JP5063980B2 - 排ガス浄化触媒用複合酸化物およびフィルター - Google Patents
排ガス浄化触媒用複合酸化物およびフィルター Download PDFInfo
- Publication number
- JP5063980B2 JP5063980B2 JP2006288242A JP2006288242A JP5063980B2 JP 5063980 B2 JP5063980 B2 JP 5063980B2 JP 2006288242 A JP2006288242 A JP 2006288242A JP 2006288242 A JP2006288242 A JP 2006288242A JP 5063980 B2 JP5063980 B2 JP 5063980B2
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- Prior art keywords
- composite oxide
- exhaust gas
- gas purification
- purification catalyst
- catalyst
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- 239000003054 catalyst Substances 0.000 title claims description 53
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- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical group [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 28
- 229910052684 Cerium Inorganic materials 0.000 claims description 17
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 10
- 229910052747 lanthanoid Inorganic materials 0.000 claims description 10
- 150000002602 lanthanoids Chemical class 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 10
- 239000001301 oxygen Substances 0.000 claims description 10
- 229910052760 oxygen Inorganic materials 0.000 claims description 10
- 229910052777 Praseodymium Inorganic materials 0.000 claims description 9
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical group [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 claims description 9
- 229910052746 lanthanum Inorganic materials 0.000 claims description 9
- 238000002441 X-ray diffraction Methods 0.000 claims description 8
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- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 10
- 229910017604 nitric acid Inorganic materials 0.000 description 10
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- 229910004631 Ce(NO3)3.6H2O Inorganic materials 0.000 description 2
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- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 description 1
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- 206010037660 Pyrexia Diseases 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
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- 150000004703 alkoxides Chemical class 0.000 description 1
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- 239000007864 aqueous solution Substances 0.000 description 1
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- IXSUHTFXKKBBJP-UHFFFAOYSA-L azanide;platinum(2+);dinitrite Chemical compound [NH2-].[NH2-].[Pt+2].[O-]N=O.[O-]N=O IXSUHTFXKKBBJP-UHFFFAOYSA-L 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
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- JYYOBHFYCIDXHH-UHFFFAOYSA-N carbonic acid;hydrate Chemical compound O.OC(O)=O JYYOBHFYCIDXHH-UHFFFAOYSA-N 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 description 1
- 229910000420 cerium oxide Inorganic materials 0.000 description 1
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- QZRHHEURPZONJU-UHFFFAOYSA-N iron(2+) dinitrate nonahydrate Chemical compound O.O.O.O.O.O.O.O.O.[Fe+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O QZRHHEURPZONJU-UHFFFAOYSA-N 0.000 description 1
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- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 description 1
- GPNDARIEYHPYAY-UHFFFAOYSA-N palladium(ii) nitrate Chemical compound [Pd+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O GPNDARIEYHPYAY-UHFFFAOYSA-N 0.000 description 1
- 229910000027 potassium carbonate Inorganic materials 0.000 description 1
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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
- F01N3/02—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for cooling, or for removing solid constituents of, exhaust
- F01N3/021—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for cooling, or for removing solid constituents of, exhaust by means of filters
- F01N3/033—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for cooling, or for removing solid constituents of, exhaust by means of filters in combination with other devices
- F01N3/035—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for cooling, or for removing solid constituents of, exhaust by means of filters in combination with other devices with catalytic reactors, e.g. catalysed diesel particulate filters
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- B01D53/34—Chemical or biological purification of waste gases
- B01D53/92—Chemical or biological purification of waste gases of engine exhaust gases
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- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
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- B01J35/613—10-100 m2/g
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- C—CHEMISTRY; METALLURGY
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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
- F01N2330/00—Structure of catalyst support or particle filter
- F01N2330/06—Ceramic, e.g. monoliths
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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
- F01N2370/00—Selection of materials for exhaust purification
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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
- F01N2510/00—Surface coverings
- F01N2510/06—Surface coverings for exhaust purification, e.g. catalytic reaction
- F01N2510/065—Surface coverings for exhaust purification, e.g. catalytic reaction for reducing soot ignition temperature
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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
- F01N3/02—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for cooling, or for removing solid constituents of, exhaust
- F01N3/021—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for cooling, or for removing solid constituents of, exhaust by means of filters
- F01N3/023—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for cooling, or for removing solid constituents of, exhaust by means of filters using means for regenerating the filters, e.g. by burning trapped particles
- F01N3/0231—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for cooling, or for removing solid constituents of, exhaust by means of filters using means for regenerating the filters, e.g. by burning trapped particles using special exhaust apparatus upstream of the filter for producing nitrogen dioxide, e.g. for continuous filter regeneration systems [CRT]
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Description
また、高価な貴金属元素を使用しなくても高い触媒活性が得られ、この場合にはDPFの材料コストが低減される。他方、白金属元素を共存させた場合には触媒活性の一層の向上が期待される。
したがって本発明は、DPFを用いた排ガス浄化機構の長寿命化およびトータルコストの削減に寄与するものである
[a]Ce、Bi、Rのモル比をCe:Bi:R=(1−x−y):x:yとするとき、0<x≦0.4、0<y<1.0
[b]Ce、Bi、R、Zrのモル比をCe:Bi:R:Zr=(1−x−y−z):x:y:zとするとき、0<x≦0.4、0<y<1.0、0<z≦0.5
なお、複合酸化物の中には酸化セリウム構造体のCeを置換していないBi、R、あるいはZrが不純物相として存在する場合があり、本発明の効果が阻害されない限りその不純物相の存在は許容される。許容される量の不純物相が存在する場合は、不純物相中のCe、Bi、R、あるいはZrを含めた複合酸化物全体としてのモル比が上記[a]または[b]を満たしていればよい。
各実施例、比較例の複合酸化物を以下のようにして作製した。
〔実施例1、2〕
Ce源として硝酸セリウム六水和物(Ce(NO3)3・6H2O)、Bi源として硝酸ビスマス五水和物(Bi(NO3)3・5H2O)を用意した。一方、R源として希土類酸化物(実施例1:Pr酸化物、実施例2:Tb酸化物)の粉末を濃硝酸溶液に溶解し、Rの硝酸溶液を用意した。
Ce源、Bi源、R源は実施例1と同じものを用意し、さらにZr源としてオキシ硝酸ジルコニウム二水和物(ZrO(NO3)2・2H2O)を用意した。これらを、Ce、Bi、Pr、Zrのモル比が0.7:0.1:0.1:0.1となる配合割合で混合し、かつ混合硝酸溶液中のCe、Bi、R、Zrの合計が0.2mol/Lとなるように水を加えて原料溶液を得た。以下、実施例1と同様の工程および条件でCeとBiとPrとZrを主成分とする複合酸化物を得た。
Ce、Bi、Prのモル比を表2に示すように変更したこと以外、実施例1と同じ条件でCeとBiとPrを主成分とする複合酸化物を得た。
硝酸セリウム六水和物(Ce(NO3)3・6H2O)、硝酸ビスマス五水和物(Bi(NO3)3・5H2O)を、CeとBiのモル比が0.7:0.3になるように秤量し、これを硝酸溶液中に溶解させ、混合硝酸溶液中のCe、Biの合計が0.2mol/Lとなるように水を加えて原料溶液を得た。以下、実施例1と同様の工程および条件でCeとBiを主成分とする複合酸化物を得た。
硝酸セリウム六水和物(Ce(NO3)3・6H2O)、硝酸ビスマス五水和物(Bi(NO3)3・5H2O)、および硝酸鉄九水和物(Fe(NO3)3・9H2O)を、Ce、Bi、Feのモル比が0.6:0.3:0.1になるように秤量し、これを硝酸溶液中に溶解させ、混合硝酸溶液中のCe、Bi、Fe合計が0.2mol/Lとなるように水を加えて原料溶液を得た。以下、実施例1と同様の工程および条件でCeとBiとFeを主成分とする複合酸化物を得た。
硝酸セリウム六水和物(Ce(NO3)3・6H2O)、硝酸ビスマス五水和物(Bi(NO3)3・5H2O)、およびオキシ硝酸ジルコニウム二水和物(ZrO(NO3)2・2H2O)を、Ce、Bi、Zrのモル比が0.6:0.3:0.1になるように秤量し、これを硝酸溶液中に溶解させ、混合硝酸溶液中のCe、Bi、Zr合計が0.2mol/Lとなるように水を加えて原料溶液を得た。以下、実施例1と同様の工程および条件でCeとBiとZrを主成分とする複合酸化物を得た。
得られた複合酸化物の耐熱性を評価するために、各複合酸化物の一部を、電気炉により空気中800℃で100時間にわたって熱処理(耐熱処理)した。
各実施例、比較例で得られた耐熱処理前の試料(800℃×2hと表示)、および上記耐熱処理後の試料(800℃×100hと表示)について、メノウ乳鉢で解粒し、粉末とした後、BET法により比表面積を求めた。測定はユアサイオニクス製の4ソーブUSを用いて行った。
各実施例、比較例で得られた試料、および上記耐熱処理後の試料について、カーボンブラックとの混合粉を作り、その中の一部を規定量分取した上、TG/DTA装置を用いてカーボンブラック燃焼開始温度を求めることによってPM燃焼開始温度を評価した。具体的には以下のようにした。
各例で得られた耐熱処理前の試料および耐熱処理後の試料について、下記の条件でX線回折パターンを測定した。
・X線回折装置: 株式会社リガク製、RINT−2100
・測定範囲: 2θ=20〜70°
・スキャンスピード: 2.0°/min
・サンプリング幅: 0.02°
・管球: Co管球(Co−Kα線使用)
・管電圧: 40kV
・管電流: 30mA
実施例1〜3、比較例1〜3の複合酸化物について、添加元素モル比、比表面積、PM燃焼開始温度を表1に示す。
次に、前掲の実施例1の複合酸化物に白金族元素を担持させた。担持方法として、実施例10ではPt濃度8.49質量%のジニトロジアンミン白金硝酸溶液2.35gを、また実施例11ではPd濃度5.27質量%の硝酸パラジウム溶液3.8gを、それぞれ実施例1で得た複合酸化物20gに添加し、蒸発乾固させ、600℃で1時間焼成させる手法を用いた。このようにして得られた白金族元素担持複合酸化物について、実施例1と同様の手法で比表面積、耐熱処理前後のPM燃焼開始温度を調べた。結果を表3に示す。表3中には実施例1の結果を併記する。なお、実施例10および11の複合酸化物をICPで分析したところ、実施例10のPt含有量は1.0質量%、実施例10のPd含有量は1.0質量%であった。
Claims (10)
- Ce、Bi、R(ただしRはLa、Ceを除くランタノイドの1種以上)および酸素で構成され、Ce、Bi、Rのモル比をCe:Bi:R=(1−x−y):x:yとするとき、0<x≦0.4、および0<y<1.0を満たす組成を有し、BET比表面積が24.3〜36.2m 2 /gである排ガス浄化触媒用複合酸化物。
- Ce、Bi、R(ただしRはLa、Ceを除くランタノイドの1種以上)および酸素で構成され、Ce、Bi、Rのモル比をCe:Bi:R=(1−x−y):x:yとするとき、0<x≦0.4、および0<y≦0.5を満たす組成を有し、BET比表面積が24.3〜36.2m 2 /gである排ガス浄化触媒用複合酸化物。
- 前記組成がCe、Bi、R(ただしRはLa、Ceを除くランタノイドの1種以上)、Zrおよび酸素で構成され、Ce、Bi、R、Zrのモル比をCe:Bi:R:Zr=(1−x−y−z):x:y:zとするとき、0<x≦0.4、0<y<1.0、および0<z≦0.5である、請求項1に記載の排ガス浄化触媒用複合酸化物。
- 前記組成がCe、Bi、R(ただしRはLa、Ceを除くランタノイドの1種以上)、Zrおよび酸素で構成され、Ce、Bi、R、Zrのモル比をCe:Bi:R:Zr=(1−x−y−z):x:y:zとするとき、0<x≦0.4、0<y≦0.5、および0<z≦0.3である、請求項2に記載の排ガス浄化触媒用複合酸化物。
- 前記RとしてPr、Tbの1種または2種を含有する請求項1〜4のいずれかに記載の排ガス浄化触媒用複合酸化物。
- 当該複合酸化物は、蛍石型構造に対応するX線回折ピークを有するものである請求項1〜5のいずれかに記載の排ガス浄化触媒用複合酸化物。
- 白金族元素を含有する請求項1〜6のいずれかに記載の排ガス浄化触媒用複合酸化物。
- 請求項1〜7のいずれかに記載の複合酸化物を含む排ガス浄化触媒。
- 当該排ガス浄化触媒はPM燃焼触媒である請求項8に記載の排ガス浄化触媒。
- ディーゼルエンジン排ガス中のPMをトラップする多孔体フィルターであって、その多孔体中の、トラップされたPMと接触する部位に、請求項1〜7のいずれかに記載の複合酸化物を存在させたディーゼル排ガス浄化用フィルター。
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JP2006288242A JP5063980B2 (ja) | 2006-10-24 | 2006-10-24 | 排ガス浄化触媒用複合酸化物およびフィルター |
PCT/JP2007/070212 WO2008050642A1 (en) | 2006-10-24 | 2007-10-10 | Composite oxide for use as exhaust gas clean-up catalyst, and filter |
US12/312,034 US8071501B2 (en) | 2006-10-24 | 2007-10-10 | Composite oxide for use as exhaust gas purification catalyst and filter |
CN2007800397461A CN101528605B (zh) | 2006-10-24 | 2007-10-10 | 排气净化催化剂用复合氧化物及过滤器 |
EP07829946.8A EP2077253B1 (en) | 2006-10-24 | 2007-10-10 | Composite oxide for use as exhaust gas clean-up catalyst, and filter |
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EP2210861B1 (en) * | 2007-10-01 | 2012-08-08 | DOWA Electronics Materials Co., Ltd. | Diesel particulate filter |
KR101574553B1 (ko) * | 2008-04-23 | 2015-12-04 | 도와 일렉트로닉스 가부시키가이샤 | 배기가스 정화촉매용 복합산화물과 그 제조방법 및 배기가스 정화촉매용 도료와 디젤 배기가스 정화용 필터 |
JP5528040B2 (ja) * | 2008-10-03 | 2014-06-25 | Dowaエレクトロニクス株式会社 | 排ガス浄化触媒用複合酸化物とその製造方法および排ガス浄化触媒用塗料とディーゼル排ガス浄化用フィルタ |
JP5381008B2 (ja) * | 2008-10-17 | 2014-01-08 | マツダ株式会社 | パティキュレートフィルタ及びその製造方法 |
JP5287222B2 (ja) * | 2008-12-25 | 2013-09-11 | 日産自動車株式会社 | Pm酸化触媒、パティキュレートフィルタ及びpm酸化触媒の製造方法 |
JP5444755B2 (ja) * | 2009-02-24 | 2014-03-19 | 三菱化学株式会社 | 排ガス浄化用触媒 |
JP5564962B2 (ja) * | 2010-01-28 | 2014-08-06 | 三菱化学株式会社 | 排ガス浄化用フィルター |
US9114389B2 (en) | 2010-08-05 | 2015-08-25 | Dowa Electronics Materials Co., Ltd. | Method for producing catalyst composition, catalyst composition, diesel particulate filter using the same, and exhaust gas purification system |
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GB1284285A (en) * | 1968-10-05 | 1972-08-02 | Sumitomo Chemical Co | Process for selective methylation of phenols |
US3857899A (en) * | 1968-10-05 | 1974-12-31 | Sumitomo Chemical Co | Process for selective methylation of phenols |
FR2695574B1 (fr) * | 1992-09-15 | 1994-11-04 | Rhone Poulenc Chimie | Composition à base d'oxyde cérique, préparation et utilisation. |
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KR100569632B1 (ko) * | 1999-05-13 | 2006-04-10 | 가부시키가이샤 닛폰 쇼쿠바이 | 불포화 알데히드 및 불포화 카르복실산을 제조하기 위한촉매 및 이 촉매를 사용하여 불포화 알데히드 및 불포화카르복실산을 제조하기 위한 방법 |
US6585944B1 (en) * | 2000-10-17 | 2003-07-01 | Delphi Technologies, Inc. | Enhancement of the OSC properties of Ce-Zr based solid solutions |
JP4030740B2 (ja) * | 2001-10-11 | 2008-01-09 | ダイヤニトリックス株式会社 | アンモ酸化用触媒の製造方法 |
JP4345909B2 (ja) * | 2001-12-11 | 2009-10-14 | 吟也 足立 | 低温酸化還元能を有する複合酸化物とその製造方法 |
US20030186805A1 (en) | 2002-03-28 | 2003-10-02 | Vanderspurt Thomas Henry | Ceria-based mixed-metal oxide structure, including method of making and use |
JP2004113936A (ja) * | 2002-09-26 | 2004-04-15 | Toyota Central Res & Dev Lab Inc | 排ガス浄化用触媒とその使用方法 |
GB0304939D0 (en) * | 2003-03-05 | 2003-04-09 | Johnson Matthey Plc | Light-duty diesel engine and a particulate filter therefor |
JP2005162914A (ja) * | 2003-12-03 | 2005-06-23 | Nippon Shokubai Co Ltd | 紫外線遮断膜、紫外線遮断用金属酸化物粒子および紫外線遮断材料形成用組成物 |
WO2005085137A1 (ja) * | 2004-03-08 | 2005-09-15 | Anan Kasei Co., Ltd. | 複合酸化物 |
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JP2006159021A (ja) * | 2004-12-03 | 2006-06-22 | Toyota Motor Corp | 排ガス浄化用触媒 |
JP4716087B2 (ja) * | 2005-02-18 | 2011-07-06 | トヨタ自動車株式会社 | 排ガス浄化用触媒 |
EP2210861B1 (en) * | 2007-10-01 | 2012-08-08 | DOWA Electronics Materials Co., Ltd. | Diesel particulate filter |
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WO2008050642A1 (en) | 2008-05-02 |
EP2077253A4 (en) | 2014-09-10 |
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CN101528605A (zh) | 2009-09-09 |
US8071501B2 (en) | 2011-12-06 |
EP2077253B1 (en) | 2017-10-04 |
EP2077253A1 (en) | 2009-07-08 |
US20100111778A1 (en) | 2010-05-06 |
JP2008105871A (ja) | 2008-05-08 |
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