CN102821836A - 包括挤出固体主体的三效尾气净化催化剂 - Google Patents
包括挤出固体主体的三效尾气净化催化剂 Download PDFInfo
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- CN102821836A CN102821836A CN2011800162937A CN201180016293A CN102821836A CN 102821836 A CN102821836 A CN 102821836A CN 2011800162937 A CN2011800162937 A CN 2011800162937A CN 201180016293 A CN201180016293 A CN 201180016293A CN 102821836 A CN102821836 A CN 102821836A
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Abstract
包括挤出固体主体的三效尾气净化催化剂，该挤出固体主体包括：10-100wt%的至少一种粘结剂/基质组分；5-90wt%的沸石型分子筛，非沸石型分子筛或它们的任何两种或多种的混合物；和0-80wt%的任选稳定化的二氧化铈，该催化剂包括至少一种贵金属和任选的至少一种非贵金属，其中：(i)该至少一种贵金属被承载在该挤出固体主体的表面上的一个或多个涂层中；(ii)至少一种金属存在于整个挤出固体主体中并且至少一种贵金属也被承载于在该挤出固体主体的表面上的一个或多个涂层中；或(iii)至少一种金属存在于整个挤出固体主体上，以更高的浓度存在于该挤出固体主体的表面上并且至少一种贵金属也被承载于在该挤出固体主体的表面上的一个或多个涂层中。
Description
本发明涉及包括挤出固体主体的三效尾气净化催化剂，其用于处理来自于内燃机的废气排放物，尤其用于静止来源和移动即车辆(汽车)应用的内燃机的废气排放物。
US 2002/0183191公开了包括沸石/氧化铝复合催化剂载体的三效尾气净化催化剂，该载体显示出至少750 psi的断裂模量和含有具有至少300的硅石/氧化铝比率的沸石，该催化剂载体浸渍有选自铂，铑，铱和钯的贵金属。该三效尾气净化催化剂具有高的泡孔密度，薄壁和没有洗涂剂(washcoat)。在一个实施方案中，催化剂载体除了含有沸石和氧化铝之外，还含有任选稳定化的二氧化锆。二氧化锆掺杂剂能够包括至多80wt%的二氧化铈，基于锆总量。然而，没有提供包括任选掺杂的二氧化锆的实施例。
US'191明确排除了用含催化剂的淤浆所进行的洗涂，以避免在蜂窝的通道尺寸上的减少和避免增大的反压力。此外，也排除了硅石粘结剂的使用，因为在硅石和铂金属之间的不相容性。因此，γ氧化铝用作粘结剂。然而，在所提供的对比实施例中，根据该本发明的催化剂的三效尾气净化催化剂性能(作为用于转化CO、NOx和烃类的点火温度来测量)，特别对于沸石:γ氧化铝的50:50和40:60重量比，无法充分地与包括仅仅氧化铝的挤出载体或沸石/硅石粘结剂型载体的对比实施例进行对比。
US 5,772,972公开了用于处理内燃机废气的汽车催化剂体系。该体系包括沸石型烃捕获剂和承载于基底整块上的钯基三效尾气净化催化剂材料的混杂体系。在一个实施方案中，该三效尾气净化催化剂在挤出沸石基底整块上成层。然而，没有提供包括挤出沸石基底整块的具体实施例。
EP 1739066公开了蜂窝状结构，它包括：具有许多通孔的许多蜂窝单元；和经由蜂窝单元(其中通孔没有打开)的各封闭外表面将蜂窝单元彼此连在一起的密封层。该蜂窝单元包括至少无机颗粒，无机纤维和/或晶须（whisker）。例举的无机颗粒是氧化铝，二氧化钛，硅石和二氧化锆；例举的无机纤维是硅石氧化铝纤维；和例举的无机粘结剂是氧化硅溶胶，氧化铝溶胶，海泡石和凹凸棒石。催化剂组分可承载于蜂窝状结构上。该催化剂组分可以包括选自贵金属(包括铂、钯和铑)，碱金属如钾和钠，碱土金属例如钡和氧化物类中的至少一种类型。该蜂窝状结构可用作用于车辆废气的转化的催化转化器例如三效尾气净化催化剂或NOx贮存催化剂。
我们现在已经开发了包括涂布有至少一种贵金属的挤出固体主体的三效尾气净化催化剂家族，该催化剂特别可用于内燃机废气的废气后处理的领域中。此类废气可来源于静止来源排放物，但是它们已经被开发来尤其用于处理移动的排放物源如轿车、卡车和公共汽车。
根据一个方面，本发明提供包括挤出固体主体的三效尾气净化催化剂，所述挤出固体主体主体包括：10-100wt%的至少一种粘结剂/基质组分；5-90wt%的沸石型分子筛，非沸石型分子筛或它们的任何两种或多种的混合物；和0-80wt%的任选稳定化的二氧化铈，
所述催化剂包括至少一种贵金属和任选的至少一种非贵金属，其中：
(i)所述至少一种贵金属被承载于所述挤出固体主体的表面上的一个或多个涂层中；
(ii) 至少一种金属存在于整个挤出固体主体中并且至少一种贵金属也被承载于在所述挤出固体主体的表面上的一个或多个涂层中；或
(iii) 至少一种金属存在于整个挤出固体主体中，以更高的浓度存在于所述挤出固体主体的表面上并且至少一种贵金属也被承载于在所述挤出固体主体的表面上的一个或多个涂层中。
本发明的优点是，通过除去常常用于催化涂层中的催化组分，涂层的数量可减少，例如从两层减少到单层。这具有降低排气系统中的回压、提高发动机的效率的益处。
与根据以上所述的US'191的催化剂相比，本发明具有多个的特殊优点。虽然该发明人承认，通过涂布一种挤出主体，在US'191中提到的一些缺点可能在本发明的三效尾气净化催化剂的某些构型中会遇到，但是这些缺点被在催化活性上的基本改进显著地超过，特别对于在US'191中公开的50:50和40:60(重量)沸石:氧化铝实施方案。 此外，本发明不局限于非硅石粘结剂的使用。另外，较低硅石:氧化铝比率分子筛可用于本发明中，它允许分子筛与可以促进HC吸附(离子交换部位通过提高硅石:氧化铝比率而除去)以减少冷起动HC排放物的那些金属进行离子交换。
也有可能的是，相对于在惰性基底整块上的涂层而言，提高在挤出固体主体中活性组分的体积。这种提高的催化剂密度对于长期耐久性和催化剂性能具有优点，这对于车载诊断(on-board diagnostics)是重要的。
在机动车辆的领域中的“车载诊断”(OBD)是用于描述由连接到合适的电子管理系统上的探测器的网络所提供的车辆系统的自诊断和报告能力的通用术语。如果检测到问题的话，OBD系统的早期例子会简单地照亮故障指示灯，但是对于问题的本质却没有提供信息。更现代的OBD系统使用标准化数字连接口并且可提供关于标准化诊断故障代码的信息和实时数据的选择，这使得车辆的系统能快速识别和解决问题。
当前的OBD要求都要求在排放系统的故障或劣化(将引起排放物超过强制性的阈值)时司机必须得到通知。因此，例如，Euro 4对汽油(gasoline)客车的OBD限制是：CO-3.2 g/km；HC-0.4 g/km；NOx-0.6 g/km；和PM-没有限制。
未来车辆排放物法规，特别在美国和欧洲，要求在诊断功能上的较高敏感性，以便连续地监测排气系统后处理催化剂满足排放物法规的能力。例如，对于强制点火(汽油)客车的目前草案OBD限制是：CO-1.9 g/km；NMHC-0.25 g/km；NOx-0.54 g/km；和PM-没有限制。
在美国，认为用于汽油/火花点火发动机的催化剂监测的OBD II法规(Title 13, California Code Regulations, Section 1968.2, Malfunction and Diagnostic System Requirements for 2004 and Subsequent Model-Year Passenger Cars, Light-Duty Trucks and Medium-Duty Vehicles and Engines)要求当催化剂体系的监测部分的NMHC转化效率的平均联邦试验规程(the average Federal Test Procedure)(FTP)测试值降低到低于50%时有故障信号。
本发明的挤出固体主题一般包括蜂窝形式的单一结构，后者具有从它的第一端延伸到第二端的均匀尺寸和平行的通道。一般，这些通道在第一端和第二端都是开通的－所谓的“穿流式”构型。界定这些通道的通道壁是多孔性的。典型地，外部“皮”包围该挤出固体主体的许多通道。挤出固体主体可从任何所需的横截面（如圆形、正方形或椭圆形）所形成。在许多通道中的各个通道可是正方形，三角形，六边形，圆形的等等。在第一上游末端的通道可被例如合适的陶瓷水泥封闭，并且在第一上游末端上没有被封闭的通道也可在第二下游末端上被封闭以形成所谓的壁流式过滤器。典型地，在第一上游末端上封闭通道的排列类似于具有封闭和开通的下游通道末端的类似排列的方格板(chequer board)。
很显然，公开在EP 1739066中的蜂窝状结构具有太低的热震参数(TSP)而不能用于单个单一挤出物中，因为该蜂窝状结构包括被粘结在一起的单独蜂窝单元的组装体。这一排列(在商购的碳化硅蜂窝中也会看到)被设计来避免灾难性的催化剂基底破坏，所述破坏尤其归因于由于挤出材料的较高热膨胀系数(CTE)所引起的热冲击。然而，从单独蜂窝单元制造蜂窝状结构是复杂的、费力的、费时和费钱的并且提高了例如在粘结上的可能的物理破坏模式的数量（与单件挤出相比较）。TSP和CTE的更完整解释可见于 “Catalytic Air Pollution Control – Commercial Technology”, 第二版, R.M. Heck等人, John Wiley & Sons, Inc., New York, 2002 Chapters 7 (相对于穿流式整块) and 9 (对于壁流式过滤器)。
因此，优选的是，当用于处理来自静止或移动排放物源的废气时，本发明的催化剂的挤出固体主体具有足以避免在挤出固体主体中的径向裂纹和环形裂纹的轴向热震参数(TSP)和径向TSP。以这种方式，挤出固体主体可从单个单一挤出物形成。对于具有特别大的横截面的挤出固体主体，仍然必要的是挤出该挤出固体主体的片段以便粘结在一起。然而，这是因为在加工具有如此大的横截面的挤出物中的困难，或因为在挤出物口模工具的尺寸上的限制。然而，分别来说，整个催化剂的各个片段将满足功能限制：当用于处理来自静止或移动排放物源的废气时，轴向TSP和径向TSP足以避免在单个挤出固体主体片段中的径向裂纹和环形裂纹。在一个实施方案中，径向TSP在750℃下>0.4，如>0.5，>0.6，>0.7，>0.8 ，>0.9或>1.0。在800℃下，径向TSP也希望>0.4和特别对于三效尾气净化催化剂(它在使用过程中经历较高的温度)，在1000℃下的TSP优选是>0.8。
壁流动式过滤器的CTE优选是20 × 10-7/℃以便由单件挤出物制备。
在实施方案中，至少一种粘结剂/基质组分可选自堇青石，氮化物，碳化物，硼化物，金属互化物，硅铝酸锂，尖晶石，任选掺杂的氧化铝，硅石源，二氧化钛，二氧化锆，二氧化钛-二氧化锆，锆英石以及它们的任何两种或多种的混合物。
尖晶石可是MgAl2O4或Mg可部分地被选自Co，Zr，Zn或Mn中的金属替代。，在MgAl2O4中MgO相对于Al2O3的含量可是0.8到2.5，其中<1.0的值是优选的。
该氧化铝粘结剂/基质组分优选是γ氧化铝，但是可是任何其它过渡型氧化铝，即α氧化铝，β氧化铝，χ氧化铝，η氧化铝，ρ氧化铝，κ氧化铝，θ氧化铝，δ氧化铝，镧β氧化铝以及任何两种或多种此类过渡型氧化铝的混合物。
优选的是，该氧化铝用至少一种非铝元素掺杂，以便提高氧化铝的热稳定性。合适的氧化铝掺杂剂包括硅，锆，钡，镧系元素以及它们的任何两种或多种的混合物。合适的镧系元素掺杂剂包括La，Ce，Nd，Pr，Gd以及它们的任何两种或多种的混合物。
硅石源可包括硅石，氧化硅溶胶，石英，熔融硅石或无定形的硅石，硅酸钠，无定形硅铝酸盐，烷氧基硅烷，聚硅氧烷树脂粘结剂如甲基苯基聚硅氧烷树脂，粘土，滑石或它们的任何两种或多种的混合物。
在这一列表中，该硅石可是SiO2本身，长石，多铝红柱石，硅石-氧化铝，硅石-氧化镁，硅石-二氧化锆，硅石-二氧化钍，硅石-二氧化铍(berylia)，硅石-二氧化钛，三元硅石-氧化铝-二氧化锆，三元硅石-氧化铝-氧化镁，三元硅石-氧化镁-二氧化锆，三元硅石-氧化铝-二氧化钍以及它们的任何两种或多种的混合物。另外地，该硅石能够通过煅烧被添加到该挤出组合物中的原硅酸四甲基酯(TMOS)来形成。
合适的粘土包括漂白土，海泡石，锂蒙脱石，蒙皂石，高岭土以及它们的任何两种或多种的混合物，其中该高岭土可选自亚膨润土(subbentonite)，蠕陶土，埃洛石，高岭石，迪开石，珍珠陶土和它们的任何两种或多种的混合物；该蒙皂石可选自蒙脱石，绿脱石，蛭石，皂石和它们的任何两种或多种的混合物；和该漂白土能够是蒙脱石或坡缕石(凹凸棒石)。
无机纤维选自碳纤维，玻璃纤维，金属纤维，硼纤维，氧化铝纤维，硅石纤维，硅石-氧化铝纤维，碳化硅纤维，钛酸钾纤维纤维，硼酸铝纤维和陶瓷纤维。
用于本发明的合适分子筛是能够在汽车发动机的冷起动之后吸附未燃烃类并在超过环境温度下解吸所吸附的烃类的那些分子筛，例如当缔合的贵金属基三效尾气净化催化剂组分已经达到例如CO和HC氧化或NOx还原所需要的熄火(light-off)温度时。此类分子筛一般不是具有8-环孔隙敞开结构作为它的最大孔隙敞开结构的那些，有时被称作“小孔”分子筛。优选的分子筛是中孔(最高10-环孔隙敞开结构)，大孔(最高12-环孔隙敞开结构)或烘箱介孔（oven meso）(>12-环孔隙敞开结构)分子筛。
所述的沸石型分子筛或各种沸石分子筛或所述的非沸石型分子筛或各种非沸石型分子筛能够选自如the Structure Commission of the International Zeolite Association所定义的框架类型编码 ABW，AEL，AET，AFG，AFI，AFO，AFR，AFS，AFY，AHT，AST，ASV，ATN，ATO，ATS，ATV，AWO，AWW，BCT，BEA，BEC，BIK，BOF，BOG，BPH，BRE，BSV，CAN，CAS，CFI，CGF，CGS，-CHI，-CLO，CON，CZP，DAC，DFO，DOH，DON，EMT，EON，ESV，ETR，EUO，EZT，FAR，FAU，FER，FRA，GIU，GME，GON，HEU，IFR，IMF，ISV，ITH，ITR，IWR，IWS，IWV，IWW，JBW，JRY，LAU，LIO，-LIT，LOS，LOV，LTF，LTL，LTN，MAR，MAZ，MEI，MEL，MEP，MFI，MFS，MOR，MOZ，MRE，MSE，MSO，MTF，MTN，MTT，MTW，MWW，NAB，NAT，NES，NON，NPO，OBW，OFF，OSI，OSO，-PAR，PON，-RON，RRO，RSN，RTE，RUT，RWR，RWY，SAO，SAS，SBE，SBS，SBT，SFE，SFF，SFG，SFH，SFN，SFO，SFS，SGT，SOD，SOF，SOS，SSF，SSY，STF，STI，STO，STT，STW，-SVR，SZR，TER，TOL，TON，TUN，UOS，UOZ，USI，UTL，VET，VFI，VSV，WEI或-WEN 和这些的任何两种或多种的混合物。
优选的沸石型和非沸石型分子筛选自BEA，FAU，FER，MFI，MFS，MOR，STI，SZR以及它们的任何两种或多种的混合物。
特别优选的沸石型或非沸石型分子筛选自BEA，FER，MFI，STI以及它们的任何两种或多种的混合物。特别优选的沸石型分子筛是ZSM-5，β，镁碱沸石和它们的任何两种或多种的混合物。
虽然天然沸石型分子筛可用于本发明，但是我们优选的是硅石与氧化铝之比为10或更大，例如15-150，20-60或25-40的合成硅铝酸盐沸石型分子筛，以便获得改进的热稳定性。
在供选的实施方案中，沸石型分子筛或非沸石型分子筛是含有一种或多种取代框架金属的同形体。在这一实施方案中，所述取代框架金属或各取代框架金属可选自As，B，Be，Ce，Co，Cu，Fe，Ga，Ge，Li，Mg，Mn，Zn和Zr，其中Ce，Cu和Fe。此外，优选的同形体（isomorph）沸石型或非沸石型分子筛可选自BEA，FER，MFI，STI和它们的任何两种或多种的混合物，其中在其框架中包括Fe的BEA是特别优选的。应理解的是，制造含有一种或多种取代框架金属的同形体的方法，所述金属或各金属可以存在于最终产物中，或者仅仅存在于框架中或者存在于框架中且还有离子交换的。
在含有一种或多种取代框架金属的同形体中的硅石与氧化铝之比可为>25，如30-100或40-70。相比之下，该同形体可具有>20，如30-200或50-100的硅石与框架金属之比。
在优选的实施方案中，非沸石型分子筛是磷铝酸盐，其中包括ALPO，金属取代的ALPO(MeAlPO)，硅铝磷酸盐(SAPO)或金属取代的硅铝磷酸盐(MeAPSO)。
磷铝酸盐的硅石与氧化铝之比一般比共享相同的框架类型编码的硅铝酸盐沸石低得多。典型地，硅铝磷酸盐的硅石与氧化铝之比为<1.0，但是可以为<0.5或甚至<0.3。
该二氧化铈组分可任选地被至少一种非铈元素稳定化，以便提高二氧化铈的热稳定性。合适的二氧化铈稳定剂包括锆，镧系元素和它们的任何两种或多种的混合物。镧系元素稳定剂包括La，Nd，Pr，Gd和它们的任何两种或多种的混合物。该CeO2:ZrO2重量比可以例如是在80:20或20:80之间。商购的材料包括30wt% CeO2，63% ZrO2，5% Nd2O3，2% La2O3；和40% CeO2，50% ZrO2，4% La2O3，4% Nd2O3和2% Y2O3。
宽泛地说，在下面的至少一种中存在的至少一种金属：特征(ii)或(iii)中的(a)存在于整个挤出固体主体中的所述至少一种金属，即至少一种金属存在于挤出物组合物中；(b)以更高的浓度存在于该挤出固体主体的表面上的所述至少一种金属；和/或(c)承载于挤出固体主体的表面上的一个或多个涂层之中的所述至少一种金属都不同于在(a)、(b)和(c)的各其它位置上存在的至少一种金属。因此，至少一种金属可存在于位置(c)，(a)加(c)或(a)加(b)加(c)。当至少一种金属存在于(a)和(c)，或(a)、(b)和(c)上时，在各位置上的至少一种金属可以是相同的或不同的。
其中该至少一种金属存在于位置(a)，即在整个挤出固体主体中时，该至少一种金属可与沸石型分子筛，非沸石型分子筛或它们的任何两种或多种的混合物相结合(或相缔合)。“与...相结合或相缔合”的例子包括与沸石型分子筛组分，非沸石型分子筛组分或者混合物中的沸石型分子筛组分和非沸石型分子筛组分中的任何一种或两者进行离子交换。也可能在两种或多种分子筛的混合物中使至少一种金属与一种分子筛相结合而不与另一种分子筛相结合。例如，第一种分子筛可与铜进行离子交换，干燥和煅烧，然后与不具有所缔合的附加金属的不同分子筛混合。
已知某些相结合的金属可对于HC吸附做出贡献，具有本发明的优点。优选的吸附促进金属包括Pd和/或Cu，Ag，碱土金属和碱金属，例如Cs。
或者，混合物中的两种分子筛中的一种可与第一至少一种金属相结合，例如离子交换，然后第二至少一种金属可被添加挤出组合物中，即第二至少一种金属没有特定地与第二分子筛相结合。
与所述分子筛组分的或各分子筛组分相结合的合适的至少一种金属可独立地选自过渡金属、镧系元素或它们的任何两种或多种的混合物。合适的过渡金属包括IB族金属，IVB族金属，VB族金属，VIIB族金属和VIII族金属。优选，该至少一种过渡金属选自Fe，Cu，Ce，Hf， La，Mn和V以及它们的任何两种或多种的混合物。该镧系元素金属可为La，Pr，Ce和它们的两种或多种的混合物。
在与所述分子筛或各分子筛组分相结合的至少一种金属中的金属总含量是0.1-20wt%，如1-9wt%。
存在于在整个挤出固体主体中但不与所述分子筛或各分子筛相结合的至少一种金属；在位于挤出固体主体的表面上的大部分的至少一种金属中的至少一种金属；存在于挤出固体主体的表面上的一个或多个涂层中的至少一种金属；或以更高的浓度存在于挤出固体主体的表面上的至少一种金属可选自碱金属、碱土金属、过渡金属、镧系元素或它们的任何两种或多种的混合物。
用于本发明中的用于承载催化金属的合适涂层包括氧化铝(Al2O3)(特别地γ-氧化铝)，硅石(SiO2)，二氧化钛(TiO2)，二氧化铈(CeO2)，二氧化锆(ZrO2)，五氧化二钒(V2O5)，氧化镧(La2O3)和沸石中的一种或多种。该二氧化铈和氧化铝可任选地通过使用与用于该挤出固体主体的相同稳定剂来稳定化。合适的催化金属包括贵金属(Au，Ag和铂族金属，包括Pt，Pd和Rh))中的一种或多种。二氧化铈和稳定化的二氧化铈典型地作为氧储存组分(OSC)存在于三效尾气净化催化剂中。为了促进已经涂布有含贵金属的洗涂剂的挤出沸石的HC吸附活性，有利的是使用所谓的宽-孔载体例如氧化铝作为该贵金属的洗涂剂载体(参见例如US 6110862，即包括被分散在耐火材料无机氧化物载体相上的铂族金属组分的催化材料，该载体相包括具有一定的孔径分布的第一载体材料，其中第一载体材料的孔隙容积的约98%是由具有在约30至240埃范围内的半径的孔隙所提供的)。
将至少一种金属以更高的浓度定位于该挤出固体主体的表面上的技术包括浸渍，优选增稠的浸渍，即用流变改性剂增稠的浸渍介质。干燥法也能够用于将金属聚集在该挤出固体主体的表面上。例如，其中金属聚集在表面上的所谓“蛋壳（egg shell）”技术可通过相对缓慢地干燥浸渍的挤出固体主体以使得金属利用芯吸作用被沉积在表面上而获得。盐和pH条件的具体选择也能够用于指引金属沉积，例如通过确定该挤出固体主体的等电点和然后使用pH和金属盐的正确组合以便受益于在金属盐中的阳离子或阴离子和挤出固体主体之间的静电引力。
合适的过渡金属包括IB族金属，IVB族金属，VB族金属，VIB族金属，VIIB族金属和VIII族金属。优选，所述过渡金属或各过渡金属选自Fe，Ni，W，Cu，Ce，Hf，La，Mn，Pt，Au，Ag，In，V，Ir，Ru，Rh，Os和它们的任何两种或多种的混合物；镧系金属可是La，Pr或Ce或它们的任何两种或多种的混合物；碱金属包括K和Cs；和碱土金属可选自Ba和Sr。
在整个挤出固体主体中存在但不与所述分子筛或各分子筛组分相结合的金属总含量；位于该挤出固体主体的表面上的金属总含量；和/或以更高的浓度在挤出固体主体的表面上存在的金属总含量可以是0.1-20wt%，如1-9wt%。
该挤出固体主体的金属总含量，即包括与所述分子筛或各分子筛相结合的任何金属，可以是0.1-25wt%，如1-15wt%。
该催化剂总体（包括在挤出固体主体的表面上的包含至少一种金属的一个或多个涂层）上的金属总含量可以是0.1-30wt%，如1-25wt%。
用于在促进三效尾气净化催化活性的挤出固体主体的表面上的一个或多个涂层中的特别优选的贵金属是Pd本身，Pt和Rh的组合物，Pd和Rh的组合物或Pt、Pd和Rh的组合物。当存在超过一种的贵金属时，各金属可被布置在单独的层中，一种或多种贵金属可存在于一个层中以及一种或不是全部的贵金属可存在于另一个层中；或全部的贵金属可存在于各层中但各层可包括不同比率的各贵金属与所述其它贵金属或各种其它贵金属。
在特定的例子中，本发明的催化剂包括挤出固体主体，所述挤出固体主体包括：
10-100wt%的堇青石，氮化物，碳化物，硼化物，金属互化物，硅铝酸锂，任选掺杂的氧化铝，硅石源，二氧化钛，二氧化锆，二氧化钛-二氧化锆，锆英石和它们的任何两种或多种的混合物；
0-80wt%的尖晶石；
5-90wt%的沸石型分子筛，非沸石型分子筛或它们的任何两种或多种的混合物，各自任选含有一种或多种金属；
0-80wt%的任选稳定化的二氧化铈；和
0-25wt%的无机纤维。
至少一种粘结剂/基质组分的含量可以是>15wt%，> 20wt%，>30wt%，>35wt%，>40wt%，>45wt%，>50wt%，>55wt%，>60wt%，>65wt%或>70wt%，>75wt%，>80wt%，>85wt%或>90wt%。
尖晶石的含量可以是>10wt%，>15wt%，> 20wt%，>30wt%，>35wt%，>40wt%，> 45wt%，>50wt%，>55wt%，>60wt%，>65wt%或>70wt%。
分子筛的总含量可以是>10wt%，>wt15%，> 20wt%，>30wt%，>35wt%，>40wt%，> 45wt%，>50wt%，>55wt% ，>60wt%，>65wt%或>70wt%，>75wt%，>80wt% ，>85wt%或>90wt%。
任选稳定化的二氧化铈的含量可以是>5wt%，>10wt%，>15wt% ，> 20wt%，>30wt%，>35wt%，>40wt%，> 45wt%，>50wt%，>55wt%，>60wt%，>65wt%或>70wt%。
无机纤维的含量可以是>5wt%，>10wt%，>15wt%或> 20wt%。
在一个实施方案中，该挤出固体主体基本上由以下组成：10-100wt%的堇青石，氮化物，碳化物，硼化物，金属互化物，硅铝酸锂，尖晶石，任选掺杂的氧化铝，硅石源，二氧化钛，二氧化锆，二氧化钛-二氧化锆，锆英石和它们的任何两种或多种的混合物；50-90wt%的沸石型分子筛，非沸石型分子筛或它们的任何两种或多种的混合物，各自任选地含有一种或多种金属；和0-25wt%的无机纤维。这一挤出固体主体可作为穿流式基底整块排列或它可用于制造壁流式过滤器。优选的实施方案含有无机纤维。
其它的实施方案可使用挤出固体主体，所述挤出固体主体基本上由以下组成：10-37wt%的堇青石，氮化物，碳化物，硼化物，金属互化物，硅铝酸锂，任选掺杂的氧化铝，尖晶石，硅石源，二氧化钛，二氧化锆，二氧化钛-二氧化锆，锆英石和它们的任何两种或多种的混合物；60-88wt%的沸石型分子筛，非沸石型分子筛或它们的任何两种或多种的混合物，各自任选含有一种或多种金属；和0-20wt%的无机纤维；或基本上由以下组成：15-30wt% 的堇青石，氮化物，碳化物，硼化物，金属互化物，硅铝酸锂，任选掺杂的氧化铝，尖晶石，二氧化钛，二氧化锆，二氧化钛-二氧化锆，锆英石和它们的任何两种或多种的混合物；2-20wt%的硅石源；50-81wt%的沸石型分子筛，非沸石型分子筛或它们的任何两种或多种的混合物，各自任选含有一种或多种金属；和2-10wt%的无机纤维。
在适合用于三效尾气净化催化剂的另一个实施方案中，该挤出固体主体基本上由以下组成：10-100wt%的堇青石，氮化物，碳化物，硼化物，金属互化物，硅铝酸锂，任选掺杂的氧化铝，尖晶石，硅石源，二氧化钛，二氧化锆，二氧化钛-二氧化锆，锆英石和它们的任何两种或多种的混合物；5-50wt%的沸石型分子筛，非沸石型分子筛或它们的任何两种或多种的混合物，各自任选地含有一种或多种金属；20-80wt%任选稳定化的二氧化铈；和0-25wt%的无机纤维。优选的实施方案含有沸石和无机纤维。
在开发用于本发明的NOx捕获催化剂中的挤出固体主体时，我们在下列组成的挤出固体主体中遭遇到强度的缺乏：69wt% 的CeO2，以及23wt%的γ-Al2O3和8wt%的玻璃纤维。提高强度的当前建议包括：预煅烧该CeO2材料以减少在“坯材”挤出固体主体的煅烧过程中的表面损失；将氧化铝含量提高至50%+；改变氧化铝(例如来自商购PuralTM-DisperalTM)和/或任选稳定化的二氧化铈的粒度；添加惰性粘结剂(例如粘土)以提高机械稳定性；使用不同的氧化铝例如氧化铝溶胶；试验其它粘结剂体系例如TiO2溶胶，CeO2溶胶；乙酸铈；乙酸锆；优化pH值；和添加表面改性剂例如铝盐或其它有机表面活性剂。在初级的试验中，我们已经发现硅石的存在可影响NOx捕获特性。然而，继续进行研究，将对这一选择进一步进行考察。然而，在一个实施方案中，硅石源的含量将减少或全部除去。
当以上的挤出固体主体中的任何一种被制成壁流式过滤器时，壁流式过滤器的孔隙度可以是30-80%，如40-70%。
在本发明的更特别的例子中：
(i) 催化的烟灰过滤器包括呈现为壁流式过滤器构型的挤出固体主体，所述挤出固体主体基本上由以下组成：15-70wt%的堇青石，氮化物，碳化物，硼化物，金属互化物，硅铝酸锂，尖晶石，任选掺杂的氧化铝，二氧化钛，二氧化锆，二氧化钛-二氧化锆，锆英石和它们的任何两种或多种的混合物；0-20wt%的硅石源；5-50wt%的沸石型分子筛，非沸石型分子筛或它们的任何两种或多种的混合物，各自任选含有一种或多种金属；20-80wt%任选稳定化的二氧化铈；和0-20wt%的无机纤维，该挤出固体催化剂主体涂布有包含承载的至少一种贵金属以及任何两种或多种贵金属的组合物的一个或多个涂层；
(ii) 三效尾气净化催化剂包括穿流式构型的挤出固体主体，该挤出固体主体基本上由以下组成：15-30wt%的堇青石，氮化物，碳化物，硼化物，金属互化物，硅铝酸锂，尖晶石，任选掺杂的氧化铝，二氧化钛，二氧化锆，二氧化钛-二氧化锆，锆英石和它们的任何两种或多种的混合物；0-20wt%的硅石源；50-81wt%的沸石型分子筛，非沸石型分子筛或它们的任何两种或多种的混合物，各自任选地含有一种或多种金属；和0-20wt%的无机纤维，该挤出固体催化剂主体涂布有单层，后者包括大部分γ-氧化铝和仅仅承载钯的，承载钯和铑的混合物的，承载铂和铑的混合物的或承载铂、钯和铑的混合物的稳定化二氧化铈的混合物；
根据另一方面，本发明提供制造本发明的三效尾气净化催化剂的方法，该方法包括以下步骤：
通过混合以下这些组分的粉末状起始原料来形成固体挤出主体：至少一种粘结剂/基质组分或它们的一种或多种组分的前体；沸石型分子筛，非沸石型分子筛或它们的任何两种或多种的混合物，该沸石型分子筛、非沸石型分子筛或者沸石型和非沸石型分子筛的混合物任选地与至少一种金属相结合；任选的任选稳定化的二氧化铈；和任选的至少一种金属化合物；与任选的无机纤维；和任选地添加有机助剂；
通过在任选含有至少一种金属的金属盐的酸性或碱性水溶液中混合和/或捏合来加工成塑性复合物以形成混合物；
将该混合物挤出成催化剂主体，干燥该催化剂主体和煅烧以形成固体挤出主体；
选择定量比例的起始原料，以使得该固体挤出主体包括10-100wt%的至少一种粘结剂/基质组分；5-90wt%的沸石型分子筛，非沸石型分子筛或它们的任何两种或多种的混合物；和0-80wt%的任选稳定化的二氧化铈，和
用含有至少一种贵金属的至少一个涂层涂布该固体挤出主体的表面以及任选地用至少一种金属浸渍该固体挤出主体的表面。
典型地，使用水泥来不可渗透地堵塞挤出基底整块中的通道的末端以便形成壁流式过滤器，例如如在EP 1837063中所公开的。
非常普遍地，对于挤出固体主体的生产，粘结剂、有机的增粘化合物和用于通过掺混将材料转化成均匀浆的液体被添加到粘结剂/基质组分或其前体和分子筛，任选的任选稳定化的二氧化铈，任选的无机纤维和任选的至少一种金属化合物之中，在混合或捏合装置或挤出机中将混合物压实。混合物具有有机添加剂如粘结剂，增塑剂，表面活性剂，润滑剂，分散剂作为加工助剂来增强润湿作用，因此生产均匀的批料。所得到的塑性材料然后经过模塑（尤其使用挤压机或包括挤出模头的挤出机），所得的模塑制品然后被干燥和煅烧。在挤出固体主体的煅烧过程中有机添加剂被“烧尽”。
至少一种粘结剂/基质组分选自堇青石，氮化物，碳化物，硼化物，金属互化物，硅铝酸锂，尖晶石，任选掺杂的氧化铝，硅石源，二氧化钛，二氧化锆，二氧化钛-二氧化锆，锆英石以及它们的任何两种或多种的混合物。可使用氧化铝前体，其为氢氧化铝或勃姆石。当使用氧化铝时，为了确保与氧化铝结合，有利的是在添加其它起始原料之前将水溶性金属盐的水溶液添加到氧化铝中或氧化铝的前体物质中。
在实施方案中，硅石源可选自硅石，氧化硅溶胶，石英，熔融硅石或无定形的硅石，硅酸钠，无定形硅铝酸盐，烷氧基硅烷，聚硅氧烷树脂粘结剂，粘土，滑石或它们的任何两种或多种的混合物。
在一个具体实施方案中，硅石源是聚硅氧烷树脂粘结剂且聚硅氧烷树脂粘结剂的溶剂是异丙醇或二元酯。
本发明的方法的一个实施方案包括首先将任选掺杂的氧化铝或它的前体与该溶液掺混和随后将沸石型分子筛，非沸石型分子筛或它们的任何两种或多种的混合物和无机纤维掺混的步骤。
用于本发明的方法中的有机助剂可以是选自纤维素衍生物，有机增塑剂，润滑剂和水溶性树脂中的一种或多种。合适的纤维素衍生物的例子包括纤维素醚类，后者选自甲基纤维素，乙基纤维素，羧甲基纤维素，乙基羟乙基纤维素，羟乙基纤维素，羟基丙基纤维素，甲基羟基乙基纤维素，甲基羟基丙基纤维素和它们的任何两种或多种的组合物。纤维素衍生物提高最终产品的孔隙度，这对于固体催化剂主体的催化活性是有利的。最初，纤维素在水悬浮液中溶胀，但是在煅烧过程中最终被除去。
用于本发明的方法中的有机增塑剂选自聚乙烯醇，聚乙烯醇缩丁醛，离聚物，丙烯酸类，共聚乙烯/丙烯酸，聚氨酯，热塑性弹性体，较低分子量聚酯，亚麻子油，蓖麻油酸酯和它们的任何两种或多种的组合。
该水溶性树脂能够是聚丙烯酸酯。
用于本发明的方法中的润滑剂选自乙二醇，硬脂酸，硬脂酸钠，甘油和甘醇类中的至少一种。
取决于挤出物组合物的组成，pH可以是酸性或碱性。当该方法使用酸性水溶液时，溶液的pH值可在3和4之间。希望的是，使用乙酸来酸化该溶液。
当该方法使用碱性水溶液时，溶液的pH值可以在8和9之间。氨可用于将pH调节到碱性侧。
根据另一方面，本发明提供处理来自车辆的内燃机的废气排放物的方法，该方法包括使废气与本发明的三效尾气净化催化剂接触。废气与催化剂接触的温度优选>100℃，如>150℃，>175℃，>200℃，>225℃，>250℃，>275℃或>300℃。优选，废气接触催化剂的温度<600℃，如<550℃，<525℃或<500℃。
根据另一个方面，本发明提供用于内燃机的排气系统，该排气系统包括本发明的三效尾气净化催化剂。
根据另一方面，本发明提供包括内燃机和本发明的排气系统的车辆例如汽车。在优选的实施方案中，该内燃机是强制点火发动机，例如火花点火发动机。此类发动机典型地使用汽油燃料，但是也可以使用包括汽油和乙醇等的掺混物的“替代”燃料。
为了让本发明可得到更完全地理解，提供下列实施例，仅仅为了举例说明的目的并且参考附图，其中：
图１是显示了用于分析实施例2的三效尾气净化催化剂的活性的实验性测试出程序的图；
图2是将实施例2的三效尾气净化催化剂和实施例3的对比三效尾气净化催化剂两者在实施例4的测试中的出口处累积烃进行比较的图；
图3是将通过使用各种孔隙改性剂所制备的各种V2O3/WOx-TiO2过滤材料的孔隙体积和孔隙度相对于在穿流式构型中所使用的对照产品进行比较的图；和
图4是，相对于V2O5/WOx-TiO2对照物和商购的壁流式过滤基基底，几种的孔隙改性剂的孔隙体积与孔隙半径所作的图。
实施例1-挤出沸石整块基底
挤出沸石整块基底是按照与在US 7,507,684中公开的方法类似的方法制备的。将氢形式的粉末状商购β沸石与玻璃纤维、高岭土填料和粉末状合成品勃姆石(Pural SB)混合，然后通过与纤维素(CMC-QP10000H)，增塑剂Zusoplast(Zschimmer & Schwarz GmbH &Co KG的商标名称)和有机助剂PEO Alkox(聚氧化乙烯)掺混，在具有5-6的pH值的水溶液中加工成可成形和流动的滑移催化剂(slip)。对起始原料的定量比例进行选择，使得成品固体催化剂主体的活性材料含有69wt%的沸石，23wt%的γ-Al2O3，5wt%的玻璃纤维和3wt%的高岭土。可成形的混合物被挤出成 1”直径x 3”长的穿流式蜂窝催化剂主体，即具有连续通道和具有圆形横截面，显示300 cpsi或400 cpsi(泡孔数/每平方英寸)的泡孔密度。随后，该催化剂主体按照在WO 2009/080155中描述的方法在2mbar下冷冻干燥1小时(该专利的全部内容通过引入结合于本文中)和在580℃的温度下煅烧以形成固体催化剂主体。
实施例2-在挤出沸石基底整块上的单层三效尾气净化催化剂
通过使用在WO 99/47260中公开的方法在实施例1的300 cpsi和400 cpsi 1”x 3”挤出沸石整块基底样品上洗涂(washcoated)单层的三效尾气净化催化剂组合物，该组合物包括大部分的γ-氧化铝与承载钯(占主要部分)和铑的二氧化铈-二氧化锆的混合氧化物的混合物，该文献的全部内容通过引入结合于本文中，所述方法即涂布整块载体的方法，该方法包括以下步骤(a)将容器置于整块载体的表面之上；(b)将预定量的液体组分计量加入到容器中，其中步骤(a)和(b)的顺序是(a)然后(a)或(b)然后(a)；和(c)施加真空以将全部量的液体组分抽到整块载体的至少一部分中，和将全部量的液体组分保留在整块载体之内，但没有循环(recycle)。所得产物在600℃下干燥和煅烧。
对比实施例3
两层三效尾气净化催化剂
300 cpsi的商购的堇青石整块基底(根据在WO 99/47260中的技术)以2.00 g in-3洗涂包括β沸石和胶态硅石粘结剂的第一层，随后在600℃下干燥和煅烧。根据实施例2的第二种三效尾气净化催化剂层是在洗涂剂(washcoat)中作为覆盖层涂布在第一β沸石层上。所得产物在600℃下干燥和煅烧。从涂布的整体单块基底上裁切1"x 3"核。
实施例4-三效尾气净化催化剂试验
实施例2和对比实施例3的催化剂样品使用实验室合成催化剂活性试验(SCAT)装备来测试，根据以下步骤：
(i) 在含5% O2的N2氛围(平衡)中在500℃下贫乏(Lean)预处理15分钟，然后在N2中冷却到30℃；
(ii) 在催化剂旁通管中以16L/min(25K/h SV)的0.15% HC(由甲苯17vol%；异戊烷24vol%；和丙烯59vol%组成)，0.1% CO，10% H2O蒸气和平衡压缩空气来建立基线进料(baseline feed)；
(iii) 开始数据收集和等待30秒；
(iv) 输送HC进料(feed)到样品中以在30℃-40℃下维持30秒吸附；
(iv) 经由催化剂旁通管输送气体进料；
(v) 从进料中除去空气、HC和CO，并且用N2重新平衡以便维持16L/分钟；
(vi) 将气体进料再次引入到样品中并且以40℃/分钟将温度从30℃提高至550℃；
(vii) 终止数据收集；冷却到30℃，让N2流过样品；和
(viii) 将气流引向旁通管。
这一试验程序也用绘图方式显示在图1中，从它可看出在旁通步骤中的出口温度最初提高超过了入口温度，但是在其它阶段中入口温度和出口温度是步调一致的。
实施例2和对比实施例3的催化剂样品的结果示于图2中，从该图能够看出，与对比实施例3样品相比，实施例2的催化剂样品显示出明显改进的HC转化率(400 cpsi实施方案的HC转化率为54%，300 cpsi实施方案的HC转化率为55%，与46%相比)。
实施例5-挤出沸石整体单块基底
按照与在US 7,507,684中公开的方法类似的方法制备替代实施例1的挤出沸石整体单块基底。将氢形式的粉末状商购β沸石(Tosoh)与玻璃纤维(Vetrotex 4,5mm(Saint-Gobain))，低碱性粘土填料和粉末合成勃姆石(Pural SB)混合，在具有5-6的pH值的水溶液中通过与8wt%纤维素(基于无机固体总含量)(CVP-M-5280(Dow Wolff Cellulosics))掺混被加工成可成形和流动的滑移催化剂(slip)。对起始原料的定量比例进行选择，使得成品固体催化剂主体的活性材料含有60wt%的沸石，25wt%的粘土，7wt%的γ-Al2O3和8wt%的玻璃纤维。可成形的混合物被挤出成穿流式蜂窝催化剂主体，即在所需的泡孔密度下具有连续的通道和具有圆形的衡截面。随后，该催化剂主体按照在WO 2009/080155中描述的方法在2mbar下冷冻干燥1小时(该专利的全部内容通过引入结合于本文中)和在580℃的温度下煅烧以形成固体催化剂主体。
实施例6-挤出V
2
O
5
/WOx-TiO
2
过滤器
通过将如表1中列出的组分A，B，F和S与水掺混形成可搓捏的浆状物，与实施例1和5类似地制备对照挤出V2O5/WOx-TiO2固体主体。加入添加剂H(孔隙改性剂)，该材料被捏合10 min以分散孔隙改性剂。所得到的组合物按照在实施例1和5中所述的方法挤出、干燥和煅烧。应该指出的是，在最终的煅烧制品中存在的无机固体的百分含量是100%。在煅烧过程中通过燃烧所除去的添加剂(这里H和S)的量是以相对于100%无机固体含量的wt%来提供的。
表1
A1 = TiW (98,9%, MC 10/Cristal)
A2 = V2O5 ，从AMV获得 (78% V2O5, GFE)
B1 = 膨润土 (90%, ACE/Mizuka)
B2 = 高岭土 (97,9% TK0177/Thiele)
B3 = SiO2 (100%, Tixosil/Novus)
F1 = 玻璃纤维 (Vetrotex 4,5 mm/Saint Gobain)
H1 = 纤维素 (QP10000H/Nordmann)
H2 = PEO (Alkox/Alroko)
H3 = Zusoplast (Zschimmer&Schwarz)
S1 = MEA (Imhoff & Stahl)
S2 = NH3
S3 = C3H6O3 (Fauth)
使用下列孔隙改性剂，代替表1中的挤出添加剂H1、H2和H3，其中所显示的量是相对于表1的配方中无机固体的总重量。
表2
孔隙度和孔隙容积和孔隙半径能够例如使用压汞孔隙率测定法来测量。
包括孔隙容积和孔隙度的表2项目的结果也列出在图3中。从这些结果能够看出，对照物的孔隙度和孔隙容积能够通过孔隙改性剂的合适选择来提高，因此采用这些孔隙改性剂所制备的挤出固体主体可用于壁流式过滤器的制造。
这些结果一般针对提高孔隙度，孔隙容积等等性能，与固体挤出主体的活性组分无关。也就是说，虽然提高此实施例6的孔隙度和孔隙容积等等是使用V2O5/WOx-TiO2活性材料来举例说明的，但是公开在此实施例6中的提高孔隙度和孔隙容积等等的原理适用于任何活性材料的挤出，例如，用于包括三效尾气净化催化剂的汽油烟灰过滤器中的挤出固体主体，因为孔隙改性剂在煅烧过程中烧尽而将活性材料和填料等等作为无机固体保留下来。
图4将不同对照物的孔隙容积与使用表2中列出的其它孔隙改性剂所制备的固体挤出V2O5/WOx-TiO2材料进行对比，也与商购的壁流式过滤器(NGK)对比。从图能够看出，孔隙改性剂的包含改进了对照挤出固体主体的孔隙度和孔隙容积，因此这些材料具有与商购的壁式过滤器的那些性能接近的性能。
实施例7-挤出催化烟灰过滤器
这是预示的实施例。催化的壁流式滤器整块基底能够如下制备。可将合适量的CeO2-ZrO2混合氧化物与玻璃纤维，粉末状合成勃姆石(Pural SB)和β沸石混合，并且在具有3.5的pH值的水溶液中加工成可成形和流动的滑移催化剂(slip)，其含有1.2wt%纤维素(CMC-QP10000H)，1.0wt%的有机助剂PEO Alkox(聚氧化乙烯)和13wt%的由孔隙改性剂Rettenmaier BC200和聚丙烯腈(PAN)纤维组成的混合物。对起始原料的定量比例进行选择，使得成品固体催化剂主体的活性材料含有25wt%的CeO2-ZrO2，15wt%β沸石，52wt%的γ-Al2O3和8wt%的玻璃纤维。可成形的混合物可被挤出成蜂窝催化剂主体，具有连续通道和具有圆形横截面，显示有300 cpsi的泡孔密度(泡孔数/每平方英寸)。随后，该催化剂主体按照在WO 2009/080155中描述的方法在2mbar下冷冻干燥1小时(该专利的全部内容通过引入结合于本文中)和在580℃的温度下煅烧以形成固体催化剂主体。典型地，可以预期所得的产品将具有约10微米的平均孔隙尺寸。
包括多个通道的挤出的穿流式整块基底可以被制成壁流式过滤器排列，其中多个第一通道在上游端被堵塞和在上游端没有被堵塞的多个第二通道在下游端被堵塞，其中第一和第二通道的排列应该使得：通过按照EP 1837063(其全部内容通过引入结合于本文中)以所需图案在通道的末端插入基本上不透气的栓塞(plug)，侧向和垂直方向相邻通道是按照棋盘的外观在相对的末端被堵塞。该过滤器排列也公开在SAE 810114中(其全部内容通过引入结合于本文中)。煅烧的挤出整块基底能够按照在WO99/47260或PCT/050005(2011年1月4日提交)中公开的方法，涂布包含Pt-Rh的洗涂剂。后一种方法包括以下步骤：(i)将蜂窝整块基底保持基本上垂直；(ii)经由在基底的下端上的通道的开放端将预定量的液体引入到基底中；(iii)将所引入的液体密封保留在基底之内；(iv)颠倒含有该保留液体的基底；和(v)在基底的颠倒下端对于基底的通道的开放端施加真空，以便沿着基底的通道汲取该液体。
为了避免任何怀疑，在这里列举的任何和全部文件的全部内容通过引入结合于本文中。
Claims (35)
1.包括挤出固体主体的三效尾气净化催化剂，所述挤出固体主体包括：
10-100wt%的至少一种粘结剂/基质组分；
5-90wt%的沸石型分子筛，非沸石型分子筛或它们的任何两种或多种的混合物；和
0-80wt%的任选稳定化的二氧化铈，
所述催化剂包括至少一种贵金属和任选的至少一种非贵金属，其中：
(i) 所述至少一种贵金属被承载于所述挤出固体主体的表面上的一个或多个涂层中；
(ii) 至少一种金属存在于整个挤出固体主体中并且至少一种贵金属也被承载于在所述挤出固体主体的表面上的一个或多个涂层中；或
(iii) 至少一种金属存在于整个挤出固体主体中，以更高的浓度存在于所述挤出固体主体的表面上并且至少一种贵金属也被承载于在所述挤出固体主体的表面上的一个或多个涂层中。
2.根据前述权利要求中任一项的催化剂，其中所述至少一种金属与所述沸石型分子筛组分、所述非沸石型分子筛组分或者所述混合物中的沸石型分子筛组分和非沸石型分子筛组分中的任何一种或两种相结合。
3.根据权利要求2的催化剂，其中所述挤出固体主体包括与所述沸石型分子筛组分、所述非沸石型分子筛组分或者所述混合物中的沸石型分子筛组分和非沸石型分子筛组分中的任何一种或两种相结合的至少一种第一金属，以及不与所述沸石型分子筛组分、所述非沸石型分子筛组分或者所述混合物中的沸石型分子筛组分和非沸石型分子筛组分中的任何一种或两种相结合的至少一种第二金属。
4.根据权利要求1、2或3的三效尾气净化催化剂，其中整个挤出固体主体中但不与所述沸石型分子筛组分、所述非沸石型分子筛组分或者所述混合物中的沸石型分子筛组分和非沸石型分子筛组分中的任何一种或两种相结合的所述至少一种金属；在位于所述挤出固体主体的表面上的大部分的至少一种金属中的所述至少一种金属；在所述挤出固体主体的表面上的一个或多个涂层中的所述至少一种金属；或以较高的浓度在所述挤出固体主体的表面上的所述至少一种金属包括选自碱金属、碱土金属、镧系元素或者这些中任何两种或多种的混合物中的至少一种金属。
5.根据权利要求1、2、3或4的三效尾气净化催化剂，其中所述贵金属选自Pt，Au，Ag，Ir，Ru，Rh，Pd和Os。
6.根据权利要求4的三效尾气净化催化剂，其中所述镧系元素金属选自La、Pr和Ce。
7.根据权利要求4的三效尾气净化催化剂，其中所述碱金属是Cs。
8.根据前述权利要求中任一项的三效尾气净化催化剂，其中整个挤出固体主体上但不与所述沸石型分子筛组分、所述非沸石型分子筛组分或者所述混合物中的沸石型分子筛组分和非沸石型分子筛组分中的任何一种或两种相结合的金属总含量；在位于所述挤出固体主体的表面上的大部分的至少一种金属中的金属总含量；在所述挤出固体主体的表面上的一个或多个涂层中的金属总含量；或以较高的浓度在挤出固体主体的表面上的金属总含量是0.1-30wt%。
9.根据前述权利要求中任一项的三效尾气净化催化剂，其中所述挤出固体主体包括：
10-100wt%的堇青石，氮化物，碳化物，硼化物，金属互化物，硅铝酸锂，任选掺杂的氧化铝，硅石源，二氧化钛，二氧化锆，二氧化钛-二氧化锆，锆英石和它们的任何两种或多种的混合物；
0-80wt%的尖晶石；
5-90wt%的沸石型分子筛，非沸石型分子筛或它们的任何两种或多种的混合物，各自任选含有一种或多种金属；
0-80wt%的任选稳定化的二氧化铈；和
0-25wt%的无机纤维。
10.根据权利要求9的三效尾气净化催化剂，其中所述挤出固体主体基本上由以下组成：
10-100wt%的堇青石，氮化物，碳化物，硼化物，金属互化物，硅铝酸锂，尖晶石，任选掺杂的氧化铝，硅石源，二氧化钛，二氧化锆，二氧化钛-二氧化锆，锆英石和它们的任何两种或多种的混合物；
50-90wt%的沸石型分子筛，非沸石型分子筛或它们的任何两种或多种的混合物，各自任选含有一种或多种金属；和
0-25wt%的无机纤维。
11.根据权利要求9的三效尾气净化催化剂，其中所述挤出固体主体基本上由以下组成：
10-100wt%的堇青石，氮化物，碳化物，硼化物，金属互化物，硅铝酸锂，任选掺杂的氧化铝，尖晶石，硅石源，二氧化钛，二氧化锆，二氧化钛-二氧化锆，锆英石和它们的任何两种或多种的混合物；
5-50wt%的沸石型分子筛，非沸石型分子筛或它们的任何两种或多种的混合物，各自任选含有一种或多种金属；
20-80wt%的任选稳定化的二氧化铈；和
0-25wt%的无机纤维。
12.根据前述权利要求中任一项的三效尾气净化催化剂，其为壁流式过滤器的形式。
13.根据权利要求12的三效尾气净化催化剂，其中所述壁流式过滤器的孔隙度是30-80%。
14.根据前述权利要求中任一项的三效尾气净化催化烟灰过滤器，其包括壁流式过滤器构型的挤出固体主体，所述挤出固体催化剂主体基本上由以下组成：
15-70wt%的堇青石，氮化物，碳化物，硼化物，金属互化物，硅铝酸锂，尖晶石，任选掺杂的氧化铝，二氧化钛，二氧化锆，二氧化钛-二氧化锆，锆英石和它们的任何两种或多种的混合物；
0-20wt%的硅石源；
5-50wt%的沸石型分子筛，非沸石型分子筛或它们的任何两种或多种的混合物，各自任选含有一种或多种金属；
20-80wt%的任选稳定化的二氧化铈；和
0-20wt%的无机纤维，所述挤出固体催化剂主体涂布有包括承载的至少一种贵金属以及任何两种或多种贵金属的组合的一个或多个涂层。
15.根据权利要求1到13中任一项的三效尾气净化催化剂，其包括穿流式构型的挤出固体主体，所述挤出固体主体基本上由以下组成：
15-30wt%的堇青石，氮化物，碳化物，硼化物，金属互化物，硅铝酸锂，尖晶石，任选掺杂的氧化铝，二氧化钛，二氧化锆，二氧化钛-二氧化锆，锆英石和它们的任何两种或多种的混合物；
0-20wt%的硅石源；
50-81wt%的沸石型分子筛，非沸石型分子筛或它们的任何两种或多种的混合物，各自任选含有一种或多种金属；和
0-20wt%的无机纤维，所述挤出固体催化剂主体涂布有单层，所述单层包括大部分γ-氧化铝和仅仅承载钯的、承载钯和铑的混合物的、承载铂和铑的混合物的或承载铂、钯和铑的混合物的稳定化二氧化铈的混合物。
16.根据前述权利要求中任一项的三效尾气净化催化剂，其中所述至少一种粘结剂/基质组分选自堇青石，氮化物，碳化物，硼化物，金属互化物，硅铝酸锂，尖晶石，任选掺杂的氧化铝，硅石源，二氧化钛，二氧化锆，二氧化钛-二氧化锆，锆英石和它们的任何两种或多种的混合物。
17.根据前述权利要求中任一项的三效尾气净化催化剂，其中尖晶石是MgAl2O4或其中Mg部分地被选自Co、Zr、Zn或Mn中的金属所替代。
18.根据权利要求16或17的三效尾气净化催化剂，其中所述硅石源选自硅石，氧化硅溶胶，石英，熔融硅石或无定形的硅石，硅酸钠，无定形硅铝酸盐，烷氧基硅烷，聚硅氧烷树脂粘结剂，粘土，滑石或它们的任何两种或多种的混合物。
19.根据权利要求18的三效尾气净化催化剂，其中所述粘土选自漂白土，海泡石，锂蒙脱石，蒙皂石，高岭土和它们的任何两种或多种的混合物。
20.根据权利要求16、17、18或19的三效尾气净化催化剂，其中所述无机纤维选自碳纤维，玻璃纤维，金属纤维，硼纤维，氧化铝纤维，硅石纤维，硅石-氧化铝纤维，碳化硅纤维，钛酸钾纤维，硼酸铝纤维和陶瓷纤维。
21.根据前述权利要求中任一项的三效尾气净化催化剂，其中所述沸石型分子筛或非沸石型分子筛具有如the Structure Commission of the International Zeolite Association所定义的框架型编码 ABW，AEL，AET，AFG，AFI，AFO，AFR，AFS，AFY，AHT，AST，ASV，ATN，ATO，ATS，ATV，AWO，AWW，BCT，BEA，BEC，BIK，BOF，BOG，BPH，BRE，BSV，CAN，CAS，CFI，CGF，CGS，-CHI，-CLO，CON，CZP，DAC，DFO，DOH，DON，EMT，EON，ESV，ETR，EUO，EZT，FAR，FAU，FER，FRA，GIU，GME，GON，HEU，IFR，IMF，ISV，ITH，ITR，IWR，IWS，IWV，IWW，JBW，JRY，LAU，LIO，-LIT，LOS，LOV，LTF，LTL，LTN，MAR，MAZ，MEI，MEL，MEP，MFI，MFS，MOR，MOZ，MRE，MSE，MSO，MTF，MTN，MTT，MTW，MWW，NAB，NAT，NES，NON，NPO，OBW，OFF，OSI，OSO，-PAR，PON，-RON，RRO，RSN，RTE，RUT，RWR，RWY，SAO，SAS，SBE，SBS，SBT，SFE，SFF，SFG，SFH，SFN，SFO，SFS，SGT，SOD，SOF，SOS，SSF，SSY，STF，STI，STO，STT，STW，-SVR，SZR，TER，TOL，TON，TUN，UOS，UOZ，USI，UTL，VET，VFI，VSV，WEI或-WEN和它们的任何两种或多种的混合物。
22.根据前述权利要求中任一项的三效尾气净化催化剂，其中所述沸石型分子筛是选自ZSM-5，β，镁碱沸石和它们的任何两种或多种的混合物。
23.根据前述权利要求中任一项的三效尾气净化催化剂，其中所述沸石型分子筛是10或更大的硅石与氧化铝之比为10或更大的硅铝酸盐沸石。
24.根据权利要求21、22或23中任一项的三效尾气净化催化剂，其中所述沸石分子筛或非沸石型分子筛是含有一种或多种取代框架金属的同形体。
25.根据权利要求21的三效尾气净化催化剂，其中所述非沸石型分子筛是磷铝酸盐。
26.根据前述权利要求中任一项的三效尾气净化催化剂，其中所述二氧化铈用至少一种非铈的元素稳定化，以提高二氧化铈的热稳定性。
27.根据前述权利要求中任一项的三效尾气净化催化剂，其中特征(ii)或(iii)中的(a)存在于整个挤出固体主体中的所述至少一种金属；(b)以更高的浓度存在于所述挤出固体主体的表面上的所述至少一种金属；和(c)承载于的所述挤出固体主体的表面上的一个或多个涂层之中的所述至少一种金属各自不同于在其它位置上存在的所述至少一种金属。
28.根据前述权利要求中任一项的三效尾气净化催化剂，其包括沸石型分子筛，非沸石型分子筛或它们的任何两种或多种的混合物，其中所述至少一种金属与所述沸石型分子筛组分、所述沸石型分子筛组分或所述混合物中的沸石型分子筛组分和非沸石型分子筛组分中的任何一种或两种相结合。
29.根据权利要求28的三效尾气净化催化剂，其中与所述沸石型分子筛、所述非沸石型分子筛或所述它们的任何两种或多种的混合物中的两种分子筛相结合的所述至少一种金属或至少一种金属各自含有选自过渡金属、镧系元素或它们的任何两种或多种的混合物的一种或多种金属。
30.根据权利要求29的三效尾气净化催化剂，其中过渡金属选自Cu，Pd和Ag。
31.根据权利要求28、29或30的三效尾气净化催化剂，其中与所述沸石型分子筛组分、所述非沸石型分子筛组分或者所述混合物中的沸石型分子筛组分和非沸石型分子筛组分中的任何一种或两种相结合的所述至少一种金属中的金属总含量是0.1-20wt%。
32.制造根据前述权利要求中任一项的三效尾气净化催化剂的方法，所述方法包括以下步骤：
通过混合以下这些组分的粉末状起始原料来形成固体挤出主体：至少一种粘结剂/基质组分或它们中一种或多种组分的前体；沸石型分子筛，非沸石型分子筛或它们的任何两种或多种的混合物，所述沸石型分子筛、非沸石型分子筛或者沸石型和非沸石型分子筛的混合物任选地与至少一种金属相结合；任选的任选稳定化的二氧化铈；和任选的至少一种金属化合物；与任选的无机纤维；任选地添加有机助剂；
通过在任选含有至少一种金属的金属盐的酸性或碱性水溶液中混合和/或捏合来加工成塑性复合物以形成混合物；
将所述混合物挤出成催化剂主体，干燥所述催化剂主体并煅烧以形成固体挤出主体；
选择定量比例的起始原料，以使得所述固体挤出主体包括10-100wt%的至少一种粘结剂/基质组分；5-90wt%的沸石型分子筛，非沸石型分子筛或它们的任何两种或多种的混合物；和0-80wt%的任选稳定化的二氧化铈，和用含有至少一种贵金属的至少一种涂层涂布所述固体挤出主体的表面和任选还用至少一种金属浸渍所述固体挤出主体的表面。
33.处理来自静止来源或车辆的内燃机的废气排放物的方法，所述方法包括使废气与根据权利要求1-31中任一项的三效尾气净化催化剂接触。
34.内燃机的排气系统，所述排气系统包括根据权利要求1到31中任一项的三效尾气净化催化剂。
35.一种车辆，其包括内燃机和根据权利要求34的排气系统。
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105722591A (zh) * | 2013-12-04 | 2016-06-29 | 三井金属矿业株式会社 | 废气净化用催化剂及废气净化用催化剂构成体 |
| US9713805B2 (en) | 2013-12-04 | 2017-07-25 | Mitsui Mining & Smelting Co., Ltd. | Exhaust gas purification catalyst and exhaust gas purification catalyst structure |
| CN105722591B (zh) * | 2013-12-04 | 2018-09-11 | 三井金属矿业株式会社 | 废气净化用催化剂及废气净化用催化剂构成体 |
| CN106608637A (zh) * | 2015-10-27 | 2017-05-03 | 中国石油化工股份有限公司 | 一种合成stt结构分子筛的方法 |
| CN106608637B (zh) * | 2015-10-27 | 2019-02-01 | 中国石油化工股份有限公司 | 一种合成stt结构分子筛的方法 |
| CN109982777A (zh) * | 2016-10-04 | 2019-07-05 | 庄信万丰股份有限公司 | NOx吸附剂催化剂 |
| CN110366442A (zh) * | 2017-03-06 | 2019-10-22 | 揖斐电株式会社 | 蜂窝过滤器 |
| CN110270341A (zh) * | 2019-06-19 | 2019-09-24 | 福州大学 | 一种催化剂及其制备方法和应用 |
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