JP2017538573A - 排気システム用の一酸化二窒素除去触媒 - Google Patents
排気システム用の一酸化二窒素除去触媒 Download PDFInfo
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- JP2017538573A JP2017538573A JP2017530688A JP2017530688A JP2017538573A JP 2017538573 A JP2017538573 A JP 2017538573A JP 2017530688 A JP2017530688 A JP 2017530688A JP 2017530688 A JP2017530688 A JP 2017530688A JP 2017538573 A JP2017538573 A JP 2017538573A
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- catalyst
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- ceria
- removal
- removal catalyst
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Images
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Abstract
Description
本発明は、内燃機関の排気システム用の浄化触媒、およびその使用方法に関する。より詳細には、本発明は、内燃機関の排気流の条件下での一酸化二窒素(N2O)の除去のために有効である、セリアを基礎とする担体に担持されたロジウム(Rh)成分を含む触媒に関する。例えば、N2O除去触媒は、N2Oを窒素(N2)と酸素(O2)とに分解するため、および/またはN2Oを窒素と水および/または二酸化炭素(存在する還元剤に依存して)とに還元するために有効である。
一酸化二窒素(N2O)は、CO2の310倍の地球温暖化係数を示しかつ114年の大気中の寿命を示す温室効果ガスである。自動車の排気は、燃料の燃焼の副生成物として、および窒素酸化物(NOx)の接触還元により形成される副生成物としてのN2Oエミッションの1つの発生源である。N2Oは、従来型/化学量論的ガソリン車用のおよびガソリン直噴(GDI)型のガソリン車用の三元転化(TWC)触媒、ディーゼル酸化触媒(DOC)、触媒化スートフィルター(CSF)、リーンNOxトラップ(LNT)、NOxを尿素で還元する選択的接触還元(SCR)触媒、およびディーゼル車用の選択的アンモニア酸化触媒(AMOx)を含めた全ての主要な種類のエミッションコントロール触媒によって、遷移条件下で形成される。
本開示は、一般に、触媒組成物、およびこのような組成物を含む触媒製品を提供する。特に、このような組成物、および製品は、例えば、排気ガス流から一酸化二窒素(N2O)を削減するための触媒を含むことができる。理論上では、N2Oの削減は、N2Oの形成の最小化、またはN2Oを分解する触媒の使用により(例えば、N2Oを直接N2とO2とに転化することにより、および/またはN2OをN2およびH2Oおよび/またはCO2(還元剤に依存する)に転化することにより)達成することができる。有効なN2O触媒組成物および製品は、独立型の材料または構成要素として提供することができるか、または存在する触媒系に組み込むことができる。
この開示は、添付の図面との関連で、この開示の多様な実施態様の次の詳細な記載を考慮して、より完全に理解することができる。
本発明の多様な例示的な実施態様を説明する前に、本発明は、次の説明に記載された構成またはプロセス工程の詳細に限定されるものでないことが理解されるべきである。本発明は、他の実施態様が可能であり、かつ多様な方法で実行または実施することができる。ここでは、本発明は、特別な実施態様との関連で記載されているが、これらの実施態様は、単に本発明の原理および適用を例証しているにすぎないことが理解されるべきである。発明の精神および範囲から逸脱することなく本発明の方法および装置について多様な改良および変法を作り出すことができることは当業者に明白である。したがって、本発明は、添付された特許請求の範囲およびその均等の範囲内で改良および変法を含むことが意図される。
4NO+4NH3+O2 → 4N2+6H2O、
NO+NO2+2NH3 → 2N2+3H2O、
6NO2+8NH4 → 7N2+12H2O。
上述のように、一般的にここに開示された触媒組成物は、セリアを基礎とする担体上に(例えばセリアを基礎とする担体に含浸した)Rh成分を含む。「セリアを基礎とする担体」とは、セリアを少なくとも約50質量%含む材料(例えば、耐火金属酸化物担体材料)を意味する。特定の実施態様の場合に、セリアを基礎とする担体は、セリアを、(セリアを基礎とする担体の全質量を基準として)少なくとも約55質量%、少なくとも約60質量%、少なくとも約65質量%、少なくとも約70質量%、少なくとも約75質量%、少なくとも約80質量%、少なくとも約85質量%、少なくとも約90質量%、少なくとも約91質量%、少なくとも約92質量%、少なくとも約93質量%、少なくとも約94質量%、少なくとも約95質量%、少なくとも約96質量%、少なくとも約97質量%、少なくとも約98質量%、少なくとも約99質量%、少なくとも約99.9質量%含む。いくつかの実施態様の場合に、セリアを基礎とする担体は、セリアに加えてさらに、多様な金属酸化物(結果として混合金属酸化物複合体担体となる)を含んでいてよい。セリアを基礎とする担体中に含まれていてよい例示的な金属酸化物は、ジルコニア、ランタナ、イットリア、プラセオジミア、ネオジミア、サマリア、ガドリニア、または他の希土類金属酸化物を含む。
ロジウム成分と、本開示によるセリアを基礎とする担体を含むN2O触媒組成物は、一般に、ウォッシュコートの形で提供され、かつこのようなウォッシュコートは多様な技術により作製してよい。触媒組成物の製造は、一般に、粒子の形のセリアを基礎とする担体を、ロジウム試薬を含む溶液で含浸することを含む。ここで、この目的のために、「ロジウム試薬」の用語は、焼成またはその使用の際に、触媒活性形(すなわち、ロジウム成分)、通常では金属または金属酸化物(すなわち、ロジウムまたは酸化ロジウム)に分解されるかまたは転化されるロジウム含有化合物、塩、錯体などを意味する。
N2O + □ → N2O−□ (1)
N2O−□ → N2 + O−□ (2)
2O−□ → O2 + 2□ (3)
N2O + O−□ → N2 + O2 + □ (4)
1以上の実施態様の場合に、ここに開示されたN2O触媒組成物のための支持体は、自動車触媒の製造のために一般に使用される任意の材料から構成されていてよく、かつ一般に金属またはセラミックのハニカム構造を示す。この支持体は、一般に、N2O触媒組成物を含むウォッシュコートが施されかつ付着される複数の壁面を提供し、それにより、触媒組成物のためのキャリアとして機能する。触媒材料は、一般に、排気ガス適用のためにモノリス支持体のような支持体上に配置される。
Rh試薬/成分で含浸されたセリアを基礎とする担体粒子の形の、上述の触媒組成物を水と混合して、ここで上述の支持体の型のような触媒支持体を被覆するためにスラリーを形成する。この触媒粒子に加えてさらに、スラリーは、任意に、結合剤としてアルミナ、炭化水素(HC)貯蔵成分(例えば、ゼオライト)、水溶性または水分散性安定剤(例えば、酢酸バリウム)、助触媒(例えば、硝酸ランタン)、会合性増粘剤、および/または界面活性剤(アニオン性、カチオン性、非イオン性または両性の界面活性剤を含む)を含んでよい。
ここに開示されたような触媒は、多様なタイプの内燃機関の排気流の条件下で、排気ガス中の一酸化二窒素(N2O)の少なくとも一部を、窒素(N2)および酸素(O2)に分解するため、および/または排ガス中のN2Oの少なくとも一部を、N2、H2O、および/またはCO2(還元剤に依存する)に還元するために有効である。「少なくとも一部」とは、排気ガス流中の全N2Oのいくらかのパーセンテージが分解および/または還元されることを意味する。例えば、いくつかの実施態様の場合には、ガス流中の少なくとも約1質量%、少なくとも約2質量%、少なくとも約5質量%、少なくとも約10質量%、少なくとも約20質量%、少なくとも約30質量%、少なくとも約40質量%、少なくとも約50質量%、少なくとも約60質量%、少なくとも70質量%、少なくとも約80質量%、または少なくとも約90質量%の一酸化二窒素が、このような条件下で分解および/または還元される。この活性は、反応温度に依存することが留意される。
分解: 2N2O → 2N2+O2 (I)
還元:
N2O+H2 → N2+H2O (IIa)
N2O+HC → N2+CO2+H2O (IIb)
N2O+CO → N2+CO2 (IIc)
3N2O+2NH3 → 4N2+3H2O (IId)
本発明は、ここに記載されたN2O転化触媒組成物または製品が組み込まれたエミッション処理システムも提供する。本発明のN2O転化触媒組成物は、一般に、ディーゼル排気ガスエミッションの処理のために、1種以上の付加的構成要素を含む、組込型のエミッション処理システムにおいて使用される。このように、「排気流」、「エンジン排気流」、「排気ガス流」などの用語は、ここに記載されたようなエンジン排出物、ならびに1種以上の他の触媒システム構成要素の下流の排出物に関する。
多様な実施態様を以下に列挙する:以下に列挙された実施態様は、本発明の範囲に従って全ての態様および他の実施態様と組み合わせてよいことが理解されるであろう。
次の無限定の実施例は、本発明の多様な実施態様を説明するために提供される。これらの実施例のいずれにおいても、支持体はコーディエライトであった。
方法1.1. 硝酸Rh溶液を、所望のRh金属負荷量を達成するために、インシピエントウェットネス技術で粉末セリア担体に含浸させた。Rh含浸担体を、次いで、30%の固体を達するように脱イオン水中に分散させ、スラリーpHを、HNO3で4に調節した。生じたスラリーを粉砕し、攪拌しながら乾燥させた。乾燥したスラリーを、空気中で、500℃で2時間焼成し、次いで破砕し、反応器試験のために250〜500μmに篩別した。
表1は、かなりのCeO2担体材料について集められたBET表面積、細孔容積、平均細孔半径およびX線回折データ、ならびに得られたRh/CeO2に関して得られたH2昇温還元データを含むいくつかの物理的および化学的特性データをまとめる。全てのCeO2材料のエージングについての条件は、空気中10%のH2Oで、750℃で、20時間であった。試験したRh/CeO2触媒は、CeO2の質量に対して1%のRhを含む。
CeO2材料タイプおよび熱処理の効果を、実施例2に記載した担体を用いたRh/CeO2 1質量%の組成を示す多様なN2O触媒について分析した。表2は、製造された触媒粉末の一覧を提供する。
希土類(RE)金属酸化物で変性されたCeO2の効果を、1%Rh/−RE−CeO2の組成を示す多様なN2O分解触媒について分析した。表4は、製造された触媒粉末の一覧を提供する。
白金族または他の金属(ME)の添加により変性されたRh−CeO2の効果を、n%ME/1%Rh/CeO2の多様な組成を示す多様なN2O除去触媒について分析した。表6は、製造された触媒粉末の一覧を提供する。
N2O触媒複合体は、3.1による触媒を用いて製造した。硝酸Rh溶液を、所望のRh金属負荷量を達成するために、インシピエントウェットネス技術によって粉末担体(CeO2)に含浸した。生じる粉末を、110℃で5時間乾燥し、次いで、触媒材料を形成するために、550℃で2時間焼成し、その一部を試験のために確保した。
比較のN2O触媒複合体を、アルミナ(Al2O3)上のRhを用いて製造した。硝酸Rh溶液を、所望のRh金属負荷量を達成するために、インシピエントウェットネス技術で粉末担体(Al2O3)に含浸した。得られた粉末を、110℃で5時間乾燥し、次いで550℃で2時間焼成した。次いで、焼成した粉末を水中に分散させ、連続式ミル中でD90<12μm(90%の粒子が、12μm未満の直径を示す)にまで粉砕した。スラリーのpHを、酢酸を用いてpH=5に調節し、かつスラリーの固体含有率は、約37%であった。600セル/in2のセル密度および0.10mmの壁厚を示すモノリス支持体を、数秒間スラリー中に浸漬した。圧縮空気を被覆されたモノリスに吹き通して、過剰の被覆を除去した。被覆された試料を、流通空気中で約200℃で20分間乾燥させ、次いで、550℃で2時間焼成した。焼成後の試料は、35g/ft3のRhおよび2g/in3の担体(Al2O3)を含む。
実施例6〜7の触媒材料/焼成粉末を、N2O分解活性について、高処理量反応器中で試験した。
実施例6〜7のモノリス触媒を、次のように試験した。N2O分解活性を、実験室用、定常状態流通式反応器で、GHSV=30,000h-1で測定した。試料は、電気炉の後端部に置かれた1インチ(直径)×1インチ(長さ)のモノリスコアであった。基本反応供給物は、N2O 200ppm、CO2 5質量%、および平衡N2を含む。別の試験では、O2 5質量%またはO2 5質量%+H2O 5体積%を、基本供給物にそれぞれ添加した。活性は、15℃/minの上昇速度での温度上昇で200℃〜500℃で測定した。流出ガス組成は、MKS FTIR Analyzer(モデル2030DGB2EVS13T)により、1Hzの採取速度で測定した。各試料を、新規の試料(そのまま)およびエージングした(空気中10体積%H2Oで、750℃で20時間)試料として試験した。
Claims (34)
- 内燃機関の排気流用の一酸化二窒素(N2O)除去触媒複合体において、N2O除去触媒材料を支持体上に含み、前記触媒材料は、セリアを基礎とする担体上に担持されたロジウム(Rh)成分を含み、前記触媒材料は、水素昇温還元(H2−TPR)により測定して、約100℃以下のH2消費ピークを示し、かつ排気流中で一酸化二窒素(N2O)の少なくとも一部を窒素(N2)および酸素(O2)に分解するために有効であるか、または排気流の条件下で、N2Oの少なくとも一部を、N2および水、N2および二酸化炭素(CO2)、またはN2、水、およびCO2に還元するために有効である、内燃機関の排気流用の一酸化二窒素(N2O)除去触媒複合体。
- 空気中10体積%の水で、750℃で、20時間のエージングの後のH2消費ピークは、新規の触媒材料のH2消費ピークの温度よりも低い温度で生じる、請求項1記載のN2O除去触媒複合体。
- 10体積%の水で、750℃で、20時間のエージングの後の前記触媒材料のN2O除去活性は、新規の触媒材料のN2O除去活性よりも高い、請求項1記載のN2O除去触媒複合体。
- 前記セリアを基礎とする担体は、空気中10質量%の水で、750℃で、20時間のエージングの後で、前記担体の細孔容積の約90〜約100%を保持する、請求項1記載のN2O除去触媒複合体。
- 前記セリアを基礎とする担体は、約90〜約100質量%のCeO2を含み、かつ少なくとも約0.20cm3/gの細孔容積を示す、請求項1記載のN2O除去触媒複合体。
- 前記セリアを基礎とする担体は、約40〜約200m2/gの範囲の新規表面積を示す、請求項1記載のN2O除去触媒複合体。
- 前記セリアを基礎とする担体は、空気中10質量%の水で、750℃で、20時間のエージングの後に、約20〜約140m2/gの範囲の表面積を示す、請求項1記載のN2O除去触媒複合体。
- 前記セリアは、X線回折(XRD)により測定して、約3〜約20nmの範囲のクリスタリットサイズを示す、請求項1記載のN2O除去触媒複合体。
- 前記セリアを基礎とする担体は、空気中10%のH2Oで、750℃で、20時間エージングした材料の、新規の材料に対する約2.5以下のX線回折クリスタリットサイズ比率を示す、請求項1記載のN2O除去触媒複合体。
- 前記セリアを基礎とする担体は、さらに、イットリア、サマリア、ガドリニア、ジルコニア、またはシリカを含む助触媒を含む、請求項1記載のN2O除去触媒複合体。
- 前記セリアを基礎とする担体は、セリアを、酸化物を基礎として担体の約56〜約100質量%の範囲の量で含む、請求項1記載のN2O除去触媒複合体。
- 前記ロジウム成分は、前記担体上で、前記担体の約0.01〜約5質量%の範囲の量で存在する、請求項1記載のN2O除去触媒複合体。
- 前記ロジウム成分は、前記担体の約0.04〜約3質量%の量で存在する、請求項1記載のN2O除去触媒複合体。
- 前記ロジウム成分は、約5nm未満のクリスタリットサイズを示す、請求項1記載のN2O除去触媒複合体。
- 前記ロジウム成分は、前記支持体上に、約1〜約105g/ft3の範囲の量で負荷されている、請求項1記載のN2O除去触媒複合体。
- 前記触媒材料は、さらに、付加的金属成分を含む、請求項1記載のN2O除去触媒複合体。
- 前記付加的金属成分は、白金(Pt)、パラジウム(Pd)、銀(Au)、銅(Cu)、またはそれらの組合せを含む、請求項16記載のN2O除去触媒複合体。
- 前記触媒材料は、さらに、前記Rh成分および/または前記付加的金属成分を補助するための金属酸化物を含む、請求項16記載のN2O除去触媒複合体。
- 前記金属酸化物は、セリア、プラセオジミア、イットリア、サマリア、またはガドリニアを含む、請求項18記載のN2O除去触媒複合体。
- 前記支持体は、モノリス支持体を含む、請求項1から19までのいずれか1項記載のN2O除去触媒複合体。
- 前記支持体は、ウォールフロー型フィルターを含む、請求項1から19までのいずれか1項記載のN2O除去触媒複合体。
- 炭化水素、一酸化炭素、および窒素酸化物を含む内燃機関排気流を処理するためのエミッション処理システムであって、前記エミッション処理システムは、
排気マニホールドを介して前記内燃機関と流体連通する排気管;
処理触媒;および
請求項1から19までのいずれか1項記載のN2O除去触媒複合体
を含む、エミッション処理システム。 - 前記処理触媒は、排気流の条件下で、炭化水素および/または一酸化炭素を酸化するために有効である、高表面積耐火金属酸化物担体上に貴金属を含む、請求項22記載のエミッション処理システム。
- 前記処理触媒は、三元転化(TWC)触媒、リーンNOxトラップ(LNT)、および選択的接触還元(SCR)触媒からなる群から選択される窒素酸化物処理触媒を含む、請求項23記載のエミッション処理システム。
- 前記N2O除去触媒複合体は、前記窒素酸化物処理触媒の下流に配置されている、請求項24記載のエミッション処理システム。
- 前記システムは、区分けされていて、かつ前記窒素酸化物処理触媒は、前方の、上流区域にあり、かつ前記N2O除去触媒複合体は、後方の、下流区域にある、請求項24記載のエミッション処理システム。
- 前記システムは、積層されていて、かつ前記窒素酸化物処理触媒は、外側層内にあり、かつ前記触媒複合体のN2O除去触媒材料は、内側層内にある、請求項24記載のエミッション処理システム。
- 前記システムは、積層されていて、かつ前記窒素酸化物処理触媒は、内側層内にあり、かつ前記N2O触媒複合体のN2O除去触媒材料は、外側層内にある、請求項24記載のエミッション処理システム。
- 請求項1から19までのいずれか1項記載のN2O除去触媒複合体を、炭化水素、一酸化炭素、および窒素酸化物を含むガス流と接触させることを含む排気ガスを処理する方法。
- 10質量%の水で、750℃で、20時間のエージングの後の前記触媒材料のN2O除去活性は、新規触媒材料のN2O除去活性よりも高い、請求項29記載の方法。
- 内燃機関の排気流用の、請求項1記載の触媒複合体において、支持体上のウォッシュコート内にN2O除去触媒材料を含み、前記触媒材料は、セリアを基礎とする担体上に担持されたロジウム(Rh)成分を含み、かつ前記排気流の条件下で一酸化二窒素(N2O)を転化するために有効であり、前記セリアを基礎とする担体は、
約90〜約100質量%のCeO2、
約0.20〜約0.40cm3/gの範囲にある細孔容積、
約40〜約200m2/gの範囲にある新規表面積、および
空気中10質量%の水で、750℃で、20時間のエージングの後で、約20〜約140m2/gの範囲であるエージングした表面積
を示す、触媒複合体。 - 一酸化二窒素(N2O)除去触媒複合体の製造方法であって、前記方法は、
ロジウム前駆体を、少なくとも約0.20cm3/gの細孔容積を示す新規セリアを基礎とする担体に堆積させ、かつこれからウォッシュコートを形成させること、
フロースルー型モノリスまたはウォールフロー型フィルターを含む支持体を、前記ウォッシュコートで被覆し、被覆された支持体を形成させること、および
前記被覆された支持体を空気中で高めた温度で焼成すること
を含む、一酸化二窒素(N2O)除去触媒複合体の製造方法。 - 前記焼成工程は、空気中10質量%の水で、750℃で、20時間の条件下である、請求項32記載の方法。
- さらに、前記堆積工程の前に、前記新規セリアを基礎とする担体を、約600℃〜約800℃で焼成することを含む、請求項32記載の方法。
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US11149610B2 (en) | 2021-10-19 |
US20200232366A1 (en) | 2020-07-23 |
US11713705B2 (en) | 2023-08-01 |
US10634030B2 (en) | 2020-04-28 |
WO2016094399A1 (en) | 2016-06-16 |
KR102483435B1 (ko) | 2023-01-02 |
JP6703537B2 (ja) | 2020-06-03 |
US20170362984A1 (en) | 2017-12-21 |
US20220010714A1 (en) | 2022-01-13 |
CN107223072A (zh) | 2017-09-29 |
EP3244995A1 (en) | 2017-11-22 |
CN107223072B (zh) | 2021-01-08 |
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KR20170093899A (ko) | 2017-08-16 |
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