JP2011526197A - 排出物質浄化用途のための強化されたレドックスos材料のための塩基性交換 - Google Patents
排出物質浄化用途のための強化されたレドックスos材料のための塩基性交換 Download PDFInfo
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- JP2011526197A JP2011526197A JP2011501154A JP2011501154A JP2011526197A JP 2011526197 A JP2011526197 A JP 2011526197A JP 2011501154 A JP2011501154 A JP 2011501154A JP 2011501154 A JP2011501154 A JP 2011501154A JP 2011526197 A JP2011526197 A JP 2011526197A
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Abstract
Description
酸素貯蔵(OS)材料は、例えば、セリア−ジルコニア(CeO2−ZrO2)固溶体をベースとする周知の固体電解質である。それらは、ガソリン車用の後処理触媒の普遍的な成分であって、それらは局所的な燃料リッチ(還元)又は燃料リーン(酸化)条件に対し、前記触媒中の活性成分を緩衝することができる。OS材料はこの緩衝を、酸素の減損した過渡状態(transients)下にそれらの3D構造から活性酸素を急速かつ再現性のある手法で放出し、酸素に富む条件が生じる際に気相からの吸着によるこの‘失われた’酸素を再生することにより、行う。この還元−酸化(以下、レドックス)化学は、Ce4+←→Ce3+レドックス対に起因するものであり、その際に、Ceの酸化状態は局所的なO2含量に依存している。酸素のこの高い利用可能性は、包括的な酸化/還元化学、例えばガソリン三元触媒のためのCO/NO化学の促進にとって、又はより最近には、例えばUS2005 0282698 A1の触媒ディーゼル微粒子捕集フィルター(CDPF)における粒子状物質(すす)の直接接触酸化にとって重要である。
実質的に純相の(phase pure)立方晶蛍石構造を含有するZrO2/CeO2固溶体をベースとする酸素貯蔵(OS)材料の性能の有意な改善は、塩基、すなわち非貴金属族の金属の特殊なイオン交換により達成されることができる。本明細書に記載されるイオン交換法は、化学的に塩基性の、すなわち高いpHの条件、いわゆる高いOH-/低いヒドロニウム(H3O+)又はプロトン(H+)含量下に、実施される。前記塩基性イオン交換法は、ばらばらの後合成的な修飾であり、ひいては以前の研究(US 6,468,941及びUS 6,585,944)に記載された従来の直接合成法に比較して、組成、ドーパントイオンタイプ及び濃度の顕著により高い自由度を提供する。生じた材料は、試験されて全てのエージング条件下で、高い活性及び水熱耐久性を証明している。これは、酸性金属、例えば金属硝酸塩の通常の含浸により実現されうる促進とは異なっており、通常の場合に新鮮な材料中のバルク酸化物相の形成及びそのような酸化物相の生じる失活を伴う急速焼結が普通である。故に、開発された方法は、安定でかつ高度に活性なOS材料の幅広くかつ新規な範囲の材料を提供し、前記材料は、ガソリン車及びディーゼル車の双方のための排出物質浄化用途の幅広い範囲に有利に適用されることができる。さらに、本発明の方法は、付加的な触媒機能、例えばリーンNOx制御を組み込む又は高めるための特殊な化学的相乗効果を導入する卑金属促進剤(promotant)の選択及びテーラー化を可能にする。
a)高められた低温反応性及び卓越した水熱耐久性を有するOS材料を提供する;
b)例えばNOxトラップ/SCR等のようなイオン交換された吸着原子の活性及び補助的な触媒機能を損なわない;
c)高められた安定性、より高い分散、ひいては前記レドックス活性な元素にガス状反応物がより近寄りやすくなることによる、改善された性能;
d)所望の構造的な及び組織的な性質、例えば単相の立方晶系、高くかつ耐久性の細孔容積及びSA(表面積)のメソ孔系を有する予備形成されたOS材料の利点、ひいては後修飾の付随された性能の利点をさらに高める;
e)格子パラメーター、相純度、欠陥密度、表面酸性度、塩基性度、等の最小限の損傷を伴う、化学修飾のより大きな自由度
f)特殊な用途に"合わせられた"特性及び性質を有する仕立てられたテーラー化されかつ約束された(bespoke)材料の範囲を製造するための、包括的な既存の商業的な材料のための特殊な後修飾法を提供する。
本発明は、排出物質処理触媒のための修飾されたホスト及び前記ホストを製造する方法に関する。前記ホストは、当工業界に周知のCe−ZrOxタイプの実質的に純相の立方晶蛍石(XRD法により測定される)である。前記修飾は、提唱されるが、理論により結びつけられることが望まれるものではないが、このために選択される卑金属元素/イオンによる前記結晶の表面中及びより少ない程度でバルク中の双方に存在するCe3+−OHヒドロキシルのイオン交換から生じる。
1.OS1 100gを秤量し、含水量について校正する(水約1.5%)。
2.硝酸銀結晶3.15gを秤量する。使用される硝酸塩又は溶液中の金属の百分率について補償されなければならない。硝酸銀は銀63.52%である。
3.硝酸銀を脱イオン水50g中に溶解させる。使用される水の量は、使用される混合酸化物の水吸着容量により決定される。これは、混合酸化物1グラムあたり一般的に水0.5〜0.6gである。
4.濃NH4OHaq(約30%アンモニア)を前記硝酸銀溶液に、澄明な銀ジアンモニア性溶液が得られるまで滴加する。溶液は、最初に黒褐色に変わり、ついで水酸化アンモニウムの過剰の添加の際に澄明になる。
5.銀ジアンモニア性溶液を混合酸化物粉末に添加する。十分に混合して、均質でかつむらなく着色した湿った粉末を生じさせる。
6.粉末を室温で1時間放置する。
7.乾燥器中で約110℃で、約2時間又は乾燥するまで乾燥させる。
8.炉中で空気中540℃で4時間か焼する。
硝酸銅(II)三水和物10.86gを秤量し、脱イオン水50g中に溶解させる。30質量%水酸化アンモニウム溶液(約8.0g)を銅溶液に、ブルーブラックの銅テトラアンモニア性溶液が得られるまで添加する。ついで、銅テトラミン溶液をOS2 100g(乾燥量基準)に添加して、その際に均質な粉末が得られるまで混合する。乾燥させ、540℃で4時間か焼する。
硝酸コバルト(II)六水和物4.94gを脱イオン水50g中に溶解させる。30質量%水酸化アンモニウム溶液(約6.5g)を、鮮やかな青色のアンモニア性コバルト溶液が得られるまで添加する。pHを8.0〜9.5に維持する。過剰の水酸化アンモニウムを添加することに配慮する必要はない、なぜならこれは水酸化物形成のために前記溶液のゲル化をもたらすからである。アンモニア性コバルト溶液をOS2(乾燥) 100gに添加し、その際に均質な粉末が得られるまで混合する。乾燥させ、540℃で4時間か焼する。
硝酸銅(II)三水和物3.80gを秤量し、脱イオン水50g中に溶解させる。30質量パーセントの水酸化アンモニウム溶液(約3.0g)を銅溶液に、ブルーブラックの銅テトラミン溶液が得られるまで添加する。ついで、銅テトラミン溶液をOS2(乾燥) 100gに添加して、その際に均質な粉末が得られるまで混合する。乾燥させ、540℃で4時間か焼する。
硝酸鉄(III)九水和物18.08gを秤量し、脱イオン水400g中に溶解させる。トリエタノールアミン43.4を秤量する。前記硝酸鉄溶液をトリエタノールアミン溶液中へ、激しく撹拌しながらゆっくりと注ぐ。鉄溶解度は、アンモニアの形で限定される。正確な比は、硝酸鉄九水和物1gあたり水22g及びトリエタノールアミン2.4gである。鉄−トリエタノールアミン溶液が調製されると、それをOS3(乾燥) 100gに添加する。生じたスラリーは、低い粘度を有する流体になる。スラリー混合物を回転蒸気蒸発器中で乾燥させる。ついで540℃で4時間か焼する。
OS2=40%CeO2;50%ZrO2/HfO2;5%La2O3;5%Pr6O11
OS3=31.5%CeO2;58.5%ZrO2/HfO2;5%La2O3;5%Y2O3
全ての組成は質量%として引用される
Claims (13)
- 酸化セリウムを含有する金属酸化物担体材料を溶解されたカチオンの前駆物質溶液と、高いpH/低いヒドロニウムイオン(H3O+)/低いプロトン(H+)含量の条件下で接触させ、ここで高いpHは約8.0〜約9.5の値を指す、引き続きこうして交換/促進されたセリウムを含有する酸化物を乾燥及びか焼して、いずれの溶剤を除去し、かつカチオンを高度に分散された金属の又は金属酸化物集合又はクラスターへ変換することに基づく、遷移金属、アルカリ金属、アルカリ土類金属及びIIIb族金属からなる群から選択される高度に分散された金属原子又は金属イオンを含有する触媒材料を製造する方法。
- 使用されるカチオン溶液が、前記金属カチオンのアンモニア性錯体を含有する、請求項1記載の方法。
- 前記カチオン溶液が、前記金属カチオンの有機アミン錯体を含有する、請求項1及び/又は2記載の方法。
- 前記カチオン溶液が、前記金属カチオンの水酸化物化合物を含有する、請求項1から3までの1つ又はそれ以上に記載の方法。
- 前記材料を、350℃を超える温度でか焼して、金属前駆物質を最終的に分散された金属/金属酸化物状態へ変換する、請求項1から4までの1つ又はそれ以上に記載の方法。
- こうして導入された金属種の濃度は、約0.01質量%〜約10質量%である、請求項1から5までの1つ又はそれ以上に記載の方法。
- 酸化セリウムが、セリウム及びジルコニウム酸化物(Ce−Zr酸化物)の固溶体である、請求項1から6までの1つ又はそれ以上に記載の方法。
- Ce−Zr酸化物が、酸素イオン伝導性を有する実質的に純相の固溶体であり、かつ
a.ジルコニウム約95%まで
b.セリウム約95%まで
c.希土類、イットリウム及び前記安定剤の少なくとも1つを含んでなる組合せからなる群から選択される安定剤約20%まで
を含んでなる、請求項1から7までの1つ又はそれ以上に記載の方法。 - 請求項1から8までの1つ又はそれ以上に記載の方法により製造された材料であって、前記担体は、XRDによる相分析が、促進された材料が1100℃での水熱酸化エージング後に少なくとも95%の立方晶蛍石相を維持していることを示し、かつ常用の温度プログラムされた還元(TPR)により測定される低温で高められる酸素イオン伝導率を示す分散の高いレベルで金属を含有し、ドープされていない担体と比較した場合に、促進の程度は、金属助触媒のタイプ及び濃度に関係しているが、しかし母体となる材料に比較して、TPR極大値を約50℃〜約500℃に低下させる、材料。
- 請求項1から8までの1つ又はそれ以上に記載の方法により製造された材料であって、前記担体は、XRDによる相分析が、促進された材料が1100℃での水熱酸化エージング後に少なくとも95%の立方晶蛍石相を維持していることを示す分散の高いレベルで金属を含有し、かつTPRにより測定されるレドックスの促進が、1100℃での水熱酸化エージング後に実質的に維持される、材料。
- 請求項1から8までの1つ又はそれ以上に記載の方法により得られた材料であって、こうして導入された金属種の濃度が0.1質量%〜約2.5質量%である、材料。
- 生じた生成物は、常用のX線回折法による相分析が実質的に純相の立方晶蛍石相(>95%)を表す分散の高いレベルで金属を含有し、その際にバルク金属酸化物ドーパント相が<5%で記録され、かつ線幅の広がり/シェーラーの式測定により測定されるドーパント金属酸化物粒度が、約30Å〜約100Åである、請求項11記載の材料。
- 生じた生成物は、XRDによる相分析が、促進された材料が1100℃での水熱酸化エージング後に少なくとも95%の立方晶蛍石相を維持することを示す分散の高いレベルで金属を含有する、請求項11及び/又は12の1又はそれ以上に記載の材料。
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JP2017120754A (ja) * | 2015-12-28 | 2017-07-06 | 昭和電工株式会社 | マイクロポーラス層およびそれを用いた燃料電池 |
JP2021510119A (ja) * | 2018-01-08 | 2021-04-15 | パシフィック インダストリアル デベロップメント コーポレイション | 酸素貯蔵材料およびその製造方法 |
JP7506602B2 (ja) | 2018-01-08 | 2024-06-26 | パシフィック インダストリアル デベロップメント コーポレイション | 酸素貯蔵材料およびその製造方法 |
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CN102112223A (zh) | 2011-06-29 |
BRPI0909386A2 (pt) | 2015-10-06 |
CN101980778A (zh) | 2011-02-23 |
WO2009118189A4 (en) | 2009-11-19 |
KR20100135858A (ko) | 2010-12-27 |
CN102006923B (zh) | 2014-08-27 |
CN102006923A (zh) | 2011-04-06 |
JP2011515221A (ja) | 2011-05-19 |
EP2259870A4 (en) | 2017-11-15 |
EP2268394A1 (en) | 2011-01-05 |
WO2010002486A3 (en) | 2010-03-25 |
WO2009118189A1 (en) | 2009-10-01 |
BRPI0909381A2 (pt) | 2016-05-17 |
WO2009118190A4 (en) | 2010-03-18 |
WO2009118190A2 (en) | 2009-10-01 |
WO2009118188A1 (en) | 2009-10-01 |
WO2009118190A3 (en) | 2010-01-21 |
EP2259870A2 (en) | 2010-12-15 |
EP2268395A2 (en) | 2011-01-05 |
KR20160129913A (ko) | 2016-11-09 |
BRPI0909377A2 (pt) | 2017-06-13 |
KR20110008190A (ko) | 2011-01-26 |
JP2011526198A (ja) | 2011-10-06 |
WO2010002486A2 (en) | 2010-01-07 |
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