CN105813717A - 包含贵金属和小孔分子筛的被动式NOx吸附剂 - Google Patents

包含贵金属和小孔分子筛的被动式NOx吸附剂 Download PDF

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CN105813717A
CN105813717A CN201480066542.7A CN201480066542A CN105813717A CN 105813717 A CN105813717 A CN 105813717A CN 201480066542 A CN201480066542 A CN 201480066542A CN 105813717 A CN105813717 A CN 105813717A
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adsorbent
passive type
molecular sieve
catalyst
small pore
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CN105813717B (zh
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H-Y·陈
R·R·拉什拉姆
刘东霞
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Johnson Matthey PLC
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Johnson Matthey PLC
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Abstract

公开了一种被动式NOx吸附剂。所述被动式NOx吸附剂有效于在某个低温以下吸附NOx和在高于所述低温的温度释放吸附的NOx。所述被动式NOx吸附剂包含贵金属和小孔分子筛。所述小孔分子筛具有8个四面体原子的最大环尺寸。本发明还包括一种包括被动式NOx吸附剂的排气系统，和一种利用被动式NOx吸附剂来处理来自内燃机的废气的方法。

Description

包含贵金属和小孔分子筛的被动式NOx吸附剂
发明领域
本发明涉及被动式NOx吸附剂和其在用于内燃机的排气系统的用途。
发明背景
内燃机产生了包含各种污染物的废气，包括氮氧化物(“NOx”)，一氧化碳和未燃烧的烃，这是政府立法的主题。排放控制系统广泛地用于降低排放到大气的这些污染物的量，一旦它们达到其操作温度(通常为200℃和更高)，通常获得非常高的效率。然而，这些系统低于其操作温度(“冷启动”期间)是相对低效的。
例如，目前为了满足Euro6b排放而实施的基于尿素的选择性催化还原(SCR)应用要求尿素定量给料位置处的温度大于约180℃，之后尿素可以定量给料和用于转化NOx。使用目前的系统难以解决低于180℃的NOx转化，并且未来欧洲和美国立法将强调低温NOx储存和转化。目前，这是通过加热策略来实现的，但是这具有有害的CO2排放的效应。
随着甚至更严格的国家和区域立法降低了可以从柴油或汽油发动机排放的污染物的量，在冷启动期间降低排放成为主要的挑战。因此，用于降低在冷启动条件过程中排放的NOx的水平的方法持续被探索。
例如，PCT国际申请WO2008/047170公开了一种系统，其中来自贫燃废气的NOx在低于200℃的温度吸附和然后在高于200℃热脱附。教导NOx吸附剂由钯和铈氧化物或混合氧化物或含铈和至少一种其它过渡金属的混合氧化物或复合氧化物组成。
美国申请公开No.2011/0005200教导一种催化剂系统，其通过将氨选择性催化还原(“NH3-SCR”)催化剂配制物置于贫燃NOx捕集器的下游来同时除去氨和加强净NOx转化率。教导NH3-SCR催化剂来吸附在贫燃NOx捕集器中富燃脉冲期间产生的氨。然后，储存的氨与从上游贫燃NOx捕集器排放的NOx反应，这提高了NOx转化率，同时消耗了储存的氨。
PCT国际申请WO2004/076829公开了废气纯化系统，其包括设置在SCR催化剂上游的NOx储存催化剂。NOx储存催化剂包含用至少一种铂族金属(Pt，Pd，Rh，或Ir)涂覆或活化的至少一种碱金属、碱土金属或稀土金属。教导特别优选的NOx储存催化剂包含用铂涂覆的氧化铈和此外在基于氧化铝的载体上的铂作为氧化催化剂。EP1027919公开了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)。以负载在氧化铝上的铂为例。美国申请公开No.2012/0308439A1教导冷启动催化剂，其包含(1)包含贱金属、贵金属和沸石的沸石催化剂，和(2)包含一种或多种铂族金属和一种或多种无机氧化物载体的负载的铂族金属催化剂。
对于任何汽车系统和方法，希望的是在废气处理系统中获得仍进一步的改善，特别是在冷启动条件下。我们发现了一种提供来自内燃机的废气的增强的清洁的新被动式NOx吸附剂。该新的被动式NOx吸附剂还表现出改善的耐硫性。
发明内容
本发明为一种有效于在某个低温以下吸附NOx和在高于所述低温的温度释放吸附的NOx的被动式NOx吸附剂。被动式NOx吸附剂包含贵金属和小孔分子筛。小孔分子筛具有8个四面体原子的最大环尺寸。本发明还包括一种包括被动式NOx吸附剂的排气系统，和一种利用被动式NOx吸附剂来处理来自内燃机的废气的方法。
具体实施方式
本发明的被动式NOx吸附剂有效于在某个低温以下吸附NOx和在高于所述低温的温度释放吸附的NOx。优选地，低温为约200℃。被动式NOx吸附剂包含贵金属和小孔分子筛。贵金属优选为钯、铂、铑、金、银、铱、钌、锇或其混合物；更优选为钯、铂、铑或其混合物。钯是特别优选的。
小孔分子筛具有8个四面体原子的最大环尺寸。小孔分子筛可为任何天然或合成分子筛，包括沸石，和优选由铝、硅和/或磷组成。分子筛通常具有通过氧原子共享而连接的SiO4、AlO4和/或PO4的三维设置，但也可以为二维结构。分子筛骨架通常为阴离子型的，其通过电荷补偿阳离子来平衡，通常为碱和碱土元素(例如，Na，K，Mg，Ca，Sr，和Ba)，铵离子以及质子。其它金属(例如，Fe，Ti和Ga)可引入小孔分子筛骨架以产生金属引入的分子筛。
优选地，小孔分子筛选自铝硅酸盐分子筛、金属取代的铝硅酸盐分子筛、铝磷酸盐分子筛或金属取代的铝磷酸盐分子筛。更优选地，小孔分子筛为具有以下骨架类型的分子筛：ACO，AEI，AEN，AFN，AFT，AFX，ANA，APC，APD，ATT，CDO，CHA，DDR，DFT，EAB，EDI，EPI，ERI，GIS，GOO，IHW，ITE，ITW，LEV，KFI，MER，MON，NSI，OWE，PAU，PHI，RHO，RTH，SAT，SAV，SIV，THO，TSC，UEI，UFI，VNI，YUG，和ZON，以及任何两种或更多种的混合物或共生物。特别优选的小孔分子筛的共生物包括KFI-SIV、ITE-RTH、AEW-UEI、AEI-CHA和AEI-SAV。最优选地，小孔分子筛为AEI或CHA，或AEI-CHA共生物。
被动式NOx吸附剂可通过任何已知的方式来制备。例如，贵金属可通过任何已知的方式添加至小孔分子筛以形成被动式NOx吸附剂，添加的方式不认为是特别关键的。例如，贵金属化合物(例如硝酸钯)可通过浸渍、吸附、离子交换、初湿、沉淀等负载在分子筛上。其它金属也可以添加至被动式NOx吸附剂。
优选地，被动式NOx吸附剂中的一些贵金属(大于1％的添加的总贵金属)设置在小孔分子筛的孔隙内。更优选地，贵金属总量的大于5％设置在小孔分子筛的孔隙内；和甚至更优选贵金属总量的大于10％或大于25％或大于50％可设置在小孔分子筛的孔隙内。
优选地，被动式NOx吸附剂进一步包括流通式基材或过滤式基材。在一个实施方案中，被动式NOx吸附剂涂覆在流通式或过滤式基材上，和优选使用载体涂层程序沉积在流通式或过滤式基材上以产生被动式NOx吸附剂系统。
流通式或过滤式基材是能够包含催化组分的基材。基材优选为陶瓷基材或金属基材。陶瓷基材可由任何适合的耐火材料组成，例如，氧化铝，二氧化硅，二氧化钛，二氧化铈，氧化锆，氧化镁，沸石，氮化硅，碳化硅，锆硅酸盐，镁硅酸盐，铝硅酸盐，金属铝硅酸盐(例如堇青石和锂辉石)，或其任何两种或更多种的混合物或混合氧化物。堇青石、镁铝硅酸盐和碳化硅是特别优选的。
金属基材可由任何适合的金属组成，和特别是耐热的金属和金属合金例如钛和不锈钢以及含有铁、镍、铬和/或铝(除了其它痕量金属以外)的铁素体合金。
流通式基材优选为具有蜂窝状结构的流通式整料，所述蜂窝状结构具有多个小、平行的薄壁通道，其轴向穿过基材且从基材的入口或出口贯穿延伸。基材的通道横截面可为任何形状，但是优选正方形、正弦形、三角形、矩形、六边形、梯形、圆形或椭圆形。
过滤式基材优选为壁流式整料过滤器。壁流式过滤器的通道交替封闭，这允许废气物流从入口进入通道，然后流过通道壁，和从通向出口的不同通道离开过滤器。因此，废气物流中的颗粒被捕集在过滤器中。
被动式NOx吸附剂可通过任何已知的方式添加至流通式或过滤式基材。使用载体涂层程序制备被动式NOx吸附剂的代表性方法如下文所述。将理解的是，下文的方法可以根据不同的本发明实施方案而变化。
预成型的被动式NOx吸附剂可通过载体涂覆步骤添加至流通式或过滤式基材。替代地，可通过将未改性小孔分子筛首先载体涂覆在流通式或过滤式基材上以产生分子筛涂覆的基材来在所述基材上形成被动式NOx吸附剂。然后，可以将贵金属添加至分子筛涂覆的基材，这可通过浸渍程序等完成。
优选通过首先在恰当的溶剂(优选水)中浆化细分的被动式NOx吸附剂(或未改性小孔分子筛)颗粒以形成浆料来进行载体涂覆程序。额外组分例如过渡金属氧化物、粘合剂、稳定剂或助催化剂也可以作为水溶性或水分散性化合物的混合物引入浆料。浆料优选包含10-70重量％的固体，更优选20-50重量％。在形成浆料之前，被动式NOx吸附剂(或未改性小孔分子筛)颗粒优选经受尺寸减小处理(例如，研磨)，使得固体颗粒的平均粒度为直径小于20微米。
然后，流通式或过滤式基材可一次或多次浸入浆料或浆料可涂覆在基材上，使得希望负载量的催化材料沉积在基材上。如果贵金属没有在载体涂覆流通式或过滤式基材之前引入分子筛，分子筛涂覆的基材通常干燥和煅烧，然后贵金属可通过任何已知的方式添加至分子筛涂覆的基材，包括浸渍、吸附或离子交换，例如，利用贵金属化合物(例如硝酸钯)。优选地，流通式或过滤式基材的整个长度用浆料涂覆，使得被动式NOx吸附剂载体涂层覆盖基材整个表面。
在流通式或过滤式基材用被动式NOx吸附剂涂覆和用贵金属浸渍(如果需要)之后，经涂覆的基材优选干燥和然后通过在升高的温度加热而煅烧以形成被动式NOx吸附剂涂覆的基材。优选地，煅烧在400-600℃进行大约1-8小时。
在替代的实施方案中，流通式或过滤器基材包含被动式NOx吸附剂。在这种情况下，被动式NOx吸附剂挤出以形成流通式或过滤器基材。被动式NOx吸附剂挤出的基材优选为蜂窝状流通式整料。
挤出的分子筛基材和蜂窝状体以及制备它们的方法在本领域中是已知的。参见例如，美国专利号5,492,883，5,565,394，和5,633,217和美国专利No.Re.34,804。通常，分子筛材料与持久粘合剂如有机硅树脂和临时粘合剂如甲基纤维素混合，和混合物挤出以形成蜂窝状生坯体，其然后煅烧和烧结以形成最终的小孔分子筛流通式整料。分子筛可以在挤出之前包含贵金属，使得被动式NOx吸附剂整料通过挤出程序而产生。替代地，贵金属可添加至预成型的分子筛整料以产生被动式NOx吸附剂整料。
本发明还包括用于包括被动式NOx吸附剂的内燃机的排气系统。排气系统优选包括一个或多个另外的能够在正常操作温度从内燃机的废气除去污染物的后处理装置。优选地，排气系统包括被动式NOx吸附剂和一种或多种选自以下的其它催化剂部件：(1)选择性催化还原(SCR)催化剂，(2)颗粒过滤器，(3)SCR过滤器，(4)NOx吸附催化剂，(5)三元催化剂，(6)氧化催化剂，或任何其组合。被动式NOx吸附剂优选为独立于任何上述后处理装置的部件。替代地，被动式NOx吸附剂可以作为部件引入任何上述后处理装置。
这些后处理装置在本领域是公知的。选择性催化还原(SCR)催化剂为通过与氮化合物(例如氨或尿素)或烃(贫燃NOx还原)反应将NOx还原为N2的催化剂。典型的SCR催化剂包含氧化钒-二氧化钛催化剂，氧化钒-钨氧化物-二氧化钛催化剂，或金属/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。
颗粒过滤器为减少来自内燃机的排气的颗粒的装置。颗粒过滤器包括催化颗粒过滤器和裸(非催化)颗粒过滤器。催化颗粒过滤器(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，和二氧化铈)以氧化烃和一氧化碳(除了破坏由过滤器捕集的烟灰之外)。
选择性催化还原过滤器(SCRF)是组合SCR和颗粒过滤器的功能的单一基材装置。它们用于降低来自内燃机的NOx和颗粒排放。除了SCR催化剂涂覆，颗粒过滤器也可以包括其它金属和金属氧化物组分(例如Pt，Pd，Fe，Mn，Cu和二氧化铈)以氧化烃和一氧化碳(除了破坏由过滤器捕集的烟灰之外)。
NOx吸附催化剂(NAC)设计以在贫燃排气条件下吸附NOx，在富燃条件下释放吸附的NOx，和还原释放的NOx以形成N2。NAC通常包括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。
三元催化剂(TWC)通常在化学计量条件下用于汽油发动机以在单一装置上将NOx转化为N2，将一氧化碳转化为CO2，以及将烃转化为CO2和H2O。
氧化催化剂和特别是柴油氧化催化剂(DOC)在本领域是公知的。氧化催化剂设计以将CO氧化为CO2以及将气相烃(HC)和柴油颗粒的有机馏分(可溶的有机馏分)氧化为CO2和H2O。典型的氧化催化剂包括在高表面积无机氧化物载体如氧化铝、二氧化硅-氧化铝和沸石上的铂以及任选的钯。
可以构造排气系统，使得被动式NOx吸附剂设置成接近于发动机和额外的后处理装置设置在被动式NOx吸附剂的下游。因此，在正常操作条件下，发动机废气首先流过被动式NOx吸附剂，之后接触后处理装置。替代地，排气系统可以包含阀门或其它气体导向装置，使得在低温期间(低于约150-220℃，优选200℃的温度，如在后处理装置处测量)引导废气接触后处理装置，之后流至被动式NOx吸附剂。一旦后处理装置达到操作温度(约150-220℃，优选200℃，如在后处理装置处测量)，然后再引导废气流接触被动式NOx吸附剂，之后接触后处理装置。这确保被动式NOx吸附剂的温度保持低，持续更长的时间，因此改善了被动式NOx吸附剂的效率，同时允许后处理装置更快地达到操作温度。美国专利No.5,656,244例如教导了在冷启动和正常操作条件期间控制废气流的装置，该专利的教导通过参考引入本文。
本发明还包括一种处理来自内燃机的废气的方法。该方法包括在某个低温或低于该低温的温度将NOx吸附在被动式NOx吸附剂上，在高于所述低温的温度热脱附来自被动式NOx吸附剂的NOx，和在被动式NOx吸附剂的下游的催化剂部件上催化除去脱附的NOx。优选地，低温为约200℃。
被动式NOx吸附剂的下游的催化剂部件为SCR催化剂、颗粒过滤器、SCR过滤器、NOx吸附催化剂、三元催化剂、氧化催化剂或其组合。
以下的实施例仅描述本发明。本领域技术人员将认识到在本发明精神和权利要求范围内的多个变型。
实施例1：被动式NOx吸附剂(PNA)的制备
根据以下通用程序，钯添加至二氧化硅与氧化铝之比(SAR)为26的小孔菱沸石(CHA)沸石、SAR＝23的中孔ZSM-5(MFI)沸石和SAR＝26的大孔β(BEA)沸石，以产生PNA1A(Pd/CHA)、对比例PNA1B(Pd/MFI)和对比例PNA1C(Pd/BEA)：通过使用硝酸钯作为前体湿式浸渍沸石来制备粉末催化剂。在100℃干燥后，样品在500℃煅烧。然后，样品在750℃在包含10％H2O的空气气氛中水热老化。三种样品的Pd负载量为1wt.％。
根据记录在WO2008/047170中的程序制备对比例PNA1D(Pd/CeO2)。Pd负载量为1wt.％。样品在750℃在包含10％H2O的空气气氛中水热老化。
实施例2：NOx储存能力测试程序
PNA(0.4g)在包含NO的气体混合物中保持在吸附温度约80℃持续2分钟，所述气体混合物以2升/分钟以300L*hr-1*g-1的MHSV流动。该吸附阶段之后，程序升温脱附(TPD)以10℃/min的升温速度在包含NO的气体的存在下进行，直至床温度达到约400℃，以吹扫所有储存的NOx的催化剂，用于进一步测试。然后，代替80℃，从170℃的吸附温度开始重复测试。
在吸附和脱附两者的过程中，包含NO的气体混合物包含12vol.％的O2、200ppmNO、5vol.％的CO2、200ppmCO、50ppmC10H22和5vol.％的H2O。
参考包含约3g/in3的催化剂负载量的整料，以储存的NO2/升催化剂的量计算NOx储存。不同温度的结果在表1中给出。
表1中的结果表明，相比于对比例PNA1D，本发明PNA(PNA1A)在80和170℃表现出可比的NOx储存能力。尽管对比例PNA1B和1C在80℃表现出更高的NOx储存能力，其在170℃的NOx储存能力较低。由于应用要求在高于约170℃的温度高的NOx储存能力，PNA1A和对比例PNA1D相比于对比例PNA1B和1C具有优势。
实施例3：硫暴露之后的NOx储存能力测试程序
PNA1A和对比例PNA1D通过使其与含SO2的气体(100ppmSO2，10％的O2，5％的CO2和H2O，余量N2)在300℃接触来经受高水平的硫酸化以添加约64mgS/克催化剂。在硫酸化之前和之后，催化剂的NOx储存能力在100℃按照实施例2的程序测量。结果列在表2中。
表2中给出的结果表明本发明的PNA(PNA1A)即使在高水平的硫暴露后仍保持显著量的NOx储存能力。相反，在相同的硫酸化条件下，对比例PNA1D损失了其几乎所有的NOx吸附能力。本发明的PNA表现出很大改进的耐硫性。
实施例4：小孔分子筛负载的被动式NOx吸附剂(PNA)的制备
按照实施例1的程序，将钯添加至一系列小孔分子筛。对于所有的样品，Pd负载量保持在1wt.％。样品在750℃在包含10％H2O的空气气氛中水热老化。然后，按照实施例2的程序，测试老化样品的NOx储存能力。
这些PNA和其在80和170℃的NOx储存能力列于表3中。
表3中的结果表明，宽范围的小孔分子筛负载的PNA具有高的NOx储存能力。
实施例5：具有不同的钯负载量的小孔分子筛负载的被动式NOx吸附剂(PNA)的制备
按照实施例1的程序，将钯添加至小孔分子筛CHA。对于样品，Pd负载量增加至2wt.％。样品在750℃在包含10％H2O的空气气氛中水热老化。按照实施例2的程序，测试老化样品的NOx储存能力。在80和170℃在样品上的NOx储存能力列于表4中。
表4的结果表明，增加的Pd负载量提高NOx储存能力。
表1:NOx储存能力(gNO2/L)
催化剂 NOx储存能力(80℃) NOx储存能力(170℃)
1A 0.28 0.45
1B* 0.35 0.28
1C* 0.68 0.07
1D* 0.29 0.38
*对比实施例
表2:NOx储存能力(gNO2/L)
*对比实施例
表3:NOx储存能力(gNO2/L)
催化剂 小孔分子筛 NOx储存能力(80℃) NOx储存能力(170℃)
PNA 1A CHA(SAR＝26) 0.28 0.45
PNA 4A CHA(SAR＝12) 0.42 0.60
PNA 4B CHA(SAR＝13) 0.34 0.51
PNA 4C CHA(SAR＝17) 0.20 0.42
PNA 4D CHA(SAR＝22) 0.28 0.42
PNA 4E AEI(SAR＝20) 0.33 0.57
PNA 4F ERI(SAR＝12) 0.08 0.2
PNA 4G CHA(SAPO-34) 0.29 0.41
PNA 4H AEI-CHA共生物(SAPO) 0.22 0.23
表4:NOx储存能力(gNO2/L)

Claims (16)

1.有效于在某个低温以下吸附NOx和在高于所述低温的温度释放吸附的NOx的被动式NOx吸附剂，所述被动式NOx吸附剂包含贵金属和具有8个四面体原子的最大环尺寸的小孔分子筛。
2.根据权利要求1所述的被动式NOx吸附剂，其中所述贵金属选自铂、钯、铑、金、银、铱、钌、锇及其混合物。
3.根据权利要求1所述的被动式NOx吸附剂，其中所述贵金属为钯.
4.根据权利要求1-3任一项所述的被动式NOx吸附剂，其中所述小孔分子筛选自铝硅酸盐分子筛、金属取代的铝硅酸盐分子筛、铝磷酸盐分子筛和金属取代的铝磷酸盐分子筛。
5.根据权利要求1-4任一项所述的被动式NOx吸附剂，其中所述小孔分子筛选自如下的骨架类型：ACO，AEI，AEN，AFN，AFT，AFX，ANA，APC，APD，ATT，CDO，CHA，DDR，DFT，EAB，EDI，EPI，ERI，GIS，GOO，IHW，ITE，ITW，LEV，KFI，MER，MON，NSI，OWE，PAU，PHI，RHO，RTH，SAT，SAV，SIV，THO，TSC，UEI，UFI，VNI，YUG，ZON，和其混合物或共生物。
6.根据权利要求5所述的被动式NOx吸附剂，其中所述小孔分子筛选自AEI和CHA的骨架类型。
7.根据权利要求5所述的被动式NOx吸附剂，其中所述小孔分子筛的共生物包括KFI-SIV、ITE-RTH、AEW-UEI、AEI-CHA和AEI-SAV。
8.根据权利要求1-7任一项所述的被动式NOx吸附剂，其中所述被动式NOx吸附剂涂覆在流通式或过滤器基材上。
9.根据权利要求8所述的被动式NOx吸附剂，其中所述流通式基材为蜂窝状整料。
10.根据权利要求1-7任一项所述的被动式NOx吸附剂，其中将所述被动式NOx吸附剂挤出以形成流通式或过滤器基材。
11.根据权利要求1-10任一项所述的被动式NOx吸附剂，其中贵金属总量的大于5％设置在所述小孔分子筛的孔隙内。
12.根据权利要求1-11任一项所述的被动式NOx吸附剂，其中所述低温为200℃。
13.内燃机的排气系统，其包括根据前述权利要求任一项所述的被动式NOx吸附剂和选自选择性催化还原(SCR)催化剂、颗粒过滤器、SCR过滤器、NOx吸附剂催化剂、三元催化剂、氧化催化剂及其组合的催化剂部件。
14.减少废气中的NOx的方法，所述方法包括在某个低温以下将NOx吸附在前述权利要求任一项所述的被动式NOx吸附剂上，在高于所述低温的温度热脱附来自所述被动式NOx吸附剂的NOx，和在所述被动式NOx吸附剂的下游的催化剂部件上催化除去脱附的NOx。
15.根据权利要求14所述的方法，其中所述催化剂部件选自选择性催化还原(SCR)催化剂、颗粒过滤器、SCR过滤器、NOx吸附剂催化剂、三元催化剂、氧化催化剂及其组合。
16.根据权利要求14或权利要求15所述的方法，其中所述低温为200℃。
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