特許第4,853,202号明細書および米国特許第5,244,650号明細書に記載されている。これらの特許は引用により本明細書に包含される。これらは細孔が大きいモレキュラー・シーブである。図7は、3重量%のMnと交換したEST−10捕捉材料(Mn/ETS−10)を被覆したハニカム担体をNO2を含むガス流中に入れ、時間の経過と共に得たNO2の貯蔵および放出特性を示す。ガス供給流は水で飽和した空気(水約1.5%)、250ppmのNO2、1000ppmのトルエン、20ppmのSO2、15%のO2を含み、残りはN2であった。。このガス供給流を約30℃において反応器に導入した。ガス供給流の温度を周囲温度(約25℃)から約450℃まで13℃/分の速度で30分に亙って上昇した。図7においては、左側の縦軸はNOxおよびトルエンの消失率に対応しており、右側の縦軸は入口温度に対応し、横軸は分単位の時間に対応している。実線の曲線は入口温度を表し、正方形を含む曲線はNOxを、円を含む曲線はトルエンを表す。
実施例4
実施例1に記載したようにして3%Co3%Mn/ETS−10材料をつくり、モノリス担体の上に被覆した。試験ガス組成物は水を飽和した空気(水約1.5%)、250ppmのNO2、1000ppmのトルエン、20ppmのSO2、15%のO2を含み、残りはN2であった。ガス供給流の空間速度は30,000/時間であった。
実施例5
実施例1に従って3%Mn/Y−ゼオライト・捕捉材料を被覆したモノリス担体をつくった。ハニカム型の基質に被覆した3%Mn/Y−ゼオライト・捕捉材料の捕捉および放出の効率を周囲温度(25℃)から450℃まで検査し、得られた結果を図11に示す。供給ガスは250ppmのNO2、333ppmのプロピレン、25ppmのSO2、10%の水蒸気、12%のO2を含み、残りはN2であった。空間速度は25,000/時間であった。供給ガスの入口温度を13℃/分の割合で周囲温度から450℃まで上昇させた。図11においては、左側の縦軸はNOxおよびプロピレンの消失率に対応しており、右側の縦軸は入口温度(℃)に対応し、横軸は時間(分)に対応している。実線の曲線は入口温度を表し、円を含む曲線はNO2を表し、逆三角形を含む曲線はプロピレンを表す。
実施例6
低温NO2捕捉材料および放出されたNO2で基質を酸化するのに有効なリーンNOx触媒組成物の両方を含む系の効果を例証するために、二つのモノリス担体を含む系の性能を決定した。この実験においては、10%Mn/Yゼオライト組成物を被覆したモノリス担体を、白金と交換したZSM−5ゼオライト材料(Pt/ZSM−5材料と呼ぶ)のウォッシュコート組成物で被覆した第2のモノリス担体の上流に配置した。Pt/ZSM−5触媒は次のようにしてつくった。アミンで可溶化したモノエタノールアミン白金錯体(MEA)xPt(OH)6としての水酸化白金11.7gを水で希釈して溶液の全重量を156gにした。ZSM−5を加え、約30分間混合した。15gの酢酸および30.29gのシリカゾル(Nalco 1056)を結合剤として加えた。スラリの粒子の90%の粒径が10μよりも小さくなるまで、スラリをボールミルで処理した。寸法が0.5×1.0インチのセラミックスの基質にこのスラリを被覆し、2回の被覆で約2g/立方インチの被覆率が得られるようにし、被覆の間において乾燥およびカ焼を行った。次いで被覆した触媒を乾燥し、550℃で2時間カ焼した。
Claims (24)
- 煤フィルター;および
該煤フィルターの上流にあってそれと連なっている担体の上に沈澱した低温NO2捕捉材料
を含んで成ることを特徴とするディーゼルエンジン排気系。 - 該排気系は沈澱したNO2捕捉材料をもつ担体の上流にあるディーゼル酸化触媒をさらに含んで成ることを特徴とする請求項1記載の排気系。
- 煤フィルター;および
酸性ゼオライトおよび卑金属と交換されたゼオライトから成る群から選ばれるゼオライトを含む低温NO2捕捉材料を含んで成るディーゼルエンジン排気系であって、該低温NO2捕捉材料は該煤フィルターの上流にあってそれと連なっている担体の上に沈澱していることを特徴とするディーゼルエンジン排気系。 - ゼオライトはZSM−5,ETS−10、Yゼオライト、βゼオライト、フェリエライト、モルデナイト、珪酸チタン、および燐酸アルミニウムから成る群から選ばれることを特徴とする請求項3記載の排気系。
- 卑金属はMn、Cu、Fe、Co、W、Re、Sn、Ag、Zn、Mg、Li、Na、K、Cs、Nd、Prおよびこれらの組み合わせから成る群から選ばれることを特徴とする請求項3記載の排気系。
- ゼオライトはSiと組み合わされて酸化物の骨格をつくる3価の金属を含んで成ることを特徴とする請求項3記載の排気系。
- 3価の金属はAl、B、Ga、In、Fe、Cr、V、AsおよびSbから成る群から選ばれる少なくとも1種の金属を含んで成ることを特徴とする請求項6記載の排気系。
- ゼオライトは、最小断面寸法の細孔の開口部が少なくとも5Åであり珪素対アルミナの比が少なくとも5であることによって特徴付けられる三次元のアルミナ−シリケート・ゼオライトを含んで成ることを特徴とする請求項6記載の排気系。
- ゼオライトは珪酸チタンを含んで成ることを特徴とする請求項6記載の排気系。
- 煤フィルターの上流にあるディーゼル酸化触媒をさらに含んで成ることを特徴とする請求項3記載の排気系。
- NO2捕捉材料はディーゼル酸化触媒と煤フィルターとの間に介在してそれと連なっている担体の上に沈澱していることを特徴とする請求項10記載の排気系。
- さらにカニスターを具備し、該カニスターは低温NO2捕捉材料および煤フィルターの両方を収納していることを特徴とする請求項11記載の排気系。
- 煤フィルターは上流の軸の端と下流の軸の端を有するセラミックスのモノリス構造を含んで成り、該構造はマクロ多孔質の壁をもつ平行な流体の通路を有し、上流の軸の端の所に開口部をもつ通路は下流の軸の端の所で閉じており、下流の軸の端の所に開口部をもつ通路は上流の軸の端の所で閉じており、これによって通路の壁の上流側および下流側が規定されていることを特徴とする請求項3記載の排気系。
- 触媒組成物は煤フィルターの通路の壁の下流側に沈澱していることを特徴とする請求項13記載の排気系。
- 煤フィルターの通路の壁の下流側に沈澱している触媒組成物はリーンNOx触媒組成物を含んで成ることを特徴とする請求項14記載の排気系。
- 煤フィルターの通路の壁の下流側に沈澱している触媒組成物は未燃焼の炭化水素および一酸化炭素の燃焼に有効な触媒組成物を含んで成ることを特徴とする請求項14記載の排気系。
- 排気流を請求項1記載の排気系に通し;
少なくとも若干のNO2を低温NO2捕捉材料に吸着させ、また少なくとも若干の煤を煤フィルターに吸着させ;
低温NO2捕捉材料を加熱して吸着されたNO2の少なくとも若干を低温NO2捕捉材料から脱着させ;
脱着したNO2を用いて少なくとも若干の吸着された煤を酸化する
ことを特徴とするNO2と煤とを含むディーゼル排気流を処理する方法。 - 煤フィルターおよび該煤フィルターの上流にある担体に沈澱した低温NO2捕捉材料を含んで成るディーゼルエンジン排気系に排気流を通し;
少なくとも若干のNO2を低温NO2捕捉材料に吸着させ、また少なくとも若干の未燃焼の炭化水素を低温NO2捕捉材料に吸着させ;
低温NO2捕捉材料を加熱して吸着されたNO2の少なくとも若干と未燃焼の炭化水素の少なくとも若干とを低温NO2捕捉材料から脱着させ;
脱着したNO2を用いて少なくとも若干の未燃焼の炭化水素を酸化する
ことを特徴とするNO2と未燃焼の炭化水素とを含むディーゼル排気流を処理する方法。 - 低温NO2捕捉材料は酸性ゼオライトおよび卑金属と交換されたゼオライトから成る群から選ばれるゼオライトを含んで成ることを特徴とする請求項18記載の方法。
- 排気系はさらに煤フィルターの上に沈澱したリーンNOx触媒を含んで成ることを特徴とする請求項18記載の方法。
- 入口ガス流を低温NO2捕捉材料に接触させ、少なくとも若干のNO2を捕捉材料に吸着させることを特徴とする入口ガス流からNO2を除去する方法。
- ゼオライトはZSM−5,フェリエライト、珪酸チタン、燐酸アルミニウム、ガロシリケートおよびボロシリケートから成る群から選ばれ、卑金属はMn、Cu、Fe、Co、W、Re、Sn、Ag、Zn、Mg、Li、Na、K、Cs、NdおよびPrから成る群から選ばれることを特徴とする卑金属と交換されたゼオライトを含んで成る組成物。
- ゼオライトは珪酸チタンであり、卑金属はMnおよびCoから成る群から選ばれることを特徴とする請求項22記載の組成物。
- ゼオライトがETS−10であることを特徴とする請求項23記載の組成物。
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2001
- 2001-12-21 US US10/032,200 patent/US6912847B2/en not_active Expired - Lifetime
-
2002
- 2002-12-11 AU AU2002362131A patent/AU2002362131A1/en not_active Abandoned
- 2002-12-11 WO PCT/US2002/039497 patent/WO2003056150A2/en active Application Filing
- 2002-12-11 EP EP02797265A patent/EP1456511A2/en not_active Withdrawn
- 2002-12-11 EP EP09075049A patent/EP2048115A3/en not_active Withdrawn
- 2002-12-11 KR KR10-2004-7009860A patent/KR20040077683A/ko active IP Right Grant
- 2002-12-11 JP JP2003556648A patent/JP2005514551A/ja active Pending
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JP2007245050A (ja) * | 2006-03-17 | 2007-09-27 | Toyota Central Res & Dev Lab Inc | 窒素酸化物吸着材、その製造方法、及びそれを用いた窒素酸化物の除去方法 |
JP2007291980A (ja) * | 2006-04-26 | 2007-11-08 | Hino Motors Ltd | 排気浄化装置 |
JP2007291981A (ja) * | 2006-04-26 | 2007-11-08 | Hino Motors Ltd | 排気浄化装置 |
WO2008133181A1 (ja) | 2007-04-20 | 2008-11-06 | Toyota Jidosha Kabushiki Kaisha | NOx 吸着材の製造方法及びNOx 吸着材 |
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US20030115859A1 (en) | 2003-06-26 |
AU2002362131A8 (en) | 2003-07-15 |
EP2048115A2 (en) | 2009-04-15 |
EP1456511A2 (en) | 2004-09-15 |
WO2003056150A3 (en) | 2003-12-04 |
US6912847B2 (en) | 2005-07-05 |
WO2003056150A2 (en) | 2003-07-10 |
AU2002362131A1 (en) | 2003-07-15 |
EP2048115A3 (en) | 2009-07-29 |
KR20040077683A (ko) | 2004-09-06 |
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