CN102811798B - 氧化催化剂 - Google Patents
氧化催化剂 Download PDFInfo
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- CN102811798B CN102811798B CN201180017647.XA CN201180017647A CN102811798B CN 102811798 B CN102811798 B CN 102811798B CN 201180017647 A CN201180017647 A CN 201180017647A CN 102811798 B CN102811798 B CN 102811798B
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- 239000003054 catalyst Substances 0.000 title claims abstract description 109
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- 238000007254 oxidation reaction Methods 0.000 title claims abstract description 55
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims abstract description 120
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 83
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims description 47
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- JSKIRARMQDRGJZ-UHFFFAOYSA-N dimagnesium dioxido-bis[(1-oxido-3-oxo-2,4,6,8,9-pentaoxa-1,3-disila-5,7-dialuminabicyclo[3.3.1]nonan-7-yl)oxy]silane Chemical compound [Mg++].[Mg++].[O-][Si]([O-])(O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2)O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2 JSKIRARMQDRGJZ-UHFFFAOYSA-N 0.000 claims description 17
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Abstract
包括挤出固体主体的氧化催化剂，该挤出固体主体包括：10-100％重量的至少一种粘结剂/基质组分；5-90％重量的沸石型分子筛，非沸石型分子筛或它们的任何两种或多种的混合物；和0-80％重量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)大部分的该至少一种贵金属位于该挤出固体主体的表面上；(ii)至少一种贵金属被承载于该挤出固体主体的表面上的一个或多个涂层中；(iii)至少一种金属存在于整个挤出固体主体中并且还以更高的浓度存在于该挤出固体主体的表面上；(iv)至少一种金属存在于整个的挤出固体主体中并且还以一个或多个涂层存在于该挤出固体主体的表面上；或(v)至少一种金属存在于整个的挤出固体主体中，以更高的浓度存在于挤出固体主体的表面上并且还以一个或多个涂层存在于该挤出固体主体的表面上。
Description
本发明涉及包括挤出固体主体的氧化催化剂，其用于处理来自于静止来源和移动即车辆（汽车）应用的的内燃机中的废气排放物。
汽车工程师学会(SAE)技术论文2007-01-0658的题目是“FundamentalStudyandPossibleApplicationofNewConceptHoneycombSubstrateforEmissionControl”并且公开了包括被分散在催化载体上的铂催化剂的柴油氧化催化剂(DOC)，该催化载体包括许多的由粘合剂粘结成全尺寸模块(fullsizeblock)的γ-氧化铝、无机纤维和(未命名的)粘结材料的挤出片段。铂通过常规的浸渍方法以1.0-2.7g/每升的量施加于催化载体上。
EP1739066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挤出固体主体和至少一种金属的氧化催化剂，该催化剂特别可用于内燃机废气的废气后处理领域中。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氧化催化剂，所述挤出固体主体包括：10-100％重量的至少一种粘结剂/基质组分；5-90％重量的沸石型分子筛，非沸石型分子筛或它们的任何两种或多种的混合物；和0-80％重量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)大部分的所述至少一种贵金属位于所述挤出固体主体的表面上；(ii)所述至少一种贵金属承载于所述挤出固体主体的表面上的一个或多个涂层中；(iii)至少一种金属存在于整个挤出固体主体中并且还以更高的浓度存在于所述挤出固体主体的表面上；(iv)至少一种金属存在于整个挤出固体主体中并且还承载于所述挤出固体主体的表面上的一个或多个涂层中；或(v)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还承载于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，例如从两层到单层；或单个层可一起被除去并且催化金属可承载于挤出固体主体本身的表面上。这具有降低排气系统中的回压、提高发动机的效率的益处。
此外，通过提供未涂布催化剂的可能性，挤出固体主体可在更高的泡孔密度下、提高强度和降低泡孔壁的厚度的情况下制造，这些泡孔壁可改进熄火特性和通过传质提高活性。
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-boarddiagnostics)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，Euro4:98/69/EC对柴油客车(由70/156/EEC定义的M类车辆)的OBD限制是：一氧化碳(CO)-3.2g/km；烃类(HC)-0.4g/km；氮氧化物(NOx)-1.2g/km；和颗粒物质(PM)0.18g/km。
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法规的能力。例如，Euro5：715/2007/EC对于压缩点火(柴油)客车的目前草案OBD限制是：CO-1.9g/km；非甲烷烃类(NMHC)-0.25g/km；NOx-0.54g/km；PM-0.05g/km。
在美国，认为用于汽油/火花点火发动机的催化剂监测的OBDII法规(Title13,CaliforniaCodeRegulations,Section1968.2,MalfunctionandDiagnosticSystemRequirementsfor2004andSubsequentModel-YearPassengerCars,Light-DutyTrucksandMedium-DutyVehiclesandEngines)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(theaverageFederalTestProcedure)(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体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（chequerboard）。
很显然，公开在EP1739066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“CatalyticAirPollutionControl–CommercialTechnology”,第二版,R.M.Heck等人,JohnWiley&Sons,Inc.,NewYork,2002，第7章(相对于穿流式整块)和第9章(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和在1000℃下优选>0.8。
壁流式过滤器的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氧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(最大12-环孔隙敞开结构)或烘箱介孔（ovenmeso）(>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可选自如theStructureCommissionoftheInternationalZeoliteAssociation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()或者是它们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，NSI，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30％重量CeO2，63%ZrO2，5%Nd2O3，2%La2O3；和40%CeO2，50%ZrO2，4%La2O3，4%Nd2O3和2%Y2O3。
宽泛地说，可存在于特征(iii)、(iv)和(v)中的(a)整个该挤出固体主体中（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；和/或(c)承载在特征(iii)、(iv)和(v)中的挤出固体主体的表面上的一个或多个涂层之中的至少一种金属不同于在(a)、(b)和(c)的每一个其它位置上存在的至少一种金属。因此，根据本发明，该至少一种金属可存在于位置(b)，(c)，(a)加(b)，(a)加(c)或(a)加(b)加(c)。当至少一种金属存在于(a)和(b)，(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。
本申请的发明人发现，通过用过渡金属例如铁对沸石例如β沸石进行离子交换，如随附实施例中可见，氧化催化剂的热耐久性以及活性可得到改进。
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进行结合，例如离子交换，然后第二至少一种金属可被添加到挤出物组合物中。
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。
在与所述分子筛组分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0.1-20％重量，如1-9％重量。
存在于整个的挤出固体主体中但不与所述分子筛或各分子筛相结合；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；在该挤出固体主体的表面上的一个或多个涂层中；或以更高的浓度存在于该挤出固体主体的表面上的至少一种金属可选自过渡金属、镧系金属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使用与用于该挤出固体主体的相同稳定剂来稳定化。相对于在一个或多个涂层中没有分子筛但分子筛存在于该挤出固体主体中的氧化催化剂(参见实施例3B)，除了分子筛在挤出固体主体中的存在，分子筛(沸石)在一个或多个涂层中的存在已经有利地显示可以改进烃转化率。因此，分子筛在一个或多个涂层中的存在是优选的。合适的催化金属包括贵金属(Au，Ag和铂族金属，其中包括Pt，Pd和Rh))中的一种或多种。
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（eggshell）”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族金属和VIII族金属。优选，所述贵金属或各贵金属是选自Pt，Pd，Au，Ag，Ir，Ru，Rh，Os和它们的任何两种或多种的混合物；和合适的镧系金属可以是La，Pr或Ce或它们的任何两种或多种的混合物。
在整个挤出固体主体中但不与所述分子筛组分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0.1-20％重量，如1-9％重量。
该挤出固体主体（即包括与所述分子筛或各分子筛相结合的任何金属）的金属总含量，可以是0.1-25％重量，如1-15％重量。
该催化剂作为总体（包括挤出固体主体的表面上包含至少一种金属的一个或多个涂层）的金属总含量，可以是0.1-30％重量，如1-25％重量。
至少一种粘结剂/基质组分的含量可以是>15％重量，>20％重量，>30％重量，>35％重量，>40％重量，>45％重量，>50％重量，>55％重量，>60％重量，>65％重量或>70％重量，>75％重量，>80％重量，>85％重量或>90％重量。
尖晶石的含量可以是>10%重量，>15%重量，>20%重量，>30%重量，>35%重量，>40%重量，>45%重量，>50%重量，>55%重量，>60%重量，>65%重量或>70%重量。
分子筛的总含量可以是>10%重量，>15%重量，>20%重量，>30%重量，>35%重量，>40%重量，>45%重量，>50%重量，>55%重量，>60%重量，>65%重量或>70%重量，>75%重量，>80%重量或>85%重量。
任选地稳定化的二氧化铈的含量可以是>5%重量，>10%重量，>15%重量，>20%重量，>30%重量，>35%重量，>40%重量，>45%重量，>50%重量，>55%重量，>60%重量，>65%重量或>70%重量。
无机纤维的含量可以是>5%重量，>10%重量，>15%重量或>20%重量。
在一个实施方案中，该挤出固体主体基本上由以下组成：10-100％重量的堇青石，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；50-90％重量的沸石型分子筛、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0-25％重量的无机纤维。
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：10-37％重量的堇青石，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；60-88％重量的沸石型分子筛、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0-20%重量的无机纤维；或基本上由以下组成：15-30%重量的堇青石，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；2-20%重量的硅石源；50-81%重量的沸石型分子筛、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2-10%重量的无机纤维。
在适合用于柴油氧化催化剂的另一个实施方案中，该挤出固体主体基本由以下组成：10-100％重量的堇青石，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；5-50％重量的沸石型分子筛、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；20-80％重量任选稳定化的二氧化铈；和0-25％重量的无机纤维。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：69%重量的CeO2，以及23%重量的γ-Al2O3和8%重量的玻璃纤维。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。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。
在本发明的更特别的例子中：
(i)柴油氧化催化剂包括呈现为穿流式构型(flow-throughconfiguration)的挤出固体主体，所述挤出固体主体基本上由以下组成：15-70％重量的堇青石，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；0-20％重量的硅石源；50-81％重量的沸石型分子筛，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0-20％重量的无机纤维，该挤出固体催化剂主体涂布有包含承载的Pt、Pd、Au、Pt和Pd、Pd和Au的第一内层；和包含承载的Pt、Pd、Au、Pt和Pd、Pd和Au的第二外部催化剂层；和其中当内层和外层中存在的金属相同时，则在内层中的金属负载量不同于外层中的金属负载量；和
(ii)催化的烟灰过滤器包括呈现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：15-70％重量的堇青石，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；0-20％重量的硅石源；5-50％重量的沸石型分子筛，非沸石型分子筛或它们的任何两种或多种的混合物，各任选含有一种或多种金属；20-80％重量任选稳定化的二氧化铈；和0-20％重量的无机纤维，该挤出固体催化剂主体涂覆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的一个或多个涂层；
根据另一方面，本发明提供制造本发明的氧化催化剂的方法，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，以使得该固体挤出主体包括10-100％重量的至少一种粘结剂/基质组分；5-90％重量的沸石型分子筛，非沸石型分子筛或它们的任何两种或多种的混合物；和0-80％重量的任选稳定化的二氧化铈和任选至少一种金属，和
用至少一种金属浸渍该固体挤出主体的表面和/或用含有至少一种金属的至少一种个层涂敷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EP1837063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。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其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选自如下的纤维素醚类：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。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静止来源或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氧化催化剂接触。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℃。
根据另一方面，提供了用于内燃机的排气系统，该排气系统包括本发明的氧化催化剂。该内燃机可以是压燃式发动机或强制点火(positiveignition)发动机。强制点火发动机通常使用汽油燃料燃烧，但是可使用其它燃料，包括与氧化产物掺混的汽油燃料，包括甲醇和/或乙醇、液化石油气或压缩天然气。压燃式发动机可使用柴油机燃料燃烧，柴油机燃料与生物柴油或费-托(Fischer-Tropsch)衍生燃料的掺混物，生物柴油本身或天然气本身。现代的压燃式发动机包括已知为稀释控制燃烧系统(DCCS)的那些，例如Toyota’sSmoke-lessRichCombustionconcept。也可以处理来自均匀充量压缩点火(HCCI)发动机的排放物。尤其，可以处理其中燃烧用的基本上全部的燃料在燃烧开始之前被注入到燃烧室中的现代发动机。
根据本发明另一方面，提供包括内燃机(任选如以上所定义)和本发明的排气系统的车辆。
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是在实施例6中所述的试验程序中将实施例3A和3B的650℃老化柴油氧化催化剂与实施例5A和5B的类似老化的对比柴油氧化催化剂的%烃转化活性进行比较的图；
图2是在实施例6中所述的试验程序中，将实施例3A和3B的800℃老化柴油氧化催化剂与实施例5A和5B的类似老化的对比柴油氧化催化剂的%烃转化活性随温度的变化进行比较的图；
图3是将实施例3A和4的650℃老化柴油氧化催化剂与空的堇青石穿流式基底的%烃转化活性随温度的变化进行比较的图；
图4是将实施例3C、5C和5D的一氧化碳(CO)转化活性和总烃(THC)转化活性随温度的变化进行比较的图；
图5是将使用各种孔隙改性剂所制备的各种V2O5/WOx-TiO2过滤材料与在穿流式构型中所使用的对照产品的孔隙体积和孔隙度进行比较的图；和
图6是几种孔隙改性剂，与V2O5/WOx-TiO2对照物和商购的壁流式过滤基底的孔隙体积对孔隙半径所作的图。
实施例1-含有H-β沸石的挤出沸石整块基底
挤出沸石整块基材是按照与在US7,507,684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勃姆石(PuralSB)混合，然后通过与纤维素(CMC-QP10000H)，增塑剂Zusoplast(Zschimmer&SchwarzGmbH&CoKG的商标名称)和有机助剂PEOAlkox(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69％重量的沸石，23％重量的γ-Al2O3，5％重量的玻璃纤维和3％重量的高岭土。可成形的混合物被挤出成1”直径x3”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400cpsi的泡孔密度(泡孔数/每平方英寸)。随后，该催化剂主体按照在WO2009/080155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-含有FE-β沸石的挤出沸石整块基底
将氢形式的粉末状的商购β沸石与氢氧化铁、玻璃纤维、低碱性粘土填料和粉末状合成勃姆石(PuralSB)混合，然后在具有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)。当混合物被充分塑化时，以基于100%的总无机固体含量的8％重量的量添加纤维素。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55％重量的沸石，25％重量的粘土，7％重量的γ-Al2O3，8％重量的玻璃纤维和5％重量的铁和铁化合物。可成形的混合物被挤出成1”直径x3”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400cpsi的泡孔密度(泡孔数/每平方英寸)。随后，该催化剂主体按照在WO2009/080155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)和按照在2010年8月21日提交的PCT专利申请no.PCT/EP2010/005140(其全部内容通过引入结合于本文中)中的方法在580℃的温度下还原煅烧以形成固体催化剂主体。发现，通过使用所述的方法，引入到混合物中的至少一些铁与沸石进行离子交换。
实施例3-在实施例1的挤出沸石整块基底上的两层柴油氧化催化剂
向实施例1所制备的400cpsi挤出β沸石1”x3”穿流式样品中洗涂(washcoated)(按照在WO99/47260中的技术)包括Pt和Pd/γ-氧化铝洗涂剂的混合物的第一层(实施例3A)或包括Pt和Pd/γ-氧化铝和H-β沸石的混合物的第一层(实施例3B)。所得产物被干燥和煅烧至600℃。覆盖第一层的Pt/γ-氧化铝的第二洗涂层被施涂于实施例3A和3B的每一个之上，随后将所得到的涂覆部分干燥和然后在600℃下煅烧。所存在的贵金属的比率是2Pt:Pd，具有105gin-3的总贵金属负载量。
单独的400cpsi5”x6”基底整块按照针对实施例3B所述的方法被涂覆两层催化剂，用于在实施例7中的发动机试验。该5”x6”催化剂在800℃下在5%H2O中老化50小时，并且表示为实施例3C。
实施例4-在实施例2的挤出沸石整块基底上的两层柴油氧化催化剂
实施例2的400cpsi挤出5％重量离子交换Fe-β沸石1”x3”穿流式样品按照针对实施例3A所述的方法被涂覆两层催化剂。这一样品在5%H2O中在空气氛围中在650℃下老化64小时。
对比实施例5-在堇青石整块基底上的两层柴油氧化催化剂
使用商购400cpsi堇青石基底整块代替挤出沸石整块基底来制备与实施例3A和3B相同的两层催化剂，并且从它们上裁切1”x3”核芯(分别为对比实施例5A和5B)。
单独的400cpsi5”x6”基底整块按照针对实施例3A和3B所述的方法被涂覆两层催化剂，用于在实施例7中的发动机试验。该5”x6”催化剂在800℃下在5%H2O中老化50小时，并且分别表示为实施例5C和5D。
实施例6-柴油氧化催化剂实验室试验
实施例3A和3B和对比实施例4A和4B中的每一个实施例的1"x3"样品在空气氛围中，在5%H2O中在650℃下老化64小时(结果如图1中所示)；或在5%H2O中在800℃下老化50小时(结果如图2中所示)。
在实验室合成催化剂活性试验(SCAT)装备中，使用下列合成规则贫乏(lean)条件来对各样品进行测试：扫过容积(SV)=60K，C10H22=100ppmC1，CO=200ppm，NOx=200ppm，O2=12%，CO2=5%，H2O=5%，在N2中；温度以40℃/每分钟的速率从120℃升高至400℃。
从图1和2中可以看出，与对比实施例5A和5B相比，实施例3A和3B在较低温度例如120-240℃下都显示出明显更好的烃转化活性。还可以看出，在实施例3A和3B之间，除了挤出基底之外还在内部第一层中含有H-β沸石的实施例3B比在内部洗涂层中没有H-β沸石的实施例3A表现更好。
从图3中能够看出，实施例4的催化剂具有比实施例3A的催化剂更高的烃转化活性。发明人推断出，与其中β沸石没有金属化(H-β)的挤出固体主体相比，包含包括Fe离子交换β的挤出固体主体的催化剂更有效地保持了老化活性。
实施例7-柴油氧化催化剂发动机试验
实施例3C和实施例5C和5D的催化剂依次通过将它们装配在装有发动机测功器的一种试验台安装2007合格6.4升轻重役柴油机(bench-mounted2007certified6.4litrelightheavydutydieselengine)的排气系统中来进行测试。发动机在足以产生150℃的催化剂入口温度(在100K/hr扫过容积下)的速度和扭矩速率下运转。该扭矩按照足够以15℃/每分钟的速率下使催化剂入口温度提高至350℃的总入口温度(在140K/hr扫过容积下)的线性速率提高。
在测试过程中确定催化剂上的CO%转化率和总烃(THC)%转化率并且相对于温度在附图4中作图，从附图4中可以看出，在其洗涂底层中包括沸石的实施例5D的催化剂在150℃下最初显示出合理的THC转化率，然而，在回收之前降低到低于实施例5C在200℃下的THC转化率，与在高于275℃的温度下的实施例5C等同。本申请的发明人解释了实施例5D的初始THC转化率大于实施例5C归因于在低温下的HC吸附。然而，可以看出，本发明的实施例3C的THC转化率优于在挤出基底主体中不包括沸石的实施例5C或5D。
本发明的实施例3C的CO转化率广泛地类似于实施例5C的结果，其中在低温下观察到活性的一些更好的提升(light)。
实施例8-挤出沸石整块基底
按照与在US7,507,684中公开的方法类似的方法制备替代实施例1的挤出沸石整块基底。将氢形式的粉末状商购β沸石(Tosoh)与玻璃纤维(Vetrotex4,5mm(Saint-Gobain))，低碱性粘土填料和粉末合成勃姆石(PuralSB)混合，然后在具有5-6的pH值的水溶液中通过与8％重量的纤维素(基于总无机固体含量)(CVP-M-5280(DowWolffCellulosics))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，这样成品固体催化剂主体的活性材料含有60％重量的沸石，25％重量的粘土，7％重量的γ-Al2O3和8％重量的玻璃纤维。可成形的混合物被挤出成穿流式蜂窝催化剂主体，即以所需的泡孔密度具有连续的通道和具有圆形横截面。随后，该催化剂主体按照在WO2009/080155中猫鼠的方法在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9-挤出V
2
O
5
/WOx-TiO
2
过滤器
通过将在表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类似地制备对照物挤出V2O5/WOx-TiO2固体主体。加入添加剂H(孔隙改性剂)，该材料被捏合10min以分散孔隙改性剂。将所得到的组合物按照在实施例1、2和7中所述的方法挤出、干燥和煅烧。应该注意的是，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(这里是H和S)的量是以相对于100%无机固体含量的％重量来提供的。
表1
A1=TiW(98,9%,MC10/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(Vetrotex4,5mm/SaintGobain)
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5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6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，使得这些材料具有与商购的壁流式过滤器的那些性能接近的性能。
实施例10-挤出催化的烟灰过滤器
这是预示的实施例。催化的壁流式滤器整块基底可如下制备。可将合适量的与玻璃纤维混合的CeO2-ZrO2混合氧化物，粉末状合成勃姆石(PuralSB)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1.2％重量纤维素(CMC-QP10000H)，1.0％重量的有机助剂PEOAlkox(聚氧化乙烯)和13％重量的由孔隙改性剂RettenmaierBC200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25％重量的CeO2-ZrO2，15％重量的β沸石，52％重量的γ-Al2O3和8％重量的玻璃纤维。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300cpsi的泡孔密度(泡孔数/每平方英寸)。随后，该催化剂主体按照在WO2009/080155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使得：通过按照EP1837063(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SAE810114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-Pd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 (28)
1.包括挤出固体主体的氧化催化剂，所述挤出固体主体包括：
10-95％重量的至少一种粘结剂/基质组分；
5-90％重量的沸石型分子筛，非沸石型分子筛或它们的任何两种或多种的混合物；和
0-80％重量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)大部分的所述至少一种贵金属位于所述挤出固体主体的表面上；
(ii)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；
(iii)至少一种非贵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且存在于整个挤出固体主体中并且所述至少一种贵金属以更高的浓度存在于所述挤出固体主体的表面上；或
(iv)至少一种非贵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且存在于整个挤出固体主体上并且所述至少一种贵金属承载于所述挤出固体主体的表面上的一个或多个涂层中。
2.根据权利要求1的氧化催化剂，其中与所述沸石型分子筛、非沸石型分子筛或者与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非贵金属或至少一种非贵金属各自含有选自Fe、Cu、Ce、Hf、La、Mn、V的一种或多种金属或它们的任何两种或多种的混合物。
3.根据权利要求2的氧化催化剂，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者相结合的所述至少一种金属中的金属总含量是0.1-20％重量。
4.根据前述权利要求中任一项的氧化催化剂，其中在位于所述挤出固体主体的表面上的至少一种金属的大部分中的所述至少一种贵金属；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贵金属；或以更高的浓度在所述挤出固体主体的表面上的所述至少一种贵金属选自Pt、Pd、Au、Ag、Ir、Ru、Rh和Os。
5.根据权利要求4的氧化催化剂，其中在位于所述挤出固体主体的表面上的所述至少一种金属的大部分中、在所述挤出固体主体的表面上的所述一个或多个涂层中或以更高浓度在所述挤出固体主体的表面上的金属总含量是0.1-30％重量。
6.根据权利要求1-3中任一项的氧化催化剂，其中所述挤出固体主体包括：
10-95％重量的堇青石、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；
0-80％重量的尖晶石；
5-90％重量的沸石型分子筛、非沸石型分子筛或它们的任何两种或多种的混合物，所述分子筛或各分子筛任选含有一种或多种金属；
0-80％重量的任选稳定化的二氧化铈；和
0-25％重量的无机纤维。
7.根据权利要求6的氧化催化剂，其中所述挤出固体主体基本上由以下组成：
10-95％重量的堇青石、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；
50-90％重量的沸石型分子筛、非沸石型分子筛或它们的任何两种或多种的混合物，所述分子筛或各分子筛任选含有一种或多种金属；和
0-25％重量的无机纤维。
8.根据权利要求6的氧化催化剂，其中该挤出固体主体基本上由以下组成：
10-95％重量的堇青石、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；
5-50％重量的沸石型分子筛、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；
20-80％重量的任选稳定化的二氧化铈；和
0-25％重量的无机纤维。
9.包含根据权利要求1-3中任一项的氧化催化剂的柴油氧化催化剂，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：
15-70％重量的堇青石、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；
0-20％重量的硅石源；
50-81％重量的沸石型分子筛、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
0-20％重量的无机纤维，所述挤出固体催化剂主体涂覆有包括承载的Pt、Pd、Au、Pt和Pd、Pd和Au的第一内层；和包括承载的Pt、Pd、Au、Pt和Pd、Pd和Au的第二外部催化剂层；且其中当所述内层和外层中存在的金属相同时，在所述内层与外层之间金属负载量不同。
10.包含根据权利要求1-3中任一项的氧化催化剂的催化烟灰过滤器，其包括壁流式过滤器构型的挤出固体主体，所述挤出固体主体基本上由以下组成：15-70％重量的堇青石、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；0-20％重量的硅石源；5-50％重量的沸石型分子筛、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；20-80％重量任选稳定化的二氧化铈；和0-20％重量的无机纤维，所述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的一个或多个涂层。
11.根据权利要求1-3中任一项的氧化催化剂，其为壁流式过滤器的形式。
12.根据权利要求11的氧化催化剂，其中所述壁流式过滤器的孔隙度是30-80％。
13.根据权利要求1-3中任一项的氧化催化剂，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。
14.根据权利要求13的氧化催化剂，其中所述尖晶石是MgAl2O4或其中Mg部分地被选自Co、Zr、Zn或Mn的金属所替代。
15.根据权利要求13的氧化催化剂，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。
16.根据权利要求15的氧化催化剂，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。
17.根据权利要求6的氧化催化剂，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。
18.根据权利要求1-3中任一项的氧化催化剂，其中所述沸石型分子筛或所述非沸石型分子筛具有如theStructureCommissionoftheInternationalZeoliteAssociation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。
19.根据权利要求18的氧化催化剂，其中所述沸石型分子筛或所述非沸石型分子筛具有框架型编码BEA、FER、MFI或是它们的任何两种或多种的混合物。
20.根据权利要求1-3中任一项的氧化催化剂，其中所述沸石型分子筛是硅石与氧化铝之比为10或更大的硅铝酸盐沸石。
21.根据权利要求1-3中任一项的氧化催化剂，其中所述沸石分子筛或所述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。
22.根据权利要求21的氧化催化剂，其中所述沸石型分子筛或所述非沸石型分子筛是在其框架中包括Fe的BEA。
23.根据权利要求18的氧化催化剂，其中所述非沸石型分子筛是磷铝酸盐。
24.根据权利要求1-3中任一项的氧化催化剂，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。
25.制造根据权利要求1-8和11-24中任一项的氧化催化剂的方法，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10-95％重量的至少一种粘结剂/基质组分；5-90％重量的沸石型分子筛，非沸石型分子筛或它们的任何两种或多种的混合物；和0-80％重量的任选稳定化的二氧化铈和任选至少一种非贵金属，和
用至少一种贵金属浸渍所述固体挤出主体的表面和/或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。
26.处理来自静止来源或车辆的内燃机的废气排放物的方法，所述方法包括使所述废气与根据权利要求1-8和11-24中任一项的氧化催化剂接触。
27.内燃机的排气系统，所述排气系统包括根据权利要求1-8和11-24中任一项的氧化催化剂。
28.一种车辆，其包括内燃机和根据权利要求27的排气系统。
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| CN100998941A (zh) * | 2007-01-04 | 2007-07-18 | 华东理工大学 | 一种前置催化剂及其制备方法 |
| CN101322941A (zh) * | 2007-06-13 | 2008-12-17 | 曾庆琳 | 节能型汽车尾气净化纳米催化剂 |
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