CN108246353A - 冷起动催化剂和它在排气系统中的应用 - Google Patents

冷起动催化剂和它在排气系统中的应用 Download PDF

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Publication number
CN108246353A
CN108246353A CN201810037335.9A CN201810037335A CN108246353A CN 108246353 A CN108246353 A CN 108246353A CN 201810037335 A CN201810037335 A CN 201810037335A CN 108246353 A CN108246353 A CN 108246353A
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Prior art keywords
catalyst
zeolite
cold start
zeolites
metal
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CN201810037335.9A
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H-Y·陈
S·穆拉
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Johnson Matthey PLC
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Johnson Matthey PLC
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    • B01D53/9445—Simultaneously removing carbon monoxide, hydrocarbons or nitrogen oxides making use of three-way catalysts [TWC] or four-way-catalysts [FWC]
    • B01D53/945—Simultaneously removing carbon monoxide, hydrocarbons or nitrogen oxides making use of three-way catalysts [TWC] or four-way-catalysts [FWC] characterised by a specific catalyst
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Abstract

公开了一种冷起动催化剂。该冷起动催化剂包含沸石催化剂和负载的铂族金属催化剂。该沸石催化剂包含贱金属、贵金属和沸石。该负载的铂族金属催化剂包含一种或多种铂族金属和一种或多种无机氧化物载体。本发明还包括一种排气系统，其包括该冷起动催化剂。该冷起动催化剂和该方法得到了在冷起动期间改进的NOx储存和NOx转化，改进的烃储存和转化，和改进的CO氧化。

Description

冷起动催化剂和它在排气系统中的应用
本申请是基于申请号为201280031306.2、申请日为2012年5月31日、发明名称为“冷起动催化剂和它在排气系统中的应用”的中国专利申请的分案申请。
发明领域
本发明涉及一种冷起动催化剂和它在内燃机排气系统中的应用。
发明背景
内燃机产生了含有多种污染物的废气，包括氮氧化物(“NOx”)、一氧化碳和未燃烧的烃，其是政府立法的主题。排放控制系统被广泛用于降低这些污染物排放到大气中的量，并且一旦它们达到了它们的运行温度(典型地为200℃和更高)，则通常实现非常高的效率。但是这些系统在低于它们的运行温度，例如在“冷起动”期间是相对低效的。
因为甚至更严格的国家和地区立法降低了可以从柴油机或者汽油机排放的污染物的量，因此降低冷起动期的排放正在变成一个主要的挑战。因此，持续开发了用于降低在冷起动条件过程中NOx和烃的排放水平的方法。
对于冷起动烃控制来说，已经研究了基于沸石的烃捕集组分。在这些系统中，沸石在起动期间吸收和储存烃，并且当废气温度高到足以解吸烃时则释放出所储存的烃。随后当下游催化组分达到它们的运行温度时，该解吸的烃被转化。
对于冷起动NOx控制来说，特别是在贫燃条件下，已经研究了NOx储存和释放催化剂。该催化剂在预热期间吸附NOx和在更高的废气温度热解吸NOx。下游催化剂(例如选择性催化还原(“SCR”)或者NOx吸附剂催化剂(“NAC”))有效地将解吸的NOx还原成氮。
典型地，NOx吸附剂材料由无机氧化物组成，例如氧化铝、二氧化硅、氧化铈、氧化锆、二氧化钛或者混合氧化物，其涂覆有至少一种铂族金属。PCT国际申请WO 2008/047170公开了一种系统，其中来自贫燃废气的NOx在低于200℃的温度被吸附，随后在高于200℃热解吸。据教导，该NOx吸附剂的组成为钯和氧化铈或者混合氧化物或复合氧化物，其含有铈和至少一种其他的过渡金属。
PCT国际申请WO 2004/076829公开了一种废气净化系统，其包括排列在SCR催化剂上游的NOx储存催化剂。该NOx储存催化剂包括至少一种碱金属、碱土金属或者稀土金属，其用至少一种铂族金属(Pt、Pd、Rh或者Ir)涂覆或者活化。据教导，一种特别优选的NOx储存催化剂包括用铂涂覆的氧化铈，和基于氧化铝的载体上作为氧化催化剂的另外的铂。EP1027919公开了一种NOx吸附剂材料，其包含多孔载体材料，例如氧化铝、沸石、氧化锆、二氧化钛和/或氧化镧，和至少0.1wt％的贵金属(Pt，Pd和/或Rh)。一个例子是负载在氧化铝上的铂。
另外，美国专利5,656,244和5,800,793描述了一种系统，其组合了NOx储存/释放催化剂与三效催化剂。据教导，该NOx吸附剂包含了铬、铜、镍、锰、钼或钴以及其他金属的氧化物，其负载在氧化铝、莫来石、堇青石或者碳化硅。PCT国际申请WO 03/056150描述了一种系统，其组合了低温NO2捕集材料和烟灰过滤器。据教导，该低温NO2捕集材料包含用贱金属阳离子交换的沸石，并且该沸石选自ZSM-5、ETS-10、Y-沸石、β沸石、镁碱沸石、丝光沸石、硅酸钛和磷酸铝，该贱金属选自Mn、Cu、Fe、Co、W、Re、Sn、Ag、Zn、Mg、Li、Na、K、Cs、Nd和Pr。
不幸的是，这些系统的NOx吸附能力不够高，特别是在高NOx储存效率时更是如此。由于日益严格的全球立法对于从内燃机排放到大气中的NOx和烃的量的管控，因此一直存在着对于在冷起动条件过程中更有效清洁废气的需求。
对于任何汽车系统和工艺，需要实现在废气处理系统中、特别是在冷起动条件下的更进一步的改进。我们已经发现一种新的冷起动催化剂，其提供对于来自内燃机的废气的增强的清洁。
发明内容
本发明是一种用于排气系统的冷起动催化剂。该冷起动催化剂包含沸石催化剂和负载的铂族金属催化剂。该沸石催化剂包含贱金属、贵金属和沸石。该负载的铂族金属催化剂包含一种或多种铂族金属和一种或多种无机氧化物载体。本发明还包括一种排气系统，其包括冷起动催化剂。该冷起动催化剂通过改进的NOx储存和NOx转化，改进的烃储存和转化以及改进的CO氧化，有效地降低了冷起动期内的排放。
具体实施方式
本发明的冷起动催化剂包含沸石催化剂和负载的铂族金属催化剂。该沸石催化剂包含贱金属、贵金属和沸石。该贱金属优选是铁、铜、锰、铬、钴、镍、锡或其混合物；更优选是铁、铜、锰、钴或其混合物。特别优选铁。贵金属优选是钯、铂、铑、银或其混合物；更优选是钯、铂、铑或其混合物。特别优选钯。
沸石可以是任何天然或合成沸石，包括分子筛，和优选包含铝、硅和/或磷。沸石典型地具有通过共享氧原子而连接的SiO4、AlO4和/或PO4的三维排列。沸石骨架典型地是阴离子的，其通过电荷补偿性阳离子而平衡，该阳离子典型地是碱金属和碱土金属元素(例如Na、K、Mg、Ca、Sr和Ba)以及质子。可以将其他金属(例如Fe、Ti和Ga)引入沸石骨架中来制备引入金属的沸石。例如，铁可以代替β沸石骨架中的铝，来制备铁-β沸石(Fe-β沸石)。
沸石优选是β沸石、八面沸石(例如X-沸石或Y-沸石、包括NaY和USY)、L-沸石、ZSM沸石(例如ZSM-5、ZSM-48)、SSZ-沸石(例如SSZ-13、SSZ-41、SSZ-33)、丝光沸石、菱沸石、硅铝钾沸石、毛沸石、斜发沸石、硅质岩、磷酸铝沸石(包括金属铝磷酸盐，例如SAPO-34)、中孔沸石(例如MCM-41、MCM-49、SBA-15)、引入金属的沸石或者其混合物；更优选该沸石是β沸石、ZSM-5沸石、Fe-β沸石、或SSZ-33、或Y-沸石。该沸石最优选β沸石、ZSM-5沸石、Fe-β沸石或SSZ-33。
沸石催化剂可以通过任何已知手段来制备。例如，贱金属和贵金属可以通过任何已知手段加入该沸石来形成沸石催化剂，添加方式不是特别关键。例如，贵金属化合物(例如硝酸钯)和贱金属化合物(例如硝酸铁)可以通过浸渍、吸附、离子交换、初始润湿、沉淀等负载在沸石上。贵金属化合物和贱金属化合物可以在一个步骤中同时加入沸石中，或者在两个或多个步骤中依次加入。
负载的铂族金属催化剂包含一种或多种铂族金属(“PGM”)和一种或多种无机氧化物载体。PGM可以是铂、钯、铑、铱或其组合，和最优选铂和/或钯。无机氧化物载体最通常包括第2、3、4、5、13和14族元素的氧化物。有用的无机氧化物载体优选的表面积是10-700m2/g，孔体积是0.1-4mL/g，和孔直径是约10-1000埃。无机氧化物载体优选是氧化铝、二氧化硅、二氧化钛、氧化锆、氧化铈、氧化铌、钽氧化物、钼氧化物、钨氧化物或者其任意两种或更多种的混合氧化物或复合氧化物，例如二氧化硅-氧化铝、氧化铈-氧化锆或氧化铝-氧化铈-氧化锆。特别优选氧化铝和氧化铈。
负载的铂族金属催化剂可以通过任意已知手段来制备。优选将一种或多种铂族金属通过任何已知手段加载到一种或多种无机氧化物上，来形成负载的PGM催化剂，添加手段不是特别关键。例如，铂化合物(例如硝酸铂)可以通过浸渍、吸附、离子交换、初始润湿、沉淀等负载到无机氧化物上。其他金属也可以加入到负载的PGM催化剂上。
本发明的冷起动催化剂可以通过现有技术中公知的方法来制备。沸石催化剂和负载的铂族金属催化剂可以物理混合来生成冷起动催化剂。优选冷起动催化剂进一步包含流通式基体或者过滤器基体。在一个实施方案中，将沸石催化剂和负载的铂族金属催化剂涂覆到流通式或者过滤器基体上，和优选使用修补基面涂覆工序沉积到流通式或者过滤器基体上，来生成冷起动催化剂体系。
流通式或者过滤器基体是可以含有催化剂组分的基体。该基体优选是陶瓷基体或金属基体。陶瓷基体可以由任何合适的耐火材料制成，例如氧化铝、二氧化硅、二氧化钛、氧化铈、氧化锆、氧化镁、沸石、氮化硅、碳化硅、硅酸锆、硅酸镁、铝硅酸盐、金属铝硅酸盐(例如堇青石和锂辉石)、或其任意两种或更多种的混合物或混合氧化物。特别优选堇青石(铝硅酸镁)和碳化硅。
金属基体可以由任何合适的金属制成，特别是耐热金属和金属合金，例如钛和不锈钢以及含有铁、镍、铬和/或铝以及其他痕量金属的铁素体合金。
流通式基体优选是具有蜂窝结构的流通式整料，其具有许多小的、平行的薄壁通道，该通道轴向穿过基体，并且从基体的入口或出口延伸通过整个基体。该基体的通道横截面可以是任何形状，但是优选是正方形、正弦曲线状、三角形、矩形、六边形、梯形、圆形或者椭圆形。
过滤器基体优选是壁流式整料过滤器。壁流式过滤器的通道交替阻断，这样使废气流从入口进入通道，然后流过通道壁，从通向出口的不同通道离开过滤器。由此废气流中的颗粒物捕集在过滤器中。
沸石催化剂和负载的铂族催化剂可以通过任何已知手段加入到流通式或者过滤器基体。下面阐述使用修补基面涂覆工序来制备冷起动催化剂的代表性方法。将理解可以根据本发明不同的实施方案来改变下面的方法。同样，沸石催化剂和负载的PGM催化剂添加到流通式或者过滤器基体上的顺序不是关键的。因此，沸石催化剂可以在负载的PGM催化剂之前修补基面涂覆到基体上，或者负载的PGM催化剂可以在沸石催化剂之前修补基面涂覆到基体上。
预先形成的沸石催化剂可以通过修补基面涂覆步骤加入到流通式或者过滤器基体。可选地，通过首先修补基面涂覆未改性的沸石、贵金属/沸石或者贱金属/沸石到基体上来生成沸石涂覆的基体，可以在流通式或者过滤器基体上形成沸石催化剂。然后贵金属和/或贱金属可以加入到沸石涂覆的基体，其可以通过浸渍工序等来完成。
修补基面涂覆工序优选通过首先将沸石催化剂(或贱金属/沸石或贵金属/沸石或未改性的沸石)的磨碎颗粒在适当的溶剂(优选水)中浆料化以形成浆料来进行。另外的组分(例如过渡金属氧化物、粘合剂、稳定剂或者促进剂)也可以作为水溶性或者水分散性化合物的混合物引入浆料中。浆料优选包含10-70重量％的固体，更优选30-50重量％。在形成浆料之前，沸石催化剂(或贱金属/沸石、贵金属/沸石或者未改性的沸石)颗粒优选经过尺寸降低处理(例如研磨)，以使得固体颗粒的平均粒度小于20微米直径。
然后流通式或者过滤器基体可以一次或多次浸入到浆料中，或者可以将浆料涂覆到基体上，以使得在基体上将沉积所需负载量的催化材料。如果在修补基面涂覆流通式或者过滤器基体之前贵金属和/或贱金属没有引入到沸石中，则典型地将沸石涂覆的基体干燥和煅烧，然后可以通过任何已知手段将贵金属和/或贱金属加入到沸石涂覆的基体，手段包括例如使用贵金属化合物(例如硝酸钯)和/或贱金属化合物(例如硝酸铁)的浸渍、吸附或者离子交换。优选用浆料涂覆流通式或者过滤器基体的整个长度，以使得沸石催化剂的修补基面涂层覆盖基体的整个表面。
在流通式或者过滤器基体已经用沸石催化剂浆料涂覆，和如果有必要的话已经用贵金属和贱金属浸渍之后，优选将涂覆的基体干燥，然后通过在升高温度加热来进行煅烧，以形成沸石催化剂涂覆的基体。优选煅烧在400-600℃进行约1-8小时。
优选通过首先将负载的PGM催化剂的磨碎颗粒在适当的溶剂(优选水)中浆料化来实现增加负载的PGM催化剂的修补基面涂层。在形成浆料之前，负载的PGM催化剂颗粒优选经过尺寸降低处理(例如研磨)，以使得固体颗粒的平均粒度小于20微米直径。另外的组分(例如过渡金属氧化物、粘合剂、稳定剂或者促进剂)也可以作为水分散性或者水溶性化合物的混合物引入浆料中。
然后沸石催化剂涂覆的基体可以一次或多次浸入到负载的PGM催化剂浆料中，或者负载的PGM催化剂浆料可以涂覆到沸石催化剂涂覆的基体上，以使得在基体上将沉积所需负载量的催化材料。
可选地，仅含有无机氧化物的浆料可以首先沉积到沸石催化剂涂覆的基体上，以形成无机氧化物涂覆的基体，随后是干燥和煅烧步骤。铂然后族金属可以通过任何已知手段加入该无机氧化物涂覆的基体，手段包括铂族金属化合物(例如硝酸铂)的浸渍、吸附或者离子交换。
优选用负载的PGM催化剂浆料涂覆流通式或者过滤器基体的整个长度，以使得负载的PGM催化剂的修补基面涂层覆盖基体的整个表面。
在已经用负载的PGM催化剂浆料涂覆流通式或者过滤器基体后，优选进行干燥和然后通过在升高温度加热来进行煅烧以生成冷起动催化剂。优选煅烧在400-600℃进行约1-8小时。
在一个替代的实施方案中，流通式或者过滤器基体包含沸石催化剂，并且将负载的铂族金属催化剂涂覆到沸石催化剂基体上。在这种情况中，将沸石挤出以形成流通式或者过滤器基体，和优选挤出以形成蜂窝状流通式整料。挤出的沸石基体和蜂窝体以及制造它们的方法是本领域已知的。参见例如美国专利5,492,883、5,565,394和5,633,217和美国专利Re.34,804中。典型地，将沸石材料与耐久粘合剂(例如硅酮树脂)和临时粘合剂(例如甲基纤维素)混合，并且将该混合物挤出以形成蜂窝体生坯，然后对齐煅烧和烧结以形成最终的沸石流通式整料。在挤出前沸石可以包含贵金属和/或贱金属，以通过挤出共处生产贵金属/沸石、贱金属/沸石或者贵金属-贱金属/沸石流通式整料。
如果形成沸石流通式整料，则然后如果有必要，该沸石整料经过浸渍工序以将贵金属和/或贱金属负载到沸石整料，随后是修补基面涂覆步骤以修补基面涂覆负载的PGM催化剂。
本发明还包括用于内燃机的一种排气系统，其包括该冷起动催化剂。该排气系统优选包括一种或多种另外的后处理装置，其能够在正常的运行温度从内燃机废气中除去污染物。优选该排气系统包括冷起动催化剂和：(1)选择性催化还原系统；(2)颗粒物过滤器；(3)选择性催化还原过滤器系统；(4)NOx吸附剂催化剂；(5)三效催化剂体系；或者其任意组合。
这些后处理装置是现有技术公知的。选择性催化还原(SCR)系统是通过与氮化合物(例如氨或者尿素)或者烃(贫燃NOx还原)的反应而将NOx还原成N2的装置。典型的SCR催化剂包括氧化钒-二氧化钛催化剂、氧化钒-氧化钨-二氧化钛催化剂或者金属/沸石催化剂(例如铁/β沸石、铜/β沸石、铜/SSZ-13、铜/SAPO-34、Fe/ZSM-5或铜/ZSM-5。
颗粒物过滤器是减少来自内燃机废气的颗粒物的装置。颗粒物过滤器包括催化颗粒物过滤器和单纯(非催化)颗粒物过滤器。催化颗粒物过滤器(用于柴油和汽油应用)包括金属和金属氧化物组分(例如Pt、Pd、Fe、Mn、Cu和氧化铈)以氧化烃和一氧化碳以及消灭过滤器所捕集的烟灰。
选择性催化还原过滤器(SCRF)是单基体装置，其组合了SCR和颗粒物过滤器的功能。它们用于还原来自内燃机的NOx和颗粒物排放。
设计NOx吸附剂催化剂(NAC)以在贫燃废气条件下吸附NOx，在富燃条件下释放所吸附的NOx，和还原所释放的NOx以形成N2。NAC典型地包含NOx储存组分(例如Ba、Ca、Sr、Mg、K、Na、Li、Cs、La、Y、Pr和Nd)、氧化组分(优选Pt)和还原组分(优选Rh)。这些组分包含在一种或多种载体上。
三效催化剂系统(TWC)典型地在化学计量条件下用于汽油发动机中，以在单个装置上将NOx转化成N2，将一氧化碳转化成CO2，和将烃转化成CO2和H2O。
可以配置排气系统，以使得冷起动催化剂接近发动机布置，和使得另外的后处理装置位于冷起动催化剂的下游。因此,在正常运行条件下，发动机废气首先流过冷起动催化剂，然后与后处理装置接触。可选地，排气系统可以包括阀门或者其他导气装置，以使得在冷起动期过程中(低于约150-220℃的温度，在后处理装置处测量)，引导废气与后处理装置接触，然后流向冷起动催化剂。一旦后处理装置达到了运行温度(约150-220℃，在该后处理装置处测量)，则重新引导废气流与冷起动催化剂接触，然后与后处理装置接触。这确保了冷起动催化剂在较长的时间内保持低温，和因此改进了冷起动催化剂的效率，而同时允许后处理装置更快达到运行温度。例如美国专利5,656,244教导了在冷起动和正常运行条件过程中用于控制废气流动的装置，其教导在此引入作为参考。
下面的实施例仅用来说明本发明。本领域技术人员将认识到，许多变型处于本发明的主旨和权利要求的范围内。
实施例1：制备本发明的催化剂
催化剂1A：Pd-Fe/β沸石+Pt/Al2O3
将β沸石加入硝酸铁水溶液中，随后加入二氧化硅粘合剂来形成浆料。将该浆料涂覆到流通式堇青石基体上以实现190g/ft3Fe的铁负载，和将该Fe/沸石涂覆的基体干燥，然后在500℃加热煅烧4小时。然后通过硝酸Pd水溶液的浸渍来将钯加入Fe/沸石涂覆的基体中，以实现50g/ft3的Pd负载量，和将该Pd-Fe/沸石涂覆的基体干燥，然后在500℃加热煅烧4小时。
将硝酸铂加入到氧化铝颗粒(研磨到平均粒度小于10微米直径)的水浆料以形成Pt/氧化铝催化剂浆料。然后将该Pt/氧化铝催化剂浆料涂覆到Pd-Fe/沸石涂覆的基体上，以实现50g/ft3的Pt负载量，并且干燥最终涂覆的基体，然后在500℃加热煅烧4小时以生成催化剂1A(包含50g/ft3的Pd、190g/ft3的Fe和50g/ft3的Pt)。
催化剂1B：Pd-Fe/β沸石+Pt/Al2O3+Pd/CeO2
催化剂1B通过将Pd/氧化铈组分加入到最终的催化剂1A中来制备。钯/氧化铈通过将硝酸钯初始润湿到氧化铈上，随后干燥和在500℃煅烧2小时来制备。然后将该Pd/氧化铈研磨到平均粒度小于10微米直径，并且加入到水中以形成浆料。将Pd/氧化铈浆料和来自催化剂1A制备的Pt/氧化铝浆料涂覆到来自催化剂1A制备的Pd-Fe/沸石涂覆的基体上，以实现50g/ft3的Pd负载量，和干燥最终的涂覆基体，然后在500℃加热煅烧4小时以生成催化剂1B(包含在沸石上的50g/ft3的Pd和190g/ft3的Fe；在氧化铝上的50g/ft3的Pt；和在氧化铈上的50g/ft3的Pd)。
催化剂1C：在挤出的β沸石上的Pd-Fe+Pd/CeO2+Pt/Al2O3
将β沸石整料(通过将β沸石挤出成蜂窝状整料来形成；参见例如美国专利5,492,883、5,565,394和5,633,217)用硝酸铁水溶液浸渍，随后干燥，和在500℃加热煅烧4小时以实现800g/ft3的Fe负载量；然后用硝酸钯溶液浸渍，随后干燥，和在500℃煅烧4小时以实现50g/ft3的Pd负载量。
然后用负载的PGM催化剂在如下两个修补基面涂覆步骤中涂覆该Fe-Pd/沸石整料。将Pd/氧化铈(如催化剂1B中制备)和氧化铝颗粒分别研磨到平均粒度小于10微米直径，并且加入水中以形成浆料。然后将该Pd/氧化铈和氧化铝浆料涂覆到Fe-Pd/沸石整料上，以实现40g/ft3的Pd负载量，干燥该涂覆的基体，然后在500℃加热煅烧4小时。然后如催化剂1A那样，用负载的Pt/氧化铝催化剂活性涂覆该基体，干燥和然后煅烧来生成催化剂1C(包含在挤出的沸石上的50g/ft3的Pd、800g/ft3的Fe；在氧化铈上的40g/ft3的Pd；和在氧化铝上的50g/ft3的Pt)。
催化剂1D：Pd-Fe/ZSM5+Pt/Al2O3
重复催化剂1A的步骤，除了使用含铁的ZSM5沸石(7wt％的Fe2O3)代替Fe/β沸石之外，以生成催化剂1D(包含在沸石上50g/ft3的Pd、170g/ft3的Fe；和在氧化铝上的50g/ft3的Pt)。
催化剂1E：负载在Fe-β沸石上的Pd+Pt/Al2O3
重复催化剂1A的程序，除了使用引入铁的β沸石(Fe-β沸石，其中Al原子已经完全被Fe取代)代替Fe/β沸石之外，以生成催化剂1E(包含在沸石上的50g/ft3的Pd、250g/ft3的Fe；和在氧化铝上的50g/ft3的Pt)。
实施例2：对比催化剂制备
对比催化剂2A：Pt/Al2O3+Pd/CeO2
对比催化剂2A是一种用于冷起动NOx控制的常规催化剂，类似于WO 2008/047170中所公开的分层体系。它根据催化剂1C的步骤制备，除了涂覆是在流通式堇青石基体上进行的，不包括在挤出的β沸石上的Pd-Fe，并且Pd和Pt负载量也增加了。对比催化剂2A包含在Pd/氧化铈上的100g/ft3的Pd和Pt/氧化铝上的100g/ft3的Pt。
对比催化剂2B：Pd-Pt/Al2O3+β沸石+Pt/Al2O3
对比催化剂2B是一种典型的柴油氧化催化剂，其包含作为烃捕集组分的沸石。它是如下来制备的。
将硝酸铂和硝酸钯加入到氧化铝颗粒(研磨到平均粒度小于10微米直径)的水浆料中，随后加入β沸石到浆料中。然后将Pt-Pd/氧化铝和β沸石浆料涂覆到流通式堇青石基体以实现17.5g/ft3的Pt负载量和35g/ft3的Pd负载量，干燥该涂覆的基体，然后在500℃煅烧4小时。
然后如催化剂1A的步骤，用负载的PGM催化剂修补基面涂覆该沸石整料，以得到52.5g/ft3的第二修补基面涂层Pt负载量。干燥该基体，然后煅烧以生成对比催化剂2B，其含有70g/ft3的Pt和35g/ft3的Pd。
实施例3：测试程序
全部催化剂在流通式催化剂涂覆的堇青石基体的芯样品(2.54cm×8.4cm)上测试。催化剂芯首先在流通条件下在炉中，在750℃的水热条件(5％的H2O，余量为空气)下老化16小时。然后在实验反应器中，使用供料气流(通过调整单个废气组分的质量流量来制备)测试芯的催化活性。气体流速保持在21.2Lmin-1，产生的气体时空速率为30000h-1(GHSV＝30,000h-1)。
在贫燃条件下，使用合成废气供料流来测试催化剂，该供料流的组成为200ppm的NO、200ppm的CO、500ppm的癸烷(基于C1)、10％的O2、5％的CO2、5％的H2O和余量的氮气(体积％)。将催化剂曝露于供料气流，首先在80℃的等温入口气体温度保持100秒，其后入口气体温度随着时间以100℃/min线性增加。
催化剂1C也是在化学计量条件下，使用合成气组合物来测试，该合成气的组成为2000ppm的NO、1％的CO、0.33％的H2、600ppm的丙烷(基于C1)、600ppm的丙烯(基于C1)、0.76％的O2、14％的CO2、10％的H2O和余量的氮气(体积％)。将该催化剂曝露于供料气流，首先在80℃的等温入口气体温度保持100秒，其后入口气体温度随着时间以100℃/min线性增加。因此，在测试的起初100秒，该催化剂曝露于80℃的合成气流，并且在测试的起初172秒后，温度超过200℃。
表1的结果显示，与对比催化剂2A和2B相比，当曝露于合成贫燃气流时，本发明的催化剂(1A-1E)在低温(在测试的起初100秒测试是80℃)表现出更高的NOx储存能力，和典型地在200℃以下(即，测试的约起初172秒)表现出更高的NOx储存能力。两种对比催化剂2A和2B都表现出在催化剂出口的瞬间的、急剧的NOx逃逸，这表明在低温可忽略的NOx储存。200℃以下的总NOx储存能力代表了低于该温度的NOx储存量和在温度升高到200℃过程中能够由催化剂转化(至少部分转化)的NOx的量。因此，200℃以下的总NOx储存能力代表了在温度升高到200℃过程中由催化剂转化(至少部分转化)的NOx，或者在温度高于200℃由催化剂随后释放，然后通过下游的NOx还原催化剂(因为它们会达到其操作窗口)所转化的NOx。
尽管催化剂1A仅具有对比催化剂2A一半的PGM负载量和与对比催化剂2B相当的总PGM负载量，但是催化剂1A在冷起动条件下有效地储存了明显更高量的NOx，这表明贱金属和贵金属存在于沸石上所增加的益处。用催化剂1B(其中除了沸石，Pd也负载在氧化铈上)和催化剂1C(其中沸石作为基体本体挤出)实现了冷起动NOx储存中进一步明显的增加，并且仍然提供了高的NOx储存能力。催化剂1D和1E显示，ZSM-5和引入铁的β沸石(Fe-β沸石)也可以用于冷起动条件下的NOx储存。
本发明的催化剂在冷起动阶段过程中也有效地储存了烃。在150℃以下的温度，催化剂1A、1B和1C储存了与对比催化剂2A和2B类似量的烃(HC)。例如，对于催化剂1A-1C和对比催化剂2A和2B来说，在80℃100秒中储存的烃量是约0.29g的CH4/L催化剂。在高于150℃的温度，对于对比催化剂2A和2B来说，相比于催化剂1A、1B和1C，HC逃逸明显更高。参见表2。由测试对比催化剂2A和2B所形成的最高烃浓度(大于100ppm)是催化剂1A，1B和1C所获得的(约50ppm)两倍，这表明本发明的催化剂不仅在冷起动过程中有效地储存了烃，而且在温度升高时，还更有效地转化了所储存的烃。
本发明的催化剂还表现出在冷起动阶段过程中对于N2O更低的选择性。在150℃以下的温度，催化剂1A、1B和1C和对比催化剂2A和2B均没有显示出产生N2O。150℃以上，对于全部的催化剂检出了N2O。但是，表2还显示，如在预热过程中所释放的最高N2O浓度所指示，在催化剂1A、1B和1C上仅形成了低水平的N2O。相反，在两种对比催化剂上检出了明显更高量的N2O。这些结果表明，本发明的催化剂表现出对N2更高的选择性。
除了冷起动NOx和HC控制之外，催化剂1A-1C还出人意料地表现出改进的CO氧化活性。从表3中可见，与对比催化剂2B(典型的柴油氧化催化剂)相比，催化剂1A-1C表现出对于实现在预热过程中90％CO转化率来说明显更低的温度(“T90”)。因为PGM的量影响了CO氧化活性，因此具有明显更高量的PGM的对比催化剂2A预期具有最低的T90。
另外，一旦本发明的催化剂达到运行温度(例如>200℃)，则催化剂1A-1C全部表现出与对比催化剂2B相当的NO到NO2氧化活性。在表4中，这通过在400℃的入口气体温度，所形成的NO2与总NOx之比来表示。再次需要注意的是，对比催化剂2A具有比催化剂1A、1B、1C(50g/ft3)或者对比催化剂2B(70g/ft3)更高的Pt负载量(100g/ft3)，这解释了它相对更高的CO和NO氧化活性。
除了它们在贫燃运行条件下的能力之外，当在化学计量条件下测试时，催化剂1C也表现出对于冷起动条件来说良好的NOx和烃储存能力以及良好的CO氧化活性，如表5所示。
总之，本发明的冷起动催化剂体系表现出多种功能，包括：(1)低温NOx储存和转化，具有对N2的高选择性；(2)低温烃储存和转化；(3)改进的CO氧化活性；和(4)在预热后相当的NO到NO2氧化活性。
表1：NOx储存容量结果
*对比例
nm＝未检出
表2：150℃以上的烃(HC)和N2O释放
*对比例
表3：预热期间90％CO转化的温度(T90)
催化剂 T90(℃)
1A 145
1B 154
1C 150
2A* 102
2B* 219
*对比例
表4：400℃下NO2/NOx比
催化剂 NO2/NOx
1A 0.63
1B 0.62
1C 0.74
2A* 0.89
2B* 0.73
*对比例
表5：化学计量条件下催化剂1C的表现

Claims (15)

1.一种冷起动催化剂，其包含：(1)沸石催化剂，其包含贱金属、贵金属和沸石；和(2)负载的铂族金属催化剂，其包含一种或多种铂族金属和一种或多种无机氧化物载体。
2.权利要求1的冷起动催化剂，其中该贱金属选自铁、铜、锰、铬、钴、镍、锡及其混合物。
3.权利要求1的冷起动催化剂，其中该贱金属是铁。
4.权利要求1的冷起动催化剂，其中该贵金属选自铂、钯、铑及其混合物。
5.权利要求1的冷起动催化剂，其中该贵金属是钯。
6.权利要求1的冷起动催化剂，其中该沸石选自β沸石、八面沸石、L-沸石、ZSM沸石、SSZ-沸石、丝光沸石、菱沸石、硅铝钾沸石、毛沸石、斜发沸石、硅质岩、磷酸铝沸石、中孔沸石、引入金属的沸石及其混合物。
7.权利要求1的冷起动催化剂，其中该沸石选自β沸石、ZSM-5、Fe-β沸石、SSZ-33、Y-沸石及其混合物。
8.权利要求1的冷起动催化剂，其中该一种或多种铂族金属选自铂、钯、铑、铱及其混合物。
9.权利要求1的冷起动催化剂，其中该一种或多种无机氧化物载体选自氧化铝、二氧化硅、二氧化钛、氧化锆、氧化铈、氧化铌、钽氧化物、钼氧化物、钨氧化物及其混合氧化物或复合氧化物。
10.一种排气系统，其包括权利要求1的冷起动催化剂和流通式或者过滤器基体。
11.权利要求10的排气系统，其中该流通式基体是蜂窝状整料。
12.权利要求10的排气系统，其中将该沸石催化剂和该负载的铂族金属催化剂涂覆到该流通式或者过滤器基体上。
13.权利要求10的排气系统，其中该流通式或者过滤器基体包含该沸石催化剂，和将该负载的铂族金属催化剂涂覆到该沸石催化剂流通式或者过滤器基体上。
14.一种用于内燃机的排气系统，其包括权利要求1的冷起动催化剂。
15.权利要求14的排气系统，其进一步包括：选择性催化还原催化剂体系；颗粒物过滤器；选择性催化剂还原过滤器系统；NOx吸附剂催化剂；三效催化剂体系；或者其组合。
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