CN101605968B - 具有氨阻滞作用的催化活化的柴油机粒子过滤器 - Google Patents
具有氨阻滞作用的催化活化的柴油机粒子过滤器 Download PDFInfo
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- CN101605968B CN101605968B CN2008800046703A CN200880004670A CN101605968B CN 101605968 B CN101605968 B CN 101605968B CN 2008800046703 A CN2008800046703 A CN 2008800046703A CN 200880004670 A CN200880004670 A CN 200880004670A CN 101605968 B CN101605968 B CN 101605968B
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- diesel particulate
- particulate filter
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- catalytic
- filter
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- 229940095054 ammoniac Drugs 0.000 title description 4
- 230000000903 blocking effect Effects 0.000 title description 4
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- 238000000576 coating method Methods 0.000 claims abstract description 100
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- MWUXSHHQAYIFBG-UHFFFAOYSA-N nitrogen oxide Inorganic materials O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 claims abstract description 79
- 230000003197 catalytic effect Effects 0.000 claims abstract description 71
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- JCXJVPUVTGWSNB-UHFFFAOYSA-N nitrogen dioxide Inorganic materials O=[N]=O JCXJVPUVTGWSNB-UHFFFAOYSA-N 0.000 description 2
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- 241001074085 Scophthalmus aquosus Species 0.000 description 1
- XHCLAFWTIXFWPH-UHFFFAOYSA-N [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] XHCLAFWTIXFWPH-UHFFFAOYSA-N 0.000 description 1
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- VUZPPFZMUPKLLV-UHFFFAOYSA-N methane;hydrate Chemical compound C.O VUZPPFZMUPKLLV-UHFFFAOYSA-N 0.000 description 1
- 229910000476 molybdenum oxide Inorganic materials 0.000 description 1
- QGLKJKCYBOYXKC-UHFFFAOYSA-N nonaoxidotritungsten Chemical compound O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 QGLKJKCYBOYXKC-UHFFFAOYSA-N 0.000 description 1
- PQQKPALAQIIWST-UHFFFAOYSA-N oxomolybdenum Chemical compound [Mo]=O PQQKPALAQIIWST-UHFFFAOYSA-N 0.000 description 1
- 150000002978 peroxides Chemical class 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
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- YOWAEZWWQFSEJD-UHFFFAOYSA-N quinoxalin-2-amine Chemical compound C1=CC=CC2=NC(N)=CN=C21 YOWAEZWWQFSEJD-UHFFFAOYSA-N 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
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- 229910052703 rhodium Inorganic materials 0.000 description 1
- 239000010948 rhodium Substances 0.000 description 1
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
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- -1 transition-metal cation Chemical class 0.000 description 1
- 229910001930 tungsten oxide Inorganic materials 0.000 description 1
- 229910001935 vanadium oxide Inorganic materials 0.000 description 1
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Classifications
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Abstract
本发明提出了一种具有氨阻滞作用的催化活化的柴油机粒子过滤器,其除了氧化活性的涂层(2)之外,还包含在SCR反应中呈催化活性的涂层(1)。借助于本发明的柴油机粒子过滤器,能够显著更加简便和低廉地构造用于从贫燃发动机的尾气中除去氮氧化物和粒子的尾气净化设备。
Description
技术领域
本发明涉及催化活化的柴油机粒子过滤器,其除了具有柴油机粒子过滤器典型的性能之外,还具有氨阻滞作用。本发明进一步涉及在于各种实施方式中采用本发明的催化活化的柴油机粒子过滤器的情况下,用于从主要在贫燃条件下工作的内燃机的尾气中除去氮氧化物和粒子的尾气净化设备。
背景技术
机动车尾气中存在的排放物可以分为两类。由此,术语“一次排放物”表示有害气体,其通过燃料在发动机中的燃烧过程直接形成,且在其通过尾气清洁装置之前已存在于所谓的原始排放物中。“二次排放物”表示可以在尾气清洁设备中作为副产物形成的那些有害气体。
贫燃发动机的尾气既包括常见的一次排放物一氧化碳CO、烃HC和氮氧化物NOx,也包括高达15体积%的相对高含量的氧。在柴油发动机的情形下,除了气态的一次排放物之外还有粒子排放物,其主要由烟灰残留物和可能的有机聚集体组成,且产生于汽缸中一部分不彻底的燃料燃烧。
特别是在柴油机动车的情形下,遵守由欧洲、北美和日本的未来生效的尾气排放法规规定的尾气极限值,不仅需要从尾气中除去氮氧化物(脱氮),而且需要其净化粒子。有害气体一氧化碳和烃可以从贫燃尾气中容易地在适宜氧化催化剂之上通过氧化而变为无害。氮氧化物还原为氮气的过程由于高氧含量而更加困难。对于粒子排放物的去除,不可避免地要使用特定的柴油机粒子过滤器。
用于从尾气中除去氮氧化物的已知方法,一方面是采用氮氧化物储存催化剂(NOx存储催化剂NSC)的方法,另一方面也是在适宜催化剂(简称SCR催化剂)上借助于氨来选择性催化还原(SCR)的方法。
氮氧化物储存催化剂的清洁作用是基于,在发动机的贫燃工作阶段中氮氧化物主要以硝酸盐形式被储存催化剂的储存材料而储存。当NSC的储存容量耗尽时,该催化剂必须在发动机的随后富燃工作阶段中得到再生。这点意味着先前形成的硝酸盐分解且再次释放的氮氧化物与还原性尾气组分在储存催化剂上反应形成氮气、二氧化碳和水。SAE文献SAE 950809中详细地描述了氮氧化物储存催化剂的工作方式。
由于柴油发动机中富燃工作阶段的实现不可能轻而易举且NSC再生所需的富燃尾气条件的建立经常要求辅助措施如补充喷射燃料到尾气管线中,因此该SCR方法优选地用于柴油机动车尾气的脱氮。
这种方法中,依据发动机理念和尾气设备的结构,区分为“主动”和“被动”SCR方法。“被动”SCR方法中,在尾气设备中,特意产生的氨二次排放物作为用于脱氮的还原剂。
例如,US 6 345 496 B1描述了清洁发动机尾气的方法,其中调节反复交替的贫燃和富燃的空气/染料比例,且将由此产生的尾气引导通过尾气设备,该尾气设备在流入侧含有仅在富燃尾气条件下将NOx转化为NH3的催化剂,同时设置在流出侧上的另一催化剂在贫燃尾气中吸收或存入NOx,且将其在富燃条件下释放,从而使得其可以与由流入侧催化剂产生的NH3反应以获得氮气。或者,依据US 6 345 496 B1,可以将NH3-吸收催化剂和氧化催化剂设置在流出侧上,其在富燃条件下储存NH3,使其在贫燃条件下解吸附并用氧气使其氧化以获得氮气和水。这种方法的其它公开内容是已知的。
类似于使用氮氧化物储存催化剂,这种“被动”SCR方法存在缺点,即它们的一个基本组成部分是提供富燃尾气条件,其通常对于原位产生作为还原剂的氨而言是需要的。
与此相反,在“主动”SCR方法中,借助于喷嘴从所携带的添加罐将还原剂计量加入尾气管线中。作为这样的还原剂,除了氨之外,也可以采用易于分解为氨的化合物,例如脲或氨基甲酸铵。必须至少以相对于氮氧化物化学计量的比例将氨供入尾气。由于机动车变化极大的工作条件,精确计量添加氨存在很大难度。这样在一些情形下导致在SCR催化剂下游有显著的氨渗透。为了防止氨的二次排放,通常在SCR催化剂下游设置氧化催化剂,其旨在将渗透的氨氧化为氮气。这种催化剂在下文中称作氨阻滞催化剂。
设置在SCR催化剂下游用于渗透的氨的氧化的氨阻滞催化剂在许多实施方式中是已知的。例如,DE 3929297 C2(US 5120695)描述了这种催化剂设置。据此,将氧化催化剂以涂层施用到单块的、作为蜂巢形式的实心挤出物(Vollextrudat)形式的还原催化剂的流出侧那部分,其中涂布有氧化催化剂的区域占据整个催化剂体积的20~50%。该氧化催化剂包括,作为催化活性的组分的至少一种沉积在作为载体材料的氧化铈、氧化锆和氧化铝上的铂族金属铂、钯和铑。
依据EP 1 399 246 B1,也可以通过浸渍铂族金属的可溶性前体而将铂族金属直接施用到作为载体材料的还原催化剂的组分上。
依据JP 2005-238199,也可以在二氧化钛、氧化锆、氧化硅或氧化铝和过渡金属或稀土金属构成的层之下,引入含有贵金属的氨-氧化催化剂层。
为了从柴油机动车的尾气中除去粒子排放物,使用特定的柴油机粒子过滤器,其可以设置有含氧化催化剂的涂层以改进他们的性能。这种涂层,如SAE文献SAE 2005-01-1756中所述,用于降低用于基于氧的粒子燃尽(烟灰燃烧)的活化能且由此降低过滤器上烟灰点燃温度,并通过尾气中含有的一氧化氮氧化为二氧化氮改进被动再生性能以及且抑制烃和一氧化氮排放物的渗透。
过滤器基材的涂覆中一个特殊问题是,由于施用的涂层而导致尾气反压(-gegendruck)的升高。该尾气反压由于工作期间在过滤器上的烟灰沉积物已连续地升高,且由此降低了发动机的效率。由此必须通过烧掉烟灰不时地将过滤器再生。当涉及的是涂布过的过滤器基材时,通常虽然便利于烟灰燃尽,但是未有积垢的、经涂布的过滤器的尾气反压经常已高于未经涂布的过滤器的尾气反压。由此不能够立即通过涂层改变,例如通过额外引入催化活性的组分而改变粒子过滤器的催化功能。
如果为了满足法定的尾气极限值的目的而需要从柴油机机动车的尾气中脱氮和除去粒子二者,则所述用于除去各个有害气体的措施通过串联在相应传统尾气设备中结合。例如,WO 99/39809描述了尾气净化***,其中用于将NOx中NO氧化为NO2的氧化催化剂、粒子过滤器、还原剂计量添加装置和SCR催化剂彼此相继。为了防止氨渗透,通常在SCR下游需要额外的氨阻滞催化剂,且其是在SCR催化剂的流出侧上的催化剂序列的延续。
DE 20 2005 008 146 U1公开了用于机动车的尾气设备,其包括至少一个可再生的粒子过滤器和在粒子过滤器下游连接的具有氨储存容量的SCR催化剂,其中该下游连接的SCR催化剂,依据该文献中的描述,用于特别是拉平(abzufangen)在粒子过滤器再生期间出现的尾气中的NH3-峰值,这就是为何将SCR催化剂连接在粒子过滤器的下游的原因。
这种传统***由于大量所需的催化剂而是昂贵的。催化剂的串联另外导致对尾气设备中安装空间的高需求。特别是在较小机动车中经常发现他们的安装是困难的。另外,催化剂的串联连接(其中每一种在待清洁的尾气上发挥其固有的背压(Staudruck)),导致在整个尾气设备之上尾气反压的不利价值,且由此降低了发动机的效率。
在DE 20 205 008 146 U1中所述***的优选实施方式中,粒子过滤器和SCR催化剂与常规***体(其一般是单片陶瓷基材)形成公共的组合单元。SCR催化剂在此仅通过在流出侧上陶瓷基材的相应涂覆而形成。
发明内容
本发明的目的是,通过改进现有粒子过滤器技术,提供这样的部件,即,通过其的使用能够使用于从贫燃发动机的尾气中同时脱氮和除去粒子的尾气净化设备简化,同时省去尾气清洁装置。同时,本发明的目的是有助于这种设备的尾气反压的最小化且同时显示成本节约的潜力。
通过催化活化的柴油机粒子过滤器实现了该目的,其包括过滤体和氧化活性催化涂层以及在SCR反应中呈催化活性的另一涂层。在SCR反应中呈催化活性的涂层的特征在于其中含有氨储存材料。该柴油机粒子过滤器的特征在于,保持层的设置,使得待清洁的尾气首先经过在SCR反应中呈催化活性的涂层和随后经过氧化活性的催化涂层。
通过用于从在主要为贫燃条件下工作的内燃机的尾气中除去氮氧化物和粒子的尾气净化设备也实现了该目的,该设备除了用于除去氮氧化物的催化剂外,还包括本发明的催化活化的柴油机粒子过滤器。
由于已任选地含于传统粒子过滤器中的氧化活性涂层与在SCR反应中呈催化活性的涂层(“SCR涂层”、“SCR活性层”)的组合,该柴油机粒子过滤器包含额外的氨阻滞作用。该涂层组合能使该粒子过滤器,除了已存在的功能(具有降低的烟灰点燃温度的粒子过滤/粒子燃尽过程;改进的被动再生性能,NO-氧化,抑制CO-和HC-排放物的渗透)之外,还一方面能将氮氧化物还原为氮气,且另一方面能将氨氧化为氮气。当待清洁的尾气首先通过SCR活性层并随后通过氧化活性涂层时,认为关于含氮有害气体转化的多功能性是基于图1中示意地所示的下列反应进程:
1)尾气中的氮氧化物和氨吸附在SCR活性层(1)上并在选择性催化反应中反应生成水和氮气,其在反应完成后解吸附。在此存在超化学计量量的、即存在过量的氨。
2)过量氨扩散到SCR活性层(1)中。一部分氨储存在此。
3)未被储存的氨经由SCR活性层(1)到达氧化活性涂层(2)。在此,产生氮气和氮氧化物。形成的氮气不变地经由SCR层(1)扩散过去并到大气中。
4)在氧化活性层(2)中形成的氮氧化物离开该***之前,它们再次通过SCR活性涂层(1)。它们在此与先前储存的氨NH3-储存的在SCR反应中反应生成N2。
为了所述反应进程能导致含氮的有害气体的最大转化率,当SCR活性涂层具有足够的氨储存容量时是有利的。为了确保这一点,本发明柴油机粒子过滤器中的SCR活性层包含氨储存材料。在该文献的上下文中,氨储存材料是含有氨可以键合于其上的酸性中心的化合物。本领域技术人员把这些区分为用于氨的物理吸附的Lewis酸中心和用于氨的化学吸附的布伦斯特()酸中心。本发明柴油机粒子过滤器中的氨储存材料必须含有主要比例的布伦斯特酸中心和任选的路易斯(Lewis)酸中心,以确保足够的氨储存能力。
借助于程序控温解吸附,可确定催化材料的氨储存能力有多高。在这种表征非均相催化剂的标准方法中,使待表征的材料在将可能吸附的组分(例如水)加热之后,负载上特定量的氨气。这点在室温下进行。随后将样品在惰性气体下以恒定加热速率加热,使得样品先前吸收的氨气解吸附并可以采用适宜的分析方法来进行定量检测。作为用于材料的氨储存能力的特征值,得到每克催化剂材料的氨数量(以毫升计),其中术语“催化剂材料”总表示为表征所使用的材料。该特征值取决于所选的加热速率。该文献中报道的数值总是指的是采用4开尔文/分钟的加热速率的测量。
本发明柴油机粒子过滤器中在SCR反应中呈催化活性的涂层的氨储存能力优选是至少20毫升氨/克催化剂材料,更优选为高达70毫升/克催化剂材料。特别适宜的SCR活性层是氨储存能力为25~40毫升氨/克催化剂材料的那些。
具有所述氨储存性能的SCR活性涂层优选地包括已与氢阳离子(“H-沸石”)或过渡金属阳离子交换过的沸石。非常适宜的是与铁或铜或铁和铜交换过的沸石,其中优选为β-沸石或Y-沸石或八面沸石或丝光沸石或ZSM-5或其组合。
在本发明特别适宜的一个方式中,本发明柴油机粒子过滤器的SCR活性涂层不含贵金属。这样确保了SCR反应中的选择性尽可能高。为了进一步改进SCR活性,也能够含有选自氧化铈、氧化钛、氧化锆、氧化钒、氧化钼、氧化钨、二氧化硅、和其混合物和/或混合氧化物的添加剂。
许多传统的柴油机粒子过滤器包括氧化活性涂层。在本发明柴油机粒子过滤器中,其优选地不含沸石。在本发明特别适宜的一个实施方式中,该氧化活性催化涂层包含在选自高表面积的活性氧化铝、氧化铈、氧化锆、氧化钛、氧化硅和其混合物或混合氧化物的载体材料之上的铂或钯或其混合物。
以特定方式将氧化活性催化涂层和在SCR反应中呈催化活性的涂层施加到适用于沉积柴油机粒子的过滤体上。适宜的过滤体选自陶瓷壁流式过滤器基材、烧结金属过滤体或者陶瓷或金属的泡沫结构。优选采用陶瓷壁流式过滤器基材,其具有开孔结构的壁,孔隙率为40~80%且平均孔直径为9~30微米。特别优选采用的陶瓷壁流式过滤器基材,其孔隙率为45~65%且平均孔直径为9~22微米。
将涂层施用到过滤体上时,一方面应注意,遵循针对所述反应机制而需要的层设置,从而使得待清洁的尾气首先经过在SCR反应中呈催化活性的涂层并随后经过氧化活性的催化涂层。此外,必须要给出尾气能够从氧化活性涂层经由SCR活性涂层扩散回到气体空间中的可能途径。另一方面,应当确保所获催化活化的柴油机粒子过滤器的背压性能基本不会恶化。这些要求的总和构成了在制备本发明的催化活化的柴油机粒子过滤器中的挑战。
不考虑所用过滤体的类型,首先将氧化活性的催化涂层(2)施加到作为支撑体的过滤体(3)上,且其占据该部件的全部长度。所得到的经氧化催化涂覆的过滤器随后作为用于在SCR反应中呈催化活性的涂层(1)的支撑体。由此,将SCR活性涂层施加到氧化活性涂层上。优选实施方式中,该SCR活性涂层仅占据该部件的一部分长度,且设置在流入侧,如图2中所示。尾气的流动方向如箭头所示。由于这种结构,待清洁的尾气,依据来自所设想的反应机理的要求,在其可以在氧化活性涂层之上转化之前,首先与SCR活性涂层进行接触。也确保了尾气经由SCR活性涂层扩散回到气体空间(两个层紧密接触是其先决条件)。另外,通过使SCR活性涂层缩减到部分的部件长度,
a)确保了该部件背压的最小化;和
b)确保了,对于催化涂布的柴油机粒子过滤器而言有利的性能,如在降低的烟灰点燃温度下的粒子燃尽、改进的被动再生性能以及抑制CO-和HC-排放物的渗透得以保持。
关于SCR活性涂层应占据该部件长度多少比例的问题,取决于待清洁的尾气的物料流速和其中含有的含氮有害气体的浓度。其的尺寸应当使得发生的氨渗透可以完全转化为氮气。在SCR反应中呈活性的催化涂层优选地占据该部件长度的5~50%,更优选10~30%。
在本发明优选的实施方式中,采用壁流式过滤器基材。为了使本发明催化活化的柴油机粒子过滤器的背压最小化,将氧化活性的催化涂层在部件的整个长度上引入到陶瓷壁流式过滤器基材的壁孔之中,使得其均匀分布在该壁流式过滤器基材的各个壁中。例如本申请人的DE 10 2004 040 548 A1中描述了如何进行这种涂布。
图3和4显示了催化活化的壁流式过滤器基材中特别优选的涂层结构,其是每种情形中具有流入通道(4)和流出通道(5)的结构截面的形式。尾气的流动方向如箭头所示。通过具有开孔结构的、用于渗透尾气的壁(3a)将流入和流出通道彼此分开,并通过气密性通道盖板(Kanalabschluβ)(3b)分别向着流出或流入侧密封。
在要将包含氧化活性涂层的传统壁流式过滤器基材扩展到氨阻滞功能且同时不丧失其现有性能时,优选地选择图3中所示的本发明催化活化的柴油机粒子过滤器的实施方式。这种传统的催化活化的壁流式过滤器基材并不罕见地具有在部件的整个长度之上均匀分布在壁中的氧化活性涂层,且其填充孔隙直到流入侧表面。为了产生氨阻滞功能,在这种粒子过滤器上,在部件的部分长度上将在SCR反应中呈催化活性的涂层施加到流入侧上。优选地该SCR活性层设置在壁的流入侧表面上,且占据该部件的长度的5~50%,更优选为10~30%。
特别优选图4中所示的实施方式,情况是当本发明的催化活化的柴油机粒子过滤器用于尾气净化设备时,且所述设备一方面具有在流入侧上游连接的高活性氧化功能用以消除CO-和HC-渗透,另一方面存在对于尾气脱氮的增强需求,只要本发明的柴油机粒子过滤器通常在其中经受范围为100~250℃的尾气温度。这种实施方式中,氧化活性涂层和SCR活性涂层二者在该部件的整个长度上均匀分布于壁中,该SCR活性涂层填充孔隙直到该壁的流入侧表面,同时氧化活性涂层填充孔隙直到该壁的流出侧表面。这种设置同样满足由于设想的反应机理和所需的背压性能而存在的全部要求。由于在该部件的整个长度上的这种SCR活性涂层的设置,以此方式催化活化的柴油机粒子过滤器不仅显示出氨阻滞功能,而且还显示出完全的低温-SCR活性。
通过使用本发明的催化活化的柴油机粒子过滤器,能够显著简化用于从主要在贫燃条件下工作的内燃机的尾气中除去氮氧化物和粒子的传统尾气净化设备。图5示例地显示了现有技术的尾气设备,如WO99/39809中所述,在该方案中是双向流(zweiflutige)设备的形式。其中发动机(0)的每个汽缸组(Zylinderbank)上连接包含柴油机氧化催化剂(6,6′)的尾气设备部分。尾气管线汇合之后,在流动方向上依次设置任选催化活化的柴油机粒子过滤器(7)、用于SCR反应中所需的还原剂(8)(例如脲)的计量加料装置和SCR催化剂(9)。为了防止氨的渗透,需要下游连接的氨阻滞催化剂(10)。
本发明部件的使用能够减少这种尾气净化设备的基本组件。为了从主要在贫燃条件下工作的内燃机的尾气中除去氮氧化物和粒子,在相应设备包括适用于除去氮氧化物的催化剂和本发明的催化活化的柴油机粒子过滤器时,这是足够的。适用于除去氮氧化物的催化剂可以是设置在依据本发明的柴油机粒子过滤器(11)的流入侧上的氮氧化物储存催化剂(12,12′)。图6中示意地显示了对于双向流的设备构造情形时的一种这样的实施方式。
在本发明尾气净化设备的优选形式中,作为适用于脱氮的催化剂采用连有计量添加氨或者可分解为氨的化合物的装置(8)的SCR催化剂(9),其同样位于本发明柴油机粒子过滤器(11)的流入侧上。图7中示意地显示了对于双向流的设备构造情形时的一种这样的实施方式。此时,当在尾气清洁设备中将柴油机氧化催化剂(6,6′)或三效催化剂(13,13′)或氮氧化物储存催化剂(12,12′)或其组合设置在主要在贫燃条件下工作的内燃机(0)与用于计量添加氨或可分解为氨的化合物的装置(8)之间时,这对于一些机动车类型中的应用而言是有利的。
附图说明
以下附图和实施例旨在详细地阐述本发明。
图1:本发明柴油机粒子过滤器在含氮有害气体的转化中的作用原理。
图2:本发明催化活化的柴油机粒子过滤器中SCR活性涂层(1)和氧化活性涂层(2)在作为支撑体的过滤体(3)上的结构设置。
图3:本发明催化活化的柴油机粒子过滤器中SCR活性涂层(1)的优选结构设置,其中氧化活性的催化涂层(2)均匀分布在壁流式过滤器基材的壁(3a)中,且与流入通道(4)直接接触;(5)表示流出通道,(3b)分别表示为气密性的通道盖板。
图4:本发明催化活化的壁流式过滤器基材中涂层的优选结构设置,其中两个涂层均匀分布在壁(3a)中,SCR活性涂层(1)填充壁(3a)并朝向流入通道(4),同时氧化活性涂层(2)填充壁(3a)并朝向流出通道(5);(3b)表示分别为气密性的通道盖板。
图5:依据现有技术的双向流方式的、用于从主要在贫燃条件下工作的内燃机(0)的尾气中除去氮氧化物和粒子的尾气净化设备,其包括柴油机氧化催化剂(6,6′)、任选催化活化的柴油机粒子过滤器(7)、用于SCR反应中所需的还原剂(例如脲)的计量添加装置(8)、SCR催化剂(9)和下游的氨阻滞催化剂(10)。
图6:双向流方式的、用于从主要在贫燃条件下工作的内燃机(0)的尾气中除去氮氧化物和粒子的本发明的尾气净化设备,其包括本发明的催化活化的柴油机粒子过滤器(11)和在流入侧上的氮氧化物储存催化剂(12,12′)。
图7:双向流方式的、用于从主要在贫燃条件下工作的内燃机(0)的尾气中除去氮氧化物和粒子的本发明的尾气净化设备,其包括本发明的催化活化的柴油机粒子过滤器(11)和在流入侧上的、连有用于计量添加氨或可分解为氨的化合物的装置(8)的SCR催化剂(9)。任选地,柴油机氧化催化剂(6,6′)和/或氮氧化物储存催化剂(12,12′)或/和三效催化剂(13,13′)可以设置在发动机(0)与计量加料装置(8)之间。
图8:氨氧化方面的活性,在设置有氧化活性涂层的现有技术的壁流式过滤器基材上([#0];◇)、以及在具有氧化活性涂层和SCR活性涂层的两个本发明的催化活化的柴油机粒子过滤器上测得。本发明的柴油机粒子过滤器[#1](●)在SCR活性涂层中包含与铁交换过的沸石,本发明的柴油机粒子过滤器[#2](▲)则包含与铜交换过的沸石。
图9:氨氧化中对于氮气的选择性,在设置有氧化活性涂层的现有技术的壁流式过滤器基材上([#0];◇)、以及在具有氧化活性涂层和SCR活性涂层的两个本发明的催化活化的柴油机粒子过滤器上测得。本发明的柴油机粒子过滤器[#1](●)在SCR活性涂层中包含与铁交换过的沸石,本发明的柴油机粒子过滤器[#2](▲)则包含与铜交换过的沸石。
具体实施方式
下述实施例中,制备了本发明催化活化的柴油机粒子过滤器的各种实施方式。与对比实施例中制得的传统柴油机粒子过滤器相对比,在模型气体试验台上研究它们在氨氧化中的反应性和选择性。在此选择如下试验条件:
借助于适宜的气体分析设备,在催化剂下游获得氨、一氧化二氮、一氧化氮和二氧化氮的浓度。在合理的假设下,即假设除了这些含氮的气体和分子氮之外,氨氧化过程之中无其它含氮反应产物形成,由如下平衡式可以确定反应目标产物N2的浓度:
由如此获得的氮气浓度和计量添加的氨浓度如下计算对氮气的选择性:
为了评价测量结果,将催化剂下游的氨浓度和对于氮气的选择性作为温度的函数作图,结果示于图8和9中。
对比实施例:
在由碳化硅构成的壁流式过滤器基材上设置借助于DE 10 2004040 548 A1中所述工作方式而引入到壁中去的传统的氧化活性涂层。
该过滤器基材的直径为14.4厘米且长度为7.62厘米,并具有47个腔孔/平方厘米且壁厚为0.3毫米。该过滤器基材的壁具有平均直径为20微米的孔隙,该壁的孔隙率为60%。
氧化活性涂层基本上包括铂,其负载在掺杂有氧化镧的高表面积氧化铝之上。选择施加的涂层数量,使得制成的柴油机粒子过滤器含有0.7g/L贵金属,基于经涂布的过滤器基材的体积计。
从制成的柴油机粒子过滤器中取出三个直径为2.54厘米的钻芯。在模型气体设备中,通过上述方法在这些钻芯的一个[#0]上研究特有的氨氧化性能。
实施例1:
在从对比实施例的柴油机粒子过滤器中取出的第二个钻芯上,将在SCR反应中呈活性的且主要包含与铁交换过的沸石的涂层施加到流入侧上。涂布区的长度为2.54厘米,即整个部件长度的33%。施加50g/L的SCR活性材料,基于过滤器基材的体积计。
根据上述方法在模型气体设备中研究由此获得的本发明催化活化的柴油机粒子过滤器[#1]特有的氨氧化性能。
实施例2:
在从对比实施例的柴油机粒子过滤器中取出的第三个钻芯上,将在SCR反应中呈活性的且主要包含与铜交换过的沸石的涂层施加到流入侧上。涂布区的长度为2.54厘米,即整个部件长度的33%。施加50g/L的SCR活性材料,基于过滤器基材的体积计。
也根据上述方法在模型气体设备中研究本发明的催化活化的柴油机粒子过滤器[#2]特有的氨氧化性能。
图8和9显示了模型气体中的研究结果。
图8中,将催化剂下游的氨浓度作为反应温度的函数作图。该数据作为氨氧化中被研究的柴油机粒子过滤器的一般活性的度量。显然,本发明柴油机粒子过滤器在其一般的氨氧化活性方面与传统的柴油机粒子过滤器无明显差异:高于250℃下,氨完全氧化。
在氨氧化反应对于氮气的选择性方面,本发明的催化活化的柴油机粒子过滤器显示出显著的优点。在传统的柴油机粒子过滤器(◇)的情形下在高于300℃时这点丧失,因为氨完全过氧化为氮氧化物(主要为NO2),而本发明的柴油机粒子过滤器在整个温度范围内显示杰出的选择性数据。对于具有含铜的SCR活性涂层的柴油机粒子过滤器[#2](▲)的情况,观察到有着大于70%的最佳选择性数值的结果,但是具有含铁的SCR活性涂层的本发明柴油机粒子过滤器[#1](●)在250~550℃的温度范围内也显示大于30%的良好的选择性数值。
本发明的具有氨阻滞功能的催化活化的柴油机粒子过滤器由此非常适合用于尾气设备中,该设备用于同时除去含氮的有害气体和粒子,且现在可以采用所述的方式依据本发明使其简化。
Claims (20)
1.一种催化活化的柴油机粒子过滤器,其包括过滤体,和氧化活性的催化涂层,以及在SCR反应中呈催化活性的另一涂层,其中含有氨储存材料,其特征在于,保持层的设置,使得待清洁的尾气首先经过在SCR反应中呈催化活性的涂层和随后经过氧化活性的催化涂层。
2.权利要求1的催化活化的柴油机粒子过滤器,其特征在于,在SCR反应中呈催化活性的涂层的氨储存能力是至少20毫升/克催化剂材料。
3.权利要求2的催化活化的柴油机粒子过滤器,其特征在于,在SCR反应中呈催化活性的涂层含有一种或多种已与氢阳离子或过渡金属阳离子进行过交换的沸石。
4.权利要求3的催化活化的柴油机粒子过滤器,其特征在于,在SCR反应中呈催化活性的涂层含有一种或多种与铁或铜或铁和铜交换过的沸石。
5.权利要求3的催化活化的柴油机粒子过滤器,其特征在于,在SCR反应中呈催化活性的涂层含有β-沸石或Y-沸石或八面沸石或丝光沸石或ZSM-5或其组合。
6.权利要求3的催化活化的柴油机粒子过滤器,其特征在于,在SCR反应中呈催化活性的涂层不含贵金属。
7.权利要求1的催化活化的柴油机粒子过滤器,其特征在于,该氧化活性的催化涂层不含沸石。
8.权利要求7的催化活化的柴油机粒子过滤器,其特征在于,该氧化活性的催化涂层含有在选自高表面积的活性氧化铝、氧化铈、氧化锆、氧化钛、氧化硅、其混合物或其混合氧化物的载体材料之上的铂或钯或其混合物。
9.权利要求1的催化活化的柴油机粒子过滤器,其特征在于,该过滤体选自陶瓷壁流式过滤器基材、烧结金属过滤体或者陶瓷或金属泡沫结构。
10.权利要求9的催化活化的柴油机粒子过滤器,其特征在于,该过滤体选自陶瓷壁流式过滤器基材,且具有有开孔结构的壁,其孔隙率为40~80%且平均孔直径为9~30微米。
11.权利要求1的催化活化的柴油机粒子过滤器,其特征在于,该过滤体用作氧化活性的催化涂层用的支撑体,其中所述涂层占据部件的整个长度,且其特征在于,将设置有氧化活性的催化涂层的过滤器基材用作在SCR反应中呈催化活性的涂层用的支撑体。
12.权利要求11的催化活化的柴油机粒子过滤器,其特征在于,在SCR反应中呈催化活性的涂层占据部件长度的5~50%,且设置在该部件的流入侧之上。
13.权利要求10的催化活化的柴油机粒子过滤器,其特征在于,将氧化活性的催化涂层在部件的整个长度上引入到陶瓷壁流式过滤器基材的壁的孔隙之中,并均匀分布在该壁流式过滤器基材的各个壁中。
14.权利要求13的催化活化的柴油机粒子过滤器,其特征在于,将该氧化活性的催化涂层填充陶瓷壁流式过滤器基材的壁中孔隙,直到各个壁的流入侧表面,且将在SCR反应中呈催化活性的涂层施加到这个表面上。
15.权利要求14的催化活化的柴油机粒子过滤器,其特征在于,在SCR反应中呈活性的催化涂层占据部件长度的5~50%,且设置在整个部件的流入侧上。
16.权利要求13的催化活化的柴油机粒子过滤器,其特征在于,该氧化活性的催化涂层填充陶瓷壁流式过滤器基材的壁中孔隙,直到各个壁的流出侧表面,且同样将在SCR反应中呈催化活性的涂层引入壁的孔隙之中并均匀分布在各个壁中,但是填充孔隙直到各个壁的流入侧表面。
17.一种用于从主要在贫燃条件下工作的内燃机的尾气中除去氮氧化物和粒子的尾气净化设备,其特征在于,该尾气净化设备含有适用于除去氮氧化物的催化剂,和依据权利要求1~16中任一项的催化活化的柴油机粒子过滤器。
18.权利要求17的尾气净化设备,其特征在于,该尾气净化设备在催化活化的柴油机粒子过滤器的流入侧上包括,用于计量添加氨或可分解为氨的化合物的装置以及SCR催化剂。
19.权利要求18的尾气净化设备,其特征在于,在主要在贫燃条件下工作的内燃机和用于计量添加氨或可分解为氨的化合物的装置之间设置柴油机氧化催化剂或三效催化剂或氮氧化物储存催化剂或其组合。
20.权利要求17的尾气净化设备,其特征在于,该尾气净化设备在催化活化的柴油机粒子过滤器的流入侧上包括氮氧化物储存催化剂。
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BRPI0807632A2 (pt) | 2014-06-03 |
RU2009135272A (ru) | 2011-03-27 |
US8226896B2 (en) | 2012-07-24 |
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JP2010519020A (ja) | 2010-06-03 |
ATE464458T1 (de) | 2010-04-15 |
EP1961933A1 (de) | 2008-08-27 |
DE502007003465D1 (de) | 2010-05-27 |
EP1961933B1 (de) | 2010-04-14 |
RU2449135C2 (ru) | 2012-04-27 |
US20100058746A1 (en) | 2010-03-11 |
KR101247550B1 (ko) | 2013-03-26 |
CN101605968A (zh) | 2009-12-16 |
BRPI0807632B1 (pt) | 2018-12-04 |
WO2008101585A1 (de) | 2008-08-28 |
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