CN102413906A - 用于从压燃式发动机排放的废气过滤颗粒物的过滤器 - Google Patents

用于从压燃式发动机排放的废气过滤颗粒物的过滤器 Download PDF

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CN102413906A
CN102413906A CN2010800192726A CN201080019272A CN102413906A CN 102413906 A CN102413906 A CN 102413906A CN 2010800192726 A CN2010800192726 A CN 2010800192726A CN 201080019272 A CN201080019272 A CN 201080019272A CN 102413906 A CN102413906 A CN 102413906A
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filter
pore size
molecular sieve
mean pore
washcoated layer
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Inventor
L·阿诺
R·布里斯利
G·R·钱德勒
A·F·基费
K·A·弗拉纳根
D·格林威尔
C·摩根
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Johnson Matthey PLC
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Johnson Matthey PLC
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Application filed by Johnson Matthey PLC filed Critical Johnson Matthey PLC
Priority to CN201610283758.XA priority Critical patent/CN105909349A/zh
Priority to CN201710913398.1A priority patent/CN107654273A/zh
Publication of CN102413906A publication Critical patent/CN102413906A/zh
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Abstract

一种用于从由压燃式发动机排放的废气过滤颗粒物(PM)的过滤器，所述过滤器包括具有进口表面和出口表面的多孔基材，其中所述进口表面通过多孔结构与所述出口表面分隔，所述多孔结构含有具有第一平均孔径大小的孔，其中所述多孔基材涂覆有包含多个固体颗粒的洗涂层，所述固体颗粒包含用至少一种金属促进的分子筛，其中洗涂的多孔基材的多孔结构含有具有第二平均孔径大小的孔，并且其中所述第二平均孔径大小小于所述第一平均孔径大小。

Description

用于从压燃式发动机排放的废气过滤颗粒物的过滤器
本发明涉及用于处理由压燃式发动机产生的颗粒物(PM)和氮氧化物的过滤器。
压燃式发动机通过将烃喷射到压缩空气中而引起烃燃烧，并且可通过柴油燃料、生物柴油燃料、柴油燃料和生物柴油燃料的共混物以及压缩天然气供给燃料。本发明目的与2010年2月26日提交的题为“Filter(过滤器)”的英国专利申请第1003244.9号要求保护的发明不同。该英国专利申请的发明目的在于用于强制点火(positive ignition)发动机废气中颗粒物的过滤器。
环境PM被大多数作者基于其空气动力学直径(空气动力学直径定义为与被测定颗粒在空气中具有相同沉降速度的1g/cm3密度球体的直径)分为以下类别：
(i)PM-10-空气动力学直径小于10μm的颗粒；
(ii)直径低于2.5μm的细颗粒(PM-2.5)；
(iii)直径低于0.1μm(或100nm)的超细颗粒；和
(iv)纳米颗粒，由小于50nm的直径表征。
自从二十世纪九十年代中期以来，由于细颗粒和超细颗粒对健康可能的不利影响，由内燃机排放的颗粒状物的粒径分布愈来愈受关注。在美国，环境空气中PM-10颗粒状物的浓度受到法律管制。由于健康研究表明人类死亡率与低于2.5μm的细颗粒的浓度之间的密切关联，因此在美国，在1997年引入了对于PM-2.5的新的另外的环境空气质量标准。
人们已转而关注由柴油发动机和汽油发动机产生的纳米颗粒，因为根据对2.5-10.0μm范围内的颗粒状物研究的结果推测，它们被认为相比较大尺寸的颗粒状物能够更加深入地渗透到人肺中，并因此被认为比较大颗粒更加有害。
柴油颗粒状物的尺寸分布具有对应于颗粒成核和附聚机理的非常确实的双峰特征，其中相应的颗粒类型分别称作核模和积聚模(参见图1)。如图1可见，在核模中，柴油PM由大量具有非常小质量的小颗粒组成。几乎所有的柴油颗粒状物尺寸均显著小于1μm，即它们包含细颗粒(即落入1997年美国法律)、超细颗粒和纳米颗粒的的混合物，。
据相信，核模颗粒主要由挥发性冷凝物(烃、硫酸、硝酸等)组成，并且含有很少的固体材料，例如灰和碳。一般认为积聚模颗粒含有与冷凝物和吸附材料(重质烃、硫物质、氮氧化物衍生物等)混合的固体(碳、金属灰等)。据相信，粗粒模颗粒不在柴油燃烧过程中产生，而是可通过例如沉积和随后从发动机气缸、排气系统或颗粒状物取样系统再夹带粒状材料等机理形成。这些模式之间的关系示于图1。
成核颗粒的组成可随发动机运行条件、环境条件(特别是温度和湿度)、稀释和取样系统条件而变。实验室工作和理论已表明，大多数核模形成和生长在低稀释比率范围内发生。在该范围内，挥发性颗粒前体(如重质烃和硫酸)的气体到颗粒的转变导致核模的成核和生长以及吸附到现有积聚模颗粒上同时发生。实验室测试(例如参见SAE980525和SAE 2001-01-0201)已表明，随着空气稀释温度的降低，核模形成强烈增加，但是关于湿度是否具有影响存在矛盾的证据。
一般而言，低温、低稀释比率、高湿度和长停留时间有利于纳米颗粒形成和生长。研究已表明，纳米颗粒主要由挥发性材料(如重质烃和硫酸)组成，有证据表明仅在非常高负载下具有固体部分。
在柴油颗粒过滤器中柴油颗粒状物的颗粒收集基于使用多孔屏障将由气体产生的颗粒状物与气相分离的原理。柴油过滤器可定义为深层过滤器和/或表面型过滤器。在深层过滤器中，过滤器介质的平均孔径大小比收集颗粒的平均直径大。通过包括扩散沉积(布朗运动)、惯性沉积(压紧)和流线截取(布朗运动或惯性)的深度过滤机理的组合，颗粒在介质上沉积。
在表面型过滤器中，过滤器介质的孔直径小于PM的直径，因此通过筛分分离PM。通过收集柴油PM本身的累积进行分离，该累积通常称为“过滤滤饼”，该方法通常称为“滤饼过滤”。
应理解的是，柴油颗粒过滤器(例如陶瓷壁流整体料)可通过深度过滤和表面过滤的组合工作：当深度过滤容量饱和并且颗粒层开始覆盖过滤表面时，过滤滤饼以较高的烟灰负载发展。深度过滤表征为比滤饼过滤稍低的过滤效率和较低的压降。
首先开发通过含氮化合物(例如氨或尿素)选择性催化还原(SCR)NOx，用于处理工业固定应用。SCR技术首先在二十世纪七十年代后期在日本用于热电厂，并自二十世纪八十年代中期以来在欧洲广泛应用。在美国，在二十世纪九十年代引入SCR系统用于燃气轮机，最近用于燃煤发电厂。除了燃煤热电联产发电厂和燃气轮机以外，SCR应用包括在化学加工工业中的工厂和炼油厂加热器和锅炉、加热炉、焦炉、市政废物处理厂和焚烧炉。最近，在欧洲、日本和美国，开发了基于SCR技术的NOx还原系统用于多种车辆(移动)应用，例如用于处理柴油废气。
在NH3 SCR系统中发生一些化学反应，所有这些化学反应代表合乎需要的将NOx还原为氮气的反应。占优势的反应用反应(1)表示。
4NO+4NH3+O2→4N2+6H2O           (1)
与氧的竞争性非选择性反应可产生二次排放或者可非生产性地消耗氨。一种该非选择性反应为示于反应(2)的氨的完全氧化。
4NH3+5O2→4NO+6H2O              (2)
另外，副反应可产生不期望的产物，例如N2O，如反应(3)所表示的。
4NH3+5NO+3O2→4N2O+6H2O         (3)
用于促进NH3-SCR的各种催化剂为已知的，包括V2O5/WO3/TiO2和过渡金属/沸石如Fe/Beta(参见US 4,961,917)和过渡金属/小孔沸石(参见WO 2008/132452)。
EP 1663458公开了一种SCR过滤器，其中该过滤器为壁流整体料，并且SCR催化剂组合物渗透壁流整体料的壁。该说明书一般性地公开了壁流过滤器的壁可在其上或其中(即，不是二者)含有一种或多种催化材料。根据该公开，当用于描述催化剂浆料在壁流整体料基材上分散时，“渗透”是指催化剂组合物在整个基材的壁中分散。
WO 2008/136232 A1公开了一种具有由多孔槽壁基础材料组成且仅在其流入侧上或在其流入和流出侧上提供表面层的槽壁，并满足以下要求(1)至(5)的蜂窝状过滤器用作DPF：(1)表面层的峰值孔直径等于或小于槽壁基础材料的平均孔直径，并且表面层的孔隙率大于槽壁基础材料；(2)关于表面层，峰值孔直径为0.3至小于20μm，并且孔隙率为60至小于95％(通过汞透入法测定)；(3)表面层的厚度(L1)为槽壁的厚度(L2)的0.5至小于30％；(4)单位过滤面积的表面层的质量为0.01至小于6mg/cm2；和(5)关于槽壁基础材料，平均孔直径为10至小于60μm，并且孔隙率为40至小于65％。还参见SAE paper2009-01-0292。
NOx吸收剂催化剂(NACs)例如由美国专利第5,473,887号得知，并且设计用于吸附贫废气(λ大于1)的氮氧化物(NOx)和在废气中的氧浓度下降时脱附NOx。脱附的NOx可使用合适的还原剂(例如，汽油燃料)还原为N2，并通过NAC本身或位于NAC下游的催化剂组分(例如铑)促进。在实践中，可响应NAC的计算剩余NOx吸附容量，将氧浓度的控制间歇地调节至所需的氧化还原组成，例如富于正常发动机运行作业(但仍贫于化学计量的或λ＝1的组成)、化学计量的或富于化学计量的(λ＜1)。可通过多种方式来调节氧浓度，例如，如在排气冲程期间将另外的烃燃料节流、喷射至发动机气缸中，或者将烃燃料直接喷射至发动机歧管下游的废气中。
典型的NAC制剂包括催化氧化组分(例如铂)、显著量(即，显著多于用作促进剂(例如TWC中的促进剂)所需)的NOx-储存组分(例如钡)和还原催化剂(例如铑)。对于该制剂，通常给出用于贫废气的NOx-储存的一种机理为：
NO+1/2O2→NO2                    (4)；和
BaO+NO2+1/2O2→Ba(NO3)2          (5)，
其中在反应(4)中，一氧化氮与氧在铂上的活性氧化部位上反应，以形成NO2。反应(5)包括通过无机硝酸盐形式的储存材料吸附NO2。
在较低氧浓度下和/或在升高的温度下，硝酸盐物质变得热动力学不稳定并分解，根据以下反应(6)产生NO或NO2。在合适的还原剂存在下，这些氮氧化物随后被一氧化碳、氢和烃还原为N2，这些反应可在还原催化剂上发生(参见反应(5))。
Ba(NO3)2→BaO+2NO+3/2O2或Ba(NO3)2→BaO+2NO2+1/2O2    (6)；和
NO+CO→1/2N2+CO2        (7)；
(其他反应包括Ba(NO3)2+8H2→BaO+2NH3+5H2O，接着是NH3+NOx→N2+yH2O或2NH3+2O2+CO→N2+3H2O+CO2等)。
在以上反应(4)-(7)中，给出反应性钡物质作为氧化物。然而，应理解的是，在空气存在下，大多数钡为碳酸盐形式或可能是氢氧化物形式。技术人员因此可改变上述反应方案以适用非氧化物的钡物质和改变废气流中的催化涂层顺序。
在欧洲，自从2000年(欧3排放标准)以来，通过新欧洲行驶循环(New European Driving Cycle，NEDC)来测试排放。它由四次重复的先前ECE 15行驶循环加上城郊行驶循环(Extra Urban Driving Cycle，EUDC)，其中在开始排放取样之前没有40秒预热期。这种修改的冷启动测试也称为“MVEG-B”行驶循环。所有排放用g/km表示。
欧5/6执行立法引入一种新的由UN/ECE颗粒测量程序(Particulate Measurement Programme，PMP)开发的PM质量排放测量方法，该方法调节PM质量排放限制以解决使用老方法和新方法的结果差异。除了基于质量的限制以外，欧5/6立法还引入了颗粒数目排放限制(PMP方法)。
2014年9月1日生效的欧洲排放立法(欧6)要求控制由柴油和汽油客车排放的颗粒数目。对于柴油EU轻型车辆，允许的限度为：500mg/km一氧化碳；80mg/km氮氧化物(NOx)；170mg/km烃与NOx的总量；4.5g/km颗粒物(PM)；和6.0×1011/km的颗粒数目标准。本说明书基于该数目在不久之后被采纳的假设。
使用催化剂组合物涂覆过滤器的难点在于平衡所需的催化活性，催化活性通常随着洗涂层(washcoat)负载、由使用中的过滤器引起的背压(增加的洗涂层负载通常提高背压)和过滤效率(以过滤效率为代价，通过采用较宽的平均孔径大小和较高孔隙率基材可降低背压)而增加。
我们现在非常意外地发现，与在EP 1663458中所公开的用洗涂层渗透过滤器壁相反，通过在其表面上用洗涂层涂覆过滤器基材整体料，可得到背压、过滤和催化活性的有益平衡。此外，我们已发现，通过适当选择分子筛尺寸，可在类似的催化活性下调节过滤器的背压，因此增加了设计选择。
根据一个方面，本发明提供一种用于从由压燃式发动机排放的废气过滤颗粒物(PM)的过滤器，所述过滤器包括具有进口表面和出口表面的多孔基材，其中所述进口表面通过多孔结构与所述出口表面分隔，所述多孔结构含有具有第一平均孔径大小的孔，其中所述多孔基材涂覆有包含多个固体颗粒的洗涂层，所述固体颗粒包含用至少一种过渡金属促进的分子筛，其中洗涂的(washcoated)多孔基材的多孔结构含有具有第二平均孔径大小的孔，并且其中所述第二平均孔径大小小于所述第一平均孔径大小。
平均孔径大小可通过汞孔隙率法测定。
应理解的是，本发明的益处实质上独立于基材的孔隙率。孔隙率衡量多孔基材中空隙空间的百分比，并且与排气系统的背压相关：一般而言，孔隙率越低，则背压越高。然而，用于本发明的过滤器的孔隙率通常大于40％或大于50％，并且可有利地使用45-75％的孔隙率，例如50-65％或55-60％。洗涂的多孔基材的平均孔径大小对于过滤是重要的。因此，可具有相对高孔隙率的多孔基材，其由于平均孔径大小也相对高，因此是差的过滤器。
多孔基材可为金属，例如烧结金属，或陶瓷，例如碳化硅、堇青石、氮化铝、氮化硅、钛酸铝、氧化铝、堇青石、莫来石例如针状莫来石(例如参见例WO 01/16050)、铯榴石、thermet例如Al2O3/Fe、Al2O3/Ni或B4C/Fe，或包含其中任何两种以上的部分的复合材料。在一个优选的实施方案中，过滤器为壁流过滤器，其包括具有多个进口通道和多个出口通道的陶瓷多孔过滤器基材，其中每个进口通道和每个出口通道被多孔结构的陶瓷壁部分地限定，其中每个进口通道通过多孔结构的陶瓷壁与出口通道分隔。该过滤器结构还公开于SAE810114，并且可参考该文件的其他细节。或者，过滤器可为泡沫或所谓的分支过滤器(partial filter)，例如在EP 1057519或WO 01/080978中所公开的那些。
在一个实施方案中，例如多孔过滤器基材的多孔结构的表面孔的第一平均孔径大小为8-45μm，例如8-25μm、10-20μm或10-15μm。在具体的实施方案中，第一平均孔径大小大于18μm，例如15-45μm，20-45μm，例如20-30μm或25-45μm。
在实施方案中，过滤器的洗涂层负载大于0.25g in-3，例如大于0.50g in-3或大于等于0.80g in-3，例如0.80-3.00g in-3。在优选的实施方案中，洗涂层负载大于1.00g in-3，例如大于等于1.2g in-3、大于1.5g in-3、大于1.6g in-3或大于2.00g in-3或例如1.6-2.4g in-3。在过滤器平均孔径大小和洗涂层负载的具体组合中，过滤器在可接受的背压下兼有所需水平的颗粒过滤和催化活性。
在第一优选的实施方案中，过滤器包括表面洗涂层，其中洗涂层实质上覆盖多孔结构的表面孔，并且洗涂的多孔基材的孔被洗涂层中颗粒之间的空间(颗粒间孔)部分地限定。也就是，实质上没有洗涂层进入多孔基材的多孔结构。制备表面涂覆的多孔过滤器基材的方法包括向多孔结构中引入聚合物(例如聚乙烯醇(PVA))，向包含聚合物的多孔过滤器基材施用洗涂层并干燥，随后煅烧涂覆的基材以烧尽聚合物。该第一实施方案的示意图示于图2A。
涂覆多孔过滤器基材的方法为技术人员已知，包括但不限于在WO 99/47260中所公开的方法，即，涂覆整体料载体的方法，包括以下步骤：(a)在载体上面设置密闭装置，(b)将预定量的液体组分装入所述密闭装置中，以(a)然后(b)的顺序或(b)然后(a)的顺序，以及(c)通过施加压力或真空，将所述液体组分带至载体的至少一部分中，并在载体内保留实质上所有的所述量。在干燥该第一涂层，以及任选的燃烧/煅烧之后，可从整体料载体的另一端重复这些工艺步骤。
在该第一实施方案中，多孔洗涂层的平均颗粒间孔径大小为5.0nm-5.0μm，例如0.1-1.0μm。
在该第一表面涂层实施方案中，固体洗涂层颗粒的D90可大于多孔过滤器基材的平均孔径大小，并且可为10-40μm，例如15-30μm或12-25μm。本文使用的“D90”限定洗涂层中的粒径分布，其中存在的90％的颗粒的直径在指定的范围内。或者，在实施方案中，固体洗涂层颗粒的平均尺寸为1-20μm。应理解的是，洗涂层中粒径范围越宽，则洗涂层可进入多孔基材的多孔结构的可能性越大。因此应当相应地理解术语“实质上没有洗涂层进入基材的多孔结构”。
根据第二实施方案，可将洗涂层涂覆在进口表面和/或出口表面上以及多孔基材的多孔结构中。我们认为，在进口表面和/或出口表面处围绕孔开口的表面涂层，由此缩小例如裸露的过滤器基材表面孔径大小，促进包含PM的气相的相互作用，而未实质限制孔体积，因此不引起背压显著增加。也就是，在多孔结构的表面处的孔包括孔开口，并且洗涂层引起实质上所有的孔开口变窄。第二实施方案的示意图示于图2B。
根据第二实施方案制备过滤器的方法可包括适当配制本领域技术人员已知的洗涂层，包括调节粘度和表面润湿特性，以及在涂覆多孔基材之后施加适当的真空(亦参见WO 99/47260)。
在我们的研发工作中，我们发现，通过下述可得到第一或第二实施方案的涂覆的过滤器：在洗涂层组合物中浸涂，接着沥干涂覆的部分，随后施加低真空以除去过量的洗涂层，然后干燥和煅烧。该方法产生表面涂层(通过扫描电子显微镜(SEM)测定)，并且在该方面区别于如EP 1663458所公开的其中SCR催化剂“渗透”过滤器壁的涂覆的过滤器。
在第一和第二实施方案中，其中在多孔基材的进口表面和/或出口表面上涂覆至少部分洗涂层，可将洗涂层涂覆在进口表面上、出口表面上或在进口表面和出口表面二者上。此外，进口表面和出口表面中之一或二者可包含多个洗涂层，其中在多层内的每个洗涂层可相同或不同，例如在第一层中的平均孔径大小可不同于第二层的。在实施方案中，预期用于在出口表面上涂覆的洗涂层不必与用于进口表面的相同。
当进口表面和出口表面均被涂覆时，洗涂层制剂可相同或不同。当进口表面和出口表面均被洗涂时，在进口表面上的洗涂层的平均孔径大小可不同于在出口表面上的洗涂层的平均孔径大小。例如，在进口表面上的洗涂层的平均孔径大小可小于在出口表面上的洗涂层的平均孔径大小。在后一种情况下，在出口表面上的洗涂层的平均孔径大小可大于多孔基材的平均孔径大小。
虽然施用于进口表面的洗涂层的平均孔径大小可以大于多孔基材的平均孔径大小，但是，有利的是，使洗涂层具有比在进口表面上的洗涂层中的多孔基材小的孔，以防止或减少任何燃灰或碎片进入多孔结构。
在第二实施方案中，其中至少部分洗涂层在多孔结构中，固体洗涂层颗粒的尺寸(例如平均尺寸)可小于多孔过滤器基材的平均孔径大小，例如为0.1-20μm，例如1-18μm、1-16μm、2-15μm或3-12μm。在具体的实施方案中，固体洗涂层颗粒的上述尺寸为D90，而非平均尺寸。
在其他具体的实施方案中，洗涂层的表面孔隙率通过在其中包括空隙增加。具有这种特征的废气催化剂例如公开于我们的WO2006/040842和WO 2007/116881。
在本文的洗涂层中的“空隙”是指在由固体洗涂层材料限定的层中存在空间。空隙可包括任何空缺、细孔、隧道状态(圆柱、棱柱)、裂缝等，并且可通过以下方式引入：在用于涂覆在过滤器基材上的洗涂层组合物中包含在煅烧涂覆的过滤器基材期间燃烧的材料(例如短切棉)或者在分解或燃烧时通过形成气体而产生孔的材料。
洗涂层的平均空隙比率可为5-80％，而空隙的平均直径可为0.2-500μm，例如10-250μm。
促进剂金属可选自Cu、Hf、La、Au、In、V、镧系元素和VIII族过渡金属(例如Fe)中的至少一种。用于本发明的分子筛可为硅铝酸盐沸石、金属取代的硅铝酸盐沸石或非沸石分子筛。适用于本发明的金属取代的分子筛包括具有一种或多种金属掺入到分子筛骨架中的的那些，例如Fe在骨架中的Beta和Cu在骨架中的CHA。
当分子筛为非沸石分子筛时，其可为选自磷铝酸盐(AlPO)分子筛、金属取代的磷铝酸盐分子筛(MeAlPO)沸石、硅磷铝酸盐(SAPO)分子筛和金属取代的硅磷铝酸盐(MeAPSO)分子筛的磷铝酸盐分子筛。
具体地，分子筛可为小、中或大孔分子筛。本文中“小孔分子筛”是指含有最大环尺寸为8的分子筛，例如CHA；本文中“中孔分子筛”是指含有最大环尺寸为10的分子筛，例如ZSM-5；以及本文中“大孔分子筛”是指含有最大环尺寸为12的分子筛，例如beta。具体应用于本发明的小孔分子筛为在WO 2008/132452的表1中所列的那些中的任一种。
可用分子筛的具体实例选自AEI、ZSM-5、ZSM-20、ERI、LEV、丝光沸石、BEA、Y、CHA，MCM-22和EU-1。
金属取代基和/或过渡金属促进剂可选自周期表的IB、IIB、IIIA、IIIB、VB、VIB、VIB和VIII族。
在实施方案中，金属可选自Cr、Co、Cu、Fe、Hf、La、Ce、In、V、Mn、Ni、Zn、Ga和贵金属Ag、Au、Pt、Pd和Rh。
特别令人关注的在所谓的NH3-SCR中用作过渡金属促进剂的金属选自Ce、Fe和Cu。合适的含氮还原剂包括氨。氨可原位产生，例如在设置在过滤器上游的NAC的富再生期间(参见上述反应(6)和(7)的备选)。或者，可将含氮还原剂或其前体直接喷射至废气中。合适的前体包括甲酸铵、尿素和氨基甲酸铵。可通过水热或催化水解将前体分解为氨和其他副产物。
根据另一个方面，本发明提供一种用于压燃式发动机的排气系统，所述系统包括本发明的过滤器。用于本发明该方面的压燃式发动机可通过柴油燃料、生物柴油燃料、柴油燃料和生物柴油燃料的共混物以及压缩天然气来供给燃料。
在一个实施方案中，排气系统包括将含氮还原剂或其前体喷射至过滤器上游的废气中的装置。在一个具体的实施方案中，含氮还原剂为流体。
在另一方面，本发明提供一种压燃式发动机，所述发动机包括本发明的排气系统。
在又一个方面，本发明提供一种通过深度过滤从由压燃式发动机排放的废气捕获颗粒物(PM)的方法，所述方法包括使含有PM的废气与过滤器接触，所述过滤器包括具有进口表面和出口表面的多孔基材，其中所述进口表面通过多孔结构与所述出口表面分隔，所述多孔结构含有具有第一平均孔径大小的孔，其中所述多孔基材涂覆有包含多个固体颗粒的洗涂层，所述固体颗粒包含用至少一种金属促进的分子筛，其中所述洗涂的多孔基材的多孔结构含有具有第二平均孔径大小的孔，并且其中所述第二平均孔径大小小于所述第一平均孔径大小。
在又一方面，本发明提供一种通过以下步骤调节压燃式发动机的排气系统中的过滤器背压的方法：用第一过渡金属促进的分子筛SCR催化剂涂覆过滤器，测试过滤器背压以确定是否满足预定的背压要求，和选择第二过渡金属促进的分子筛SCR催化剂，以便降低包括涂覆有第一过渡金属促进的分子筛SCR催化剂的过滤器的系统中的背压，其中第二分子筛的孔径大小大于第一分子筛。
为了能更充分地理解本发明，参考附图，其中：
图1为显示在柴油发动机的废气中的PM的尺寸分布的图。为了比较，汽油尺寸分布示于SAE 1999-01-3530的图4；
图2A和图2B显示本发明洗涂的多孔过滤器基材的三个实施方案的示意图；
图3为涉及多孔过滤器基材、多孔洗涂层和包含多孔表面洗涂层的多孔过滤器基材的孔径大小分布的汞孔隙率法的示意图；
图4为显示烟灰负载背压研究的结果的图，该研究在可比的洗涂层负载下相对涂覆有两种不同的氧化催化剂洗涂层负载(g/in3)的5.66英寸×6英寸SiC壁流过滤器和裸露的过滤器(均不根据本发明)与Fe/beta沸石选择性催化还原(SCR)催化剂(根据本发明)的烟灰负载比较背压；
图5为比较Cu/SSZ-13沸石(小孔沸石)催化剂和Fe/Beta沸石(大孔沸石)SCR催化剂在相同的烟灰负载背压测试中的背压的图；和
图6为比较来自以下的颗粒数目(颗粒数目/千米)的柱形图：装备有标准柴油氧化催化剂的2.0升符合欧5的轻型柴油车辆，接着是涂覆有Fe/Beta沸石SCR催化剂以满足欧5/6颗粒数目排放限制6×1011km-1(UN/ECE颗粒测定程序(PMP))的23μm标称平均孔径大小的3.0升SiC过滤器，以及使用裸露的过滤器的相同系统。
图2A和图2B显示通过包含表面孔12的多孔过滤器基材10的截面图。图2A显示第一实施方案，其特征在于由固体洗涂层颗粒组成的多孔表面洗涂层14，颗粒之间的空间限定孔(颗粒间孔)。可以看到，洗涂层14实质上覆盖多孔结构的孔12，并且颗粒间孔16的平均孔径大小小于多孔过滤器基材10的平均孔径大小12。
图2B显示包含洗涂层的第二实施方案，该洗涂层涂覆在进口表面16上并另外涂覆在多孔基材10的多孔结构12中。可以看到，洗涂层14引起表面孔12的孔开口变窄，使得涂覆的多孔基材的平均孔径大小18小于多孔过滤器基材10的平均孔径大小12。
图3显示将多孔过滤器基材20、多孔洗涂层22和包括表面洗涂层24的多孔柴油过滤器基材的孔径大小与孔数目关联的图。可以看到，过滤器基材的平均孔径大小为约15μm的量级。洗涂层具有由颗粒内孔22A(在该范围的纳米端)和颗粒间孔22B(朝向该范围的微米端)组成的双峰分布。还可以看到，通过用本发明的洗涂层涂覆多孔过滤器基材，裸露的过滤器基材的孔分布在颗粒间洗涂层孔径大小的方向移动(参见箭头)。
仅通过举例说明的方式提供以下实施例。在各实施例中，烟灰负载背压(“SLBP”)测试使用在EP 1850068中所描述的装置和方法，即：
(i)用于产生和收集由液体含碳燃料燃烧产生的颗粒物的装置，所述装置包括具有喷嘴的燃料燃烧器，所述喷嘴容纳在容器中，所述容器包括气体进口和气体出口，所述气体出口与用于将气体从气体出口输送至大气的导管连接，用于检测流经气体进口的气体速率的装置以及强制氧化性气体经由容器、气体出口和导管从气体进口流动至大气的装置，从流经导管的气体收集颗粒物的站点以及用于响应在气体进口处检测到的气体流速而控制气体强制流动装置的装置，由此将在气体进口处气流的速率保持在所需的速率，以便在容器内提供亚化学计量的燃料燃烧，从而促进颗粒物形成；和
(ii)产生和收集由在氧化性气体中燃烧液体含碳燃料产生的颗粒物的方法，所述方法包括：在燃料燃烧器中的亚化学计量量的氧化性气体中燃烧燃料，所述燃料燃烧器包括喷嘴，所述喷嘴容纳在容器中；强制氧化性气体经由容器的气体出口和与气体出口连接的导管从容器的气体进口流动至大气；在位于导管内的站点收集颗粒物；检测在气体进口处氧化性气流的速率；和控制氧化性气流的速率，使得在气体进口处保持氧化性气流的所需速率。
将过滤器插入用于从流经导管的气体收集颗粒物的站点中。首先使用低硫柴油燃料(10ppm S)将新的过滤器在80kg/hr空气流速下在贫燃烧的燃烧流中预调适(pre-condition)，以将过滤器进口温度升至650℃，该温度通常用于车辆以使负载烟灰的过滤器再生。该预调适步骤温度远高于烟灰燃烧温度，并用于确保在开始时用于测试的过滤器是干净的。设置在站点上游和下游的压力传感器监测横跨过滤器的背压。将相对时间的背压绘制于附图4-6。在180kg/小时燃烧低硫柴油燃料(10ppm S)的空气流速下，在250℃过滤器进口温度下进行SLBP测试。
实施例1-CSF和SCR催化剂涂覆的过滤器背压比较
将具有60％孔隙率并且平均孔径大小为20-25μm的三种市售未涂覆的5.66英寸×6英寸SiC壁流过滤器分别各自涂覆包含负载于基于氧化铝的金属氧化物上的贵金属的用于催化烟灰过滤器(CSF)的催化剂洗涂层和Cu/Beta沸石选择性催化还原(SCR)催化剂涂层。根据在WO 99/47260中所公开的方法得到CSF涂层，即涂覆整体料载体的方法，该方法包括以下步骤：(a)在载体上面设置密闭装置，(b)将预定量的液体组分装入所述密闭装置中，以(a)然后(b)的顺序或(b)然后(a)的顺序，以及(c)通过施加压力或真空，将所述液体组分带至载体的至少一部分中，并在载体内保留实质上所有的所述量。将涂覆的产品干燥并煅烧，随后可从壁流过滤器的另一端重复工艺步骤。通过以下步骤得到SCR涂覆的过滤器：浸涂，接着是沥干，施加低真空以除去过量的洗涂层，然后干燥和煅烧。该方法产生表面涂层(通过扫描电子显微镜(SEM)测定)，并且在该方面区别于如EP 1663458所公开的其中SCR催化剂“渗透”过滤器壁的涂覆的过滤器。在0.6g/in3和1.2g/in3下得到两种不同的CSF洗涂层负载。在1.1g/in3负载下洗涂SCR涂覆的过滤器。
使用SLBP测试来测试三种涂覆的过滤器，第四种未涂覆的过滤器用作对照。结果示于图4，由该图可以看到，比起SCR涂覆的过滤器，在大致相同的洗涂层负载下CSF涂层具有显著更高的背压。因此，我们推断，在CSF和SCR涂覆的过滤器之间存在固有的涂层孔隙率差异。
实施例2-SCR催化剂涂覆的过滤器背压比较
使用Cu/SSZ-13沸石和Cu/Beta沸石SCR催化剂，将具有60％孔隙率并且平均孔径大小为20-25μm的相同的市售5.66英寸×7.5英寸SiC壁流过滤器洗涂至负载为1.1g/in3，每种催化剂具有4.8-5μm的相同粒径D90(洗涂层中90％的颗粒具有的粒径)，但是过渡金属/沸石除外，所有其他方面均实质上相同。制造方法为浸涂部件，接着沥干，施加低真以除去过量的洗涂层，随后干燥和煅烧。进行SLBP测试以比较完成的部件。
结果呈现于图5，由该图可以看到，比起涂覆有Cu/SSZ-13沸石催化剂的过滤器，涂覆有Cu/Beta沸石催化剂的过滤器具有较低的背压增加速率。由于两种SCR催化剂的基础差异为：SSZ-13沸石的孔径大小为3.8×3.8埃，而Beta沸石的孔径大小为5.6-7.7埃(来源：国际沸石协会结构委员会)，我们推断，通过选择具有适当孔径大小的基于分子筛的SCR催化剂，以达到所需的背压目标并同时满足NOx排放标准，可调节排气系统中的背压，从而增加设计选择。
实施例3-车辆测试
将通过在实施例1中所描述的浸涂方法制造的具有58％孔隙率和23μm标称平均孔径大小Cu/Beta沸石SCR催化剂涂覆的过滤器的3.0升容量SiC过滤器在标准柴油氧化催化剂后面插入2.0升符合欧5的轻型柴油车辆的排气系统。随后通过MVEG-B行驶循环驱动含有新的(即，未老化的)催化过滤器的车辆，随后是连续三次的MVEG-B循环的EUDC部分，以预调适过滤器。
在欧洲，自从2000年(欧3排放标准)以来，通过新欧洲行驶循环(NEDC)测试排放。它由四次重复的先前ECE 15行驶循环加上一次城郊行驶循环(EUDC)组成，在开始排放取样之前没有40秒预热期。该修改的冷启动测试也称为“MVEG-B”行驶循环。所有排放用g/km表示。
欧5/6执行立法引入一种新的由UN/ECE颗粒测量程序(PMP)开发的PM质量排放测量方法，该方法调节PM质量排放限制以解决使用老方法和新方法的结果差异。除了基于质量的限制以外，欧5/6立法还引入了颗粒数目排放限制(PMP方法)。使用PMP方案，6×1011km-1的新的欧5/6颗粒数目排放限制允许在测试系统之前预调适系统，以确定是否满足MVEG-B行驶循环排放标准。
随后使用预调适的系统进行重复的冷MVEG-B循环。将系统中的涂覆的过滤器换成未涂覆的过滤器作为对照。结果示于比较颗粒数目排放(颗粒数目/km)的图6的柱形图，由该图可以看到，尽管预调适，预期预调适形成提供改进的过滤的烟灰滤饼，未涂覆的过滤器开始时未通过6×10-11km-1的颗粒数目排放限制，但是，随着行驶循环，颗粒数目一直减少至排放标准内。通过对比可以看到，涂覆的过滤器在预调适之后从第一个行驶循环时已充分落入排放标准内。我们认为这些数据是指，涂覆的过滤器促进烟灰滤饼形成，其改进柴油颗粒过滤，并因此更加直接地减少颗粒数目，然而，由实施例2可以看到，在类似的洗涂层负载(参见实施例1)下，与Cu/SSZ-13沸石SCR催化剂或CSF涂层相比，Cu/Beta沸石涂覆的过滤器提供较低的背压。因此，表面Cu/Beta SCR催化剂涂层取消了在进行过滤之前在较高孔隙率/平均孔径大小的过滤器上具有烟灰层的要求。因此，与为了满足排放标准而制定的理想行驶循环条件相比，本发明提供在“真实世界”驾驶条件中颗粒数目减少的益处。
为了避免任何疑惑，本文引用的所有现有技术文件的全部内容通过引用结合到本文中。

Claims (32)

1.一种用于从由压燃式发动机排放的废气过滤颗粒物(PM)的过滤器，所述过滤器包括具有进口表面和出口表面的多孔基材，其中所述进口表面通过多孔结构与所述出口表面分隔，所述多孔结构含有具有第一平均孔径大小的孔，其中所述多孔基材涂覆有包含多个固体颗粒的洗涂层，所述固体颗粒包含用至少一种过渡金属促进的分子筛，其中洗涂的多孔基材的多孔结构含有具有第二平均孔径大小的孔，并且其中所述第二平均孔径大小小于所述第一平均孔径大小。
2.权利要求1的过滤器，其中所述多孔基材的多孔结构的第一平均孔径大小为8-45μm。
3.权利要求1或2的过滤器，其中所述洗涂层负载大于0.50gin-3。
4.权利要求3的过滤器，其中所述洗涂层负载大于1.00g in-3。
5.权利要求1、2、3或4的过滤器，所述过滤器包括表面洗涂层，其中洗涂层实质上覆盖所述多孔结构的表面孔，并且洗涂的多孔基材的孔被所述洗涂层中的颗粒之间的空间(颗粒间孔)部分地限定。
6.权利要求5的过滤器，其中多孔洗涂层的平均颗粒间孔径大小为5.0nm-5.0μm。
7.前述权利要求中任一项的过滤器，其中固体洗涂层颗粒的平均尺寸大于所述第一平均孔径大小。
8.权利要求7的过滤器，其中所述固体洗涂层颗粒的平均尺寸为1-40μm。
9.权利要求1、2、3或4的过滤器，其中在所述多孔结构的表面处的孔包括孔开口，并且所述洗涂层引起实质上所有的表面孔开口变窄。
10.权利要求9的过滤器，其中固体洗涂层颗粒的平均尺寸小于所述多孔基材的平均孔径大小。
11.权利要求10的过滤器，其中固体洗涂层颗粒的平均尺寸为0.1-20μm。
12.权利要求10的过滤器，其中固体洗涂层颗粒的D90为0.1-20μm。
13.前述权利要求中任一项的过滤器，其中在进口表面、出口表面或者进口表面和出口表面二者上涂覆所述洗涂层。
14.权利要求13的过滤器，其中所述进口表面和所述出口表面均被洗涂，并且其中在所述进口表面上的洗涂层的平均孔径大小与在所述出口表面上的洗涂层的平均孔径大小不同。
15.权利要求14的过滤器，其中在所述进口表面上的洗涂层的平均孔径大小小于在所述出口表面上的洗涂层的平均孔径大小。
16.权利要求15的过滤器，其中在所述出口表面上的洗涂层的平均孔径大小大于所述多孔基材的平均孔径大小。
17.前述权利要求中任一项的过滤器，其中所述多孔基材为陶瓷壁流过滤器、金属过滤器或陶瓷泡沫。
18.权利要求17的过滤器，其中所述金属过滤器为烧结金属过滤器、分支过滤器和/或包括丝网。
19.前述权利要求中任一项的过滤器，其中所述分子筛为硅铝酸盐沸石、金属取代的硅铝酸盐沸石或非沸石分子筛。
20.权利要求19的过滤器，其中所述非沸石分子筛为选自磷铝酸盐(AlPO)分子筛、金属取代的磷铝酸盐分子筛(MeAlPO)沸石、硅磷铝酸盐(SAPO)分子筛和金属取代的硅磷铝酸盐(MeAPSO)分子筛的磷铝酸盐分子筛。
21.权利要求19或20的过滤器，其中至少一种分子筛为小孔分子筛、中孔分子筛或大孔分子筛。
22.权利要求22或23的过滤器，其中至少一种分子筛选自AEI、ZSM-5、ZSM-20、ERI、LEV、丝光沸石、BEA、Y、CHA、MCM-22和EU-1。
23.权利要求19、20、21或22的过滤器，其中金属取代基和/或过渡金属促进剂选自周期表的IB、IIB、IIIA、IIIB、VB、VIB、VIB和VIII族。
24.权利要求23的过滤器，其中所述过渡金属选自Cr、Co、Cu、Fe、Hf、La、Ce、In、V、Mn、Ni、Zn、Ga和贵金属Ag、Au、Pt、Pd和Rh。
25.权利要求23或24的过滤器，其中所述过渡金属选自Cu、Pt、Mn、Fe、Co、Ni、Zn、Ag、Ce和Ga。
26.权利要求23、24或25的过滤器，其中所述过渡金属选自Ce、Fe和Cu。
27.一种用于压燃式发动机的排气系统，所述系统包括前述权利要求中任一项的过滤器。
28.权利要求27的排气系统，所述系统包括用于将含氮还原剂喷射至所述过滤器上游的废气中的装置。
29.一种压燃式发动机，所述发动机包括权利要求27或28的排气系统。
30.权利要求29的压燃式发动机，所述压燃式发动机以烃燃料作为燃料，所述烃燃料选自柴油燃料、生物柴油燃料、柴油燃料和生物柴油燃料的共混物以及压缩天然气。
31.一种通过深度过滤从由压燃式发动机排放的废气捕获颗粒物(PM)的方法，所述方法包括使含有PM的废气与过滤器接触，所述过滤器包括具有进口表面和出口表面的多孔基材，其中所述进口表面通过多孔结构与所述出口表面分隔，所述多孔结构含有具有第一平均孔径大小的孔，其中所述多孔基材涂覆有包含多个固体颗粒的洗涂层，所述固体颗粒包含用至少一种过渡金属促进的分子筛，其中洗涂的多孔基材的多孔结构含有具有第二平均孔径大小的孔，并且其中所述第二平均孔径大小小于所述第一平均孔径大小。
32.一种通过以下步骤调节压燃式发动机的排气系统中的过滤器背压的方法：用第一过渡金属促进的分子筛SCR催化剂涂覆过滤器，测试所述过滤器背压以确定其是否满足预定的背压要求，和选择第二过渡金属促进的分子筛SCR催化剂，以便降低包括涂覆有所述第一过渡金属促进的分子筛SCR催化剂的过滤器的系统中的背压，其中所述第二分子筛的孔径大小大于所述第一分子筛。
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