CN107008261A - NOx吸收催化剂 - Google Patents
NOx吸收催化剂 Download PDFInfo
- Publication number
- CN107008261A CN107008261A CN201610922055.7A CN201610922055A CN107008261A CN 107008261 A CN107008261 A CN 107008261A CN 201610922055 A CN201610922055 A CN 201610922055A CN 107008261 A CN107008261 A CN 107008261A
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- Prior art keywords
- metal
- extrusion
- weight
- solid
- oxide
- Prior art date
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- 239000007787 solid Substances 0.000 claims abstract description 107
- 238000001125 extrusion Methods 0.000 claims abstract description 93
- 229910052751 metal Inorganic materials 0.000 claims abstract description 88
- 239000002184 metal Substances 0.000 claims abstract description 88
- 239000000203 mixture Substances 0.000 claims abstract 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 abstract description 69
- 239000010457 zeolite Substances 0.000 claims abstract description 66
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- 238000000576 coating method Methods 0.000 claims abstract description 37
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 claims abstract description 31
- 229910052783 alkali metal Inorganic materials 0.000 claims abstract description 26
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 claims abstract description 26
- 150000001340 alkali metals Chemical class 0.000 claims abstract description 25
- 229910052784 alkaline earth metal Inorganic materials 0.000 claims abstract description 22
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- 239000000853 adhesive Substances 0.000 claims abstract description 19
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- 229910000510 noble metal Inorganic materials 0.000 claims abstract description 13
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 54
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims description 37
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 37
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 37
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 33
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- GEYXPJBPASPPLI-UHFFFAOYSA-N manganese(III) oxide Inorganic materials O=[Mn]O[Mn]=O GEYXPJBPASPPLI-UHFFFAOYSA-N 0.000 claims description 2
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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 description 13
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Abstract
包含挤出固体的NOx吸收催化剂包含:(A)10‑100重量%的至少一种粘合剂/基质组分;和5‑90重量%的沸石分子筛、非沸石分子筛或它们的任何两种或更多种的混合物,所述催化剂包含以下的至少一种金属:(a)至少一种贵金属;和(b)至少一种碱金属或至少一种碱土金属,其中(a)和(b)携带于挤出固体表面上的一个或多个涂层;或者(B)10‑100重量%的至少一种粘合剂/基质组分;和5‑80重量%的任选稳定的二氧化铈,所述催化剂包含以下的至少一种金属:(a)至少一种贵金属;和(b)至少一种碱金属或至少一种碱土金属。
Description
本申请是申请日为2011年2月1日,申请号为201180017655.4,名称为“NOx吸收催化剂”的发明专利申请的分案申请。
本发明涉及包含挤出固体的催化剂,用于处理来自固定源且特别是移动应用(即机动车辆)的内燃机的废气排放物中包含的氮氧化物。
US2002/0077247公开了蜂窝状的NOx储存催化剂,其中所述蜂窝由至少一种碱土金属硫酸盐(作为NOx储存材料的前体化合物)形成。所述催化剂一般含有过渡金属,优选选自以下的金属:钯、铂、铑、铱和钌,所述金属可通过溶胶浸渍或通过浸入盐溶液中而引入。
汽车工程师学会(SAE)技术文献2007-01-0658题为"Fundamental Study andPossible Application of New Concept Honeycomb Substrate for Emission Control(用于排放控制的新概念蜂窝基底的基础研究和可能应用)",公开了包含分散于催化载体上的铂催化剂的柴油氧化催化剂(DOC),所述催化载体包含γ-氧化铝、无机纤维和(未命名的)粘合材料的多个挤出片段,它们粘合成全尺寸块体。所述铂通过普通浸渍法以1.0-2.7g/l施用于催化载体。所述文献建议也可用相同的方式制造NOx储存催化剂(NSC),不过没有提供具体实施例。
EP1739066公开了包含以下的蜂窝结构:具有多重通孔的多重蜂窝单元;和通过蜂窝单元的各个闭合外表面将蜂窝单元彼此连接的密封层,其中所述通孔不开口。所述蜂窝单元至少包括无机颗粒、无机纤维和/或晶须(whisker)。例证的无机颗粒为氧化铝、二氧化钛、二氧化硅和二氧化锆;例证的无机纤维为二氧化硅-氧化铝纤维;且例证的无机粘合剂为二氧化硅溶胶、氧化铝溶胶、海泡石和绿坡缕石。催化剂组分可携带于所述蜂窝结构上。所述催化剂组分可包括选自贵金属(包括铂、钯和铑)、碱金属(比如钾和钠)、碱土金属(例如钡)和氧化物的至少一种类型。所述蜂窝结构可用作催化转化器(例如三效催化剂)或NOx储存催化剂,用于转化车辆的废气。
WO2009/093071公开了孔隙率为至少40%、由挤出型选择性催化还原催化剂形成的壁流式过滤器整料基底。
我们现已开发了包含挤出固体和至少一种金属的催化剂系列,所述催化剂在内燃机废气的废气后处理领域中具有特定的应用。这种废气可由固定源排放物产生,但是开发所述催化剂特别用于处理移动排放源,比如客车、卡车和公共汽车。
根据一方面,本发明提供包含挤出固体的NOx吸收催化剂,其包含:(A) 10-100重量%的至少一种粘合剂/基质组分;和5-90重量%的沸石分子筛、非沸石分子筛或它们的任何两种或更多种的混合物,所述催化剂包含以下的至少一种金属:(a) 至少一种贵金属;和(b) 至少一种碱金属或至少一种碱土金属,其中(a)和(b)携带于挤出固体表面上的一个或多个涂层;或者(B) 10-100重量%的至少一种粘合剂/基质组分;和5-80重量%的任选稳定的二氧化铈,所述催化剂包含以下的至少一种金属:(a) 至少一种贵金属;和(b) 至少一种碱金属或至少一种碱土金属,其中:
(i) 所述至少一种碱金属或至少一种碱土金属存在于整个挤出固体中;
(ii) 大部分的所述至少一种碱金属或至少一种碱土金属位于挤出固体的表面;
(iii) 所述至少一种碱金属或至少一种碱土金属携带于挤出固体表面上的一个或多个涂层:
(iv) 所述至少一种碱金属或至少一种碱土金属存在于整个挤出固体且在挤出固体的表面也以较高的浓度存在;
(v) 所述至少一种碱金属或至少一种碱土金属存在于整个挤出固体且也携带于挤出固体表面上的一个或多个涂层;或
(vi) 所述至少一种碱金属或至少一种碱土金属存在于整个挤出固体,在挤出固体的表面以较高的浓度存在且也携带于挤出固体表面上的一个或多个涂层。
将本发明分成实施方案(A)和(B)的原因是沸石分子筛和非沸石分子筛一般为酸性性质(例如取决于程序升温脱附)。但是,从废气中吸收氮氧化物的过程一般涉及将一氧化氮氧化成二氧化氮(其为温和酸性),和将二氧化氮吸收在碱性金属化合物(比如铈化合物)、碱金属化合物或碱土金属化合物上。于是,如果所述沸石分子筛或非沸石分子筛与碱性金属化合物结合,则降低了碱性金属化合物吸收氮氧化物的能力。
但是,沸石分子筛和/或非沸石分子筛的存在可为有利的,原因在于其可通过在低于贵金属组分催化烃氧化成二氧化碳和水的温度下吸附冷启动烃来促进所谓的"冷启动"烃转化,并当贵金属催化剂的温度升高至超过其用于氧化烃的"点火"温度时促进烃脱附。已知,某些结合金属可有助于HC吸附,具有用于本发明的优势。优选的吸附促进金属包括Pd和/或Cu、Ag、碱土金属和碱金属(例如Cs)。但是,对于后者情况,所述碱金属和碱土金属旨在促进烃吸附而非NOx吸收。
因此,在其中期望通过将沸石和/或非沸石分子筛包括在挤出固体内和/或一个或多个涂层中来促进冷启动烃吸附的实施方案中,将实施方案(A)和(B)设计成实质上防止旨在用于NOx吸附的碱金属化合物、碱土金属化合物或铈化合物接触所述沸石和/或非沸石分子筛。由于这个原因,在实施方案(A)中,碱金属化合物、铈化合物和/或碱土金属化合物存在于一个或多个涂层中。(B)的实施方案可包括包含沸石和/或非沸石分子筛的涂层。但是,在这些实施方案中,所述沸石和/或非沸石分子筛存在于与碱金属化合物、铈化合物和/或碱土金属化合物分离的离散层中。
本发明的一个优势是通过除去常用于催化涂层中的催化组分,可以减少涂层的数目,例如从两层减少到一层;或可以一起除去单层且催化金属可以负载在挤出固体本身的表面上。这有利于降低排气系统中的背压,提高发动机的效率。
此外,通过提供无涂层的催化剂的可能性,挤出固体可以较高的胞孔密度制造,增强了强度且降低了胞孔壁的厚度(其可改善点火性能)并提高了通过传质的活性。
相对于惰性基底整料上的涂层,也可以增加活性组分在挤出固体中的量。这种增大的催化剂密度具有长期稳定性和催化剂性能的优势,其对于车载诊断是重要的。
在机动车背景中的“车载诊断”(OBD)是通用术语,用于描述自我诊断并报告由连接于合适的电子管理系统的传感器网络提供的车辆系统的能力。如果检测到问题,OBD系统的早期实例仅仅会点亮故障指示灯,但是关于问题的本质则不提供信息。更现代的OBD系统使用标准化的数字接口且能够提供关于标准化的诊断故障代码和选择实时数据的信息,其允许车辆系统的快速问题识别和解决。
现在的OBD要件要求在排放系统的故障或劣化会导致排放物超过强制性阈值的情况下必须通知驾驶员。因此,例如,Euro 4:98/69/EC对于柴油客车(如70/156/EEC所定义的M类车辆)的OBD限制是:一氧化碳(CO)-3.2g/km;烃(HC)-0.4 g/km;氮氧化物(NOx)-1.2 g/km;和微粒物质(PM)0.18 g/km。对于汽油客车,Euro4限制是:CO-3.2 g/km;HC-0.4 g/km;NOx-0.6 g/km;和PM-无限制。
未来的车辆排放物法规(尤其在美国和欧洲)在诊断功能方面要求更高的敏感性,以便连续监视排气系统后处理催化剂的能力以符合排放物法规。例如,目前草拟的Euro 5:715/2007/EC对于压缩点火(柴油)客车的OBD限制是:CO-1.9 g/km;非甲烷系烃(NMHC)-0.25 g/km;NOx-0.54 g/km;PM-0.05 g/km;且对于主动点火(汽油)客车:CO-1.9 g/km;NMHC-0.25 g/km;NOx-0.54 g/km;和PM-无限制。
在美国,很清楚用于汽油/火花点火发动机的催化剂监视的OBD II法规(Title13, California Code Regulations, Section 1968.2, Malfunction and DiagnosticSystem Requirements for 2004 and Subsequent Model-Year Passenger Cars, Light-Duty Trucks and Medium-Duty Vehicles and Engines(标题13,加州法规编码,1968.2章,2004及以后的型号-年客车、轻型卡车和中型车辆和发动机的故障及诊断系统要求))要求,在一般联邦测试程序(FTP)对催化剂系统的被监视部分的NMHC转换效率的测试中,故障信号低于50%。
根据本发明的挤出固体一般包含蜂窝状的整体式结构,所述蜂窝具有从其第一端延伸至第二端的尺寸均匀且平行的通道。一般地,所述通道在第一和第二端都开口-所谓的"流通式"结构。限定通道的通道壁多孔。一般地,外部"表皮"包围了挤出固体的多个通道。挤出固体可由任何期望的截面形成,比如圆形、正方形或椭圆形。多个通道中的单个通道可为正方形、三角形、六边形、圆形等。可(例如用合适的陶瓷水泥)阻塞通道的第一上游端,且第一上游端未阻塞的通道也可在第二下游端阻塞来形成所谓的壁流式过滤器。一般,第一上游端阻塞的通道的排列类似于具有阻塞和开口的下游通道端的相似排列的跳棋盘。
显然,EP 1739066中公开的蜂窝结构的热震参数(TSP)太低而不能用于单一整体式挤出物,因为所述蜂窝结构包含单个蜂窝单元接合在一起的组合件。设计这种排列(也见于市售可得的碳化硅蜂窝)是为了避免催化剂基底致命失效,尤其由于挤出材料的相对高的热膨胀系数(CTE)导致的热震。但是,和单块挤出物相比,由单个蜂窝单元制造蜂窝结构复杂、费力、费时且昂贵并增大了可能的物理失效方式的数目。TSP和CTE更完整的解释可见于“Catalytic Air Pollution Control-Commercial Technology(催化空气污染控制-商业技术)”,第二版,R.M. Heck等人,John Wiley & Sons, Inc., New York, 2002,第7章(有关流通式整料)和第9章(关于壁流式过滤器)。
因此,我们优选根据本发明的催化剂的挤出固体当用于处理来自固定或移动排放源的废气时具有足以避免挤出固体中径向裂缝和环裂缝的轴向热震参数(TSP)和径向TSP。这样,挤出固体可由单一整体式挤出物形成。对于截面特别大的挤出固体,可能仍需要将挤出固体的片段挤出,用于接合在一起。但是,这是由于处理如此大截面的挤出物的困难或由于挤出物模具的尺寸限制。但是,单独考虑,整体催化剂的各个片段会满足功能限制,即当用于处理来自固定或移动排放源的废气时,轴向TSP和径向TSP足以避免单个挤出固体片段中的径向裂缝和环裂缝。在一个实施方案中,在750℃下径向TSP>0.4,比如>0.5、>0.6、>0.7、>0.8、>0.9或>1.0。在800℃下,期望径向TSP也>0.4且在1000℃下优选>0.8。
壁流式过滤器的CTE优选为20 x 10-7/℃,以便由单块挤出物形成。
在一个实施方案中,(A)或(B)中的至少一种贵金属负载于挤出固体表面上的一个或多个涂层中,其中所述或各个(the or each)涂层包含一种或多种任选稳定的氧化铝、二氧化硅、二氧化钛、任选稳定的二氧化铈、任选稳定的二氧化锆、氧化钒、氧化镧、尖晶石和它们的任何两种或更多种的混合物。在实施方案(B)的替代实施方案(ii)、(iv)和(vi)中,所述至少一种贵金属(例如Pt和/或Pd)被浸渍在挤出固体上。
在包含两个或更多个涂层的(A)或(B)的特定实施方案中,第一底层包含任选稳定的二氧化铈和尖晶石的混合物。优选地,所述第一底层包含Pt和/或Pd。在优选的实施方案中,第二层放置成覆盖第一底层,所述第二层包含负载于氧化铝和任选稳定的二氧化锆的一种或多种上的铑。在另一实施方案中,第三层放置成覆盖第二层,所述第三层包含负载于块体可还原氧化物上的沸石或铂和/或钯,所述可还原氧化物实质上不含碱金属和碱土金属。
在包含一个或多个涂层的(B)的替代实施方案中,铂和/或钯位于挤出固体的表面且第一底层包含负载于氧化铝和任选稳定的二氧化锆的一种或多种上的铑。在特定的实施方案中,覆盖第二层的第二层包含负载于块体可还原氧化物上的沸石或铂和/或钯,所述可还原氧化物实质上不含碱金属和碱土金属。
包含含有负载于块体可还原氧化物(其实质上不含碱金属和碱土金属)上的铂或铂和钯两者的层的实施方案特别可用于处理存在于柴油发动机废气中的一氧化碳和未燃烃。一般地,NOx吸收催化剂隐含地限定,结合NOx吸收催化剂使用的发动机配置成运作贫化学计量空气/燃料燃烧比,用于吸收氮氧化物并间歇地运行富化学计量空气/燃料燃烧比以便使吸收的NOx脱附并使NOx还原成N2。已非常意外地发现,通过使包含铂或铂和钯两者和可还原氧化物的氧化催化剂与富废气间歇地且瞬间地接触,氧化催化剂可恢复当铂在较高的温度下被氧化时损失的氧化活性。当氧化后,Pt组分对于CO和HC氧化的活性更小。存在的碱土金属或碱金属与Pt接触毒害了Pt氧化CO和HC的活性。
所述块体可还原氧化物可选自氧化物、复合氧化物和混合氧化物,它们包含选自以下的一种或多种金属:锰、铁、锡、铜、钴或铈和它们的任选稳定的类似物(但是优选基于铈)。因此,例如所述至少一种可还原氧化物可包含MnO2、Mn2O3、Fe2O3、SnO2、CuO、CoO和CeO2。
CeO2的稳定的类似物可包含二氧化锆、至少一种非铈稀土氧化物或二氧化锆和至少一种非铈稀土氧化物两者。
在优选的实施方案中,第一金属氧化物载体基本上由块体至少一种可还原氧化物或其任选稳定的类似物组成。或者,所述至少一种可还原氧化物或其任选稳定的类似物可负载于具有铂的第一金属氧化物载体上。
在实施方案中,所述至少一种粘合剂/基质组分可选自:堇青石、氮化物、碳化物、硼化物、金属间化合物、铝硅酸锂、尖晶石、任选掺杂的氧化铝、二氧化硅源、二氧化钛、二氧化锆、二氧化钛-二氧化锆、锆石和它们的任何两种或更多种的混合物。
尖晶石可为MgAl2O4或Mg可用选自以下的金属部分替换:Co、Zr、Zn或Mn。其中挤出固体包含尖晶石的催化剂的测试正在进行中,但是初步迹象是MgAl2O4基组分可对本发明的NOx捕集实施方案(NOx捕集器有时也称为NOx储存/还原(NSR)催化剂、DeNOx捕集器(DNT)、贫NOx捕集器(LNT)、NOx吸收催化剂(NAC)、NOx消除催化剂和NOx储存催化剂(NSC)提供特定活性益处。在这种NOx捕集实施方案中,MgAl2O4中MgO的含量相对于Al2O3可为0.8-2.5,优选<1.0的值。
所述氧化铝粘合剂/基质组分优选为γ氧化铝,但是可为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氧化铝和这些过渡型氧化铝的任何两种或更多种的混合物。
优选所述氧化铝掺有至少一种非铝元素来增强氧化铝的热稳定性。合适的氧化铝掺杂剂包括硅、锆、钡、镧系元素和它们的任何两种或更多种的混合物。合适的镧系元素掺杂剂包括La、Ce、Nd、Pr、Gd和它们的任何两种或更多种的混合物。
二氧化硅源可包括:二氧化硅、二氧化硅溶胶、石英、熔融或无定形二氧化硅、硅酸钠、无定形铝硅酸盐、烷氧基硅烷、硅酮树脂粘合剂(比如甲基苯基硅酮树脂)、粘土、滑石或它们的任何两种或更多种的混合物。
此列表中二氧化硅可为SiO2本身、长石、莫来石、二氧化硅-氧化铝、二氧化硅-氧化镁、二氧化硅-二氧化锆、二氧化硅-氧化钍、二氧化硅-氧化铍、二氧化硅-二氧化钛、三元二氧化硅-氧化铝-二氧化锆、三元二氧化硅-氧化铝-氧化镁、三元-二氧化硅-氧化镁-二氧化锆、三元二氧化硅-氧化铝-氧化钍和它们的任何两种或更多种的混合物。或者,二氧化硅可来源于焙烧加入挤出组合物的四甲基原硅酸盐(TMOS)。
合适的粘土包括漂白土、海泡石、锂蒙脱石、蒙脱石、高岭土和它们的任何两种或更多种的混合物,其中高岭土可选自:次膨润土、蠕陶土、埃洛石、高岭石、地开石、珍珠陶土和它们的任何两种或更多种的混合物;所述蒙脱石可选自:蒙脱土、绿脱石、蛭石、皂石和它们的任何两种或更多种的混合物;且所述漂白土可为蒙脱土或绿坡缕石(硅镁土)。
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、二氧化硅纤维、二氧化硅-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。
用于本发明的合适的分子筛是在汽车发动机冷起动之后能够吸附未燃烃并在高于环境温度下(例如当结合的贵金属基氧化催化剂组分已达到用于例如CO和HC氧化或NOx还原的期望的点火温度时)使被吸附的烃脱附的那些。这样的分子筛一般并不是具有8环孔开口结构作为其最大孔开口结构(有时称作小孔分子筛)的那些。优选的分子筛是中孔(最大10-环孔开口结构)、大孔(最大12-环孔开口结构)或甚至(oven)介孔(>12-环孔开口结构)分子筛。
所述或各个沸石分子筛或所述或各个非沸石分子筛可选自如国际沸石协会结构委员会(Structure Commission of the International Zeolite Association)所定义的以下代码的骨架类型:ABW、ACO、AEI、AEL、AEN、AET、AFG、AFI、AFN、AFO、AFR、AFS、AFT、AFX、AFY、AHT、ANA、APC、APD、AST、ASV、ATN、ATO、ATS、ATT、ATV、AWO、AWW、BCT、BEA、BEC、BIK、BOF、BOG、BPH、BRE、BSV、CAN、CAS、CDO、CFI、CGF、CGS、CHA、-CHI、-CLO、CON、CZP、DAC、DDR、DFO、DFT、DOH、DON、EAB、EDI、EMT、EON、EPI、ERI、ESV、ETR、EUO、EZT、FAR、FAU、FER、FRA、GIS、GIU、GME、GON、GOO、HEU、IFR、IHW、IMF、ISV、ITE、ITH、ITR、ITW、IWR、IWS、IWV、IWW、JBW、JRY、KFI、LAU、LEV、LIO、-LIT、LOS、LOV、LTA、LTF、LTL、LTN、MAR、MAZ、MEI、MEL、MEP、MER、MFI、MFS、MON、MOR、MOZ、MRE、MSE、MSO、MTF、MTN、MTT、MTW、MWW、NAB、NAT、NES、NON、NPO、NSI、OBW、OFF、OSI、OSO、OWE、-PAR、PAU、PHI、PON、RHO、-RON、RRO、RSN、RTE、RTH、RUT、RWR、RWY、SAO、SAS、SAT、SAV、SBE、SBN、SBS、SBT、SFE、SFF、SFG、SFH、SFN、SFO、SFS、SGT、SIV、SOD、SOF、SOS、SSF、SSY、STF、STI、STO、STT、STW、-SVR、SZR、TER、THO、TOL、TON、TSC、TUN、UEI、UFI、UOS、UOZ、USI、UTL、VET、VFI、VNI、VSV、WEI、-WEN、YUG、ZON和它们的任何两种或更多种的混合物。
优选的沸石和非沸石分子筛选自BEA、FAU、FER、MFI、MFS、MOR、STI、SZR和它们的任何两种或更多种的混合物。
特别优选的沸石或非沸石分子筛选自BEA、FER、MFI、STI和它们的任何两种或更多种的混合物。特别优选的沸石分子筛是ZSM-5、β、镁碱沸石和它们的任何两种或更多种的混合物。
虽然天然沸石分子筛可用于本发明,但是我们优选二氧化硅比氧化铝比率为10或更大,例如15-150、20-60或25-40的合成铝硅酸盐沸石分子筛,用于改善热稳定性。
在替代实施方案中,所述沸石分子筛或非沸石分子筛是含有一种或多种取代骨架金属的同形体。在此实施方案中,所述或各个取代骨架金属可选自As、B、Be、Ce、Co、Cu、Fe、Ga、Ge、Li、Mg、Mn、Zn和Zr;Ce、Cu和Fe。同样,优选的同形的沸石或非沸石分子筛可选自BEA、FER、MFI、STI和它们的任何两种或更多种的混合物,特别优选其骨架中包括Fe的BEA。应理解,制造这些含有一种或多种取代骨架金属的同形体的过程中,所述或各种金属可单独在骨架中或者在骨架中且被离子交换而存在于最终产品。
含有一种或多种取代骨架金属的同形体中的二氧化硅比氧化铝比率可为>25,比如30-100或40-70。相比之下,同形体的二氧化硅比骨架金属比率可为>20,比如30-200或50-100。
在优选的实施方案中,所述非沸石分子筛是铝磷酸盐,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)。优选的非沸石分子筛包括SAPO-18、SAPO-34、SAPO-44和SAPO-47。
铝磷酸盐的二氧化硅比氧化铝比率一般比共有相同骨架类型代码的铝硅酸盐沸石低得多。一般地,铝磷酸盐的二氧化硅比氧化铝比率为<1.0,但是可<0.5或甚至<0.3。
所述二氧化铈组分可用至少一种非铈元素任选稳定,来增强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更多种的混合物。镧系元素稳定剂包括La、Nd、Pr、Gd和它们的任何两种或更多种的混合物。CeO2:ZrO2重量比可在例如80:20或20:80之间。市售可得的材料包括30重量% CeO2、63% ZrO2、5% Nd2O3、2%La2O3;和40% CeO2、50% ZrO2、4% La2O3、4% Nd2O3和2% Y2O3。
所述至少一种金属可广泛地存在于:(a) 遍及整个挤出固体,即所述至少一种金属存在于挤出物组合物中;(b) 在挤出固体的表面以较高的浓度存在;和/或(c) 在实施方案(A)和在实施方案(B)特征(iii),(v)和(vi)中携带于挤出固体表面上的一个或多个涂层中,所述至少一种金属不同于在(a)、(b)和(c)的每个其它位置存在的至少一种金属。因此所述至少一种金属可存在于位置(a)、(b)、(c)、(a)加(b)、(a)加(c)或(a)加(b)加(c)。其中所述至少一种金属存在于(a)和(b)、(a)和(c)或(a)、(b)和(c),所述至少一种金属在各个位置可相同或不同。
其中所述至少一种金属存在于位置(a)(即遍及整个挤出固体)时,所述至少一种金属可与存在的沸石分子筛、非沸石分子筛或它们的任何两种或更多种的混合物结合。“结合”的实例包括与沸石分子筛组分、非沸石分子筛组分或者混合的沸石分子筛组分和非沸石分子筛组分之一或两者离子交换。也可能在两种或更多种分子筛混合物中具有与一种分子筛而非另一种结合的至少一种金属。例如,第一种分子筛可与铜离子交换、干燥并焙烧,然后与未与另外的金属结合的不同分子筛混合。
或者,混合物中的两种分子筛之一可与第一种至少一种金属结合(例如离子交换),然后可将第二种至少一种金属加入挤出物组合物,即第二种至少一种金属未具体地与第二种分子筛结合。
与所述或各个分子筛组分结合的合适的至少一种金属可单独地选自过渡金属、镧系元素或它们的任何两种或更多种的混合物。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。优选地,所述至少一种过渡金属选自Fe、Cu、Ce、Hf、La、Mn、Pt、Au、Ag、In、Rh、V、Ir、Ru和Os和它们的任何两种或更多种的混合物。所述镧系元素金属可为La、Pr、Ce和它们的两种或更多种的混合物。
与所述或各个分子筛组分结合的至少一种金属中的金属总含量为0.1-20重量%,比如1-9重量%。
存在于以下的所述至少一种金属可选自过渡金属、镧系元素或它们的任何两种或更多种的混合物:遍及整个挤出固体而未与所述或各个分子筛结合;在位于挤出固体表面的至少一种金属的大多数中;在挤出固体表面上的一个或多个涂层中;或以较高浓度在挤出固体表面。
用于负载用于本发明的催化金属的合适的涂层包括以下一种或多种:氧化铝(Al2O3)(特别是γ-氧化铝)、二氧化硅(SiO2)、二氧化钛(TiO2)、二氧化铈(CeO2)、二氧化锆(ZrO2)、氧化钒(V2O5)、氧化镧(La2O3)和沸石。所述二氧化铈和氧化铝可使用与用于挤出固体的相同的稳定剂任选稳定。合适的催化金属包括一种或多种贵金属(Au、Ag和铂族金属,包括Pt、Pd和Rh)。为了促进挤出沸石(其已涂覆了含有贵金属的载体涂层(washcoat))的HC吸附活性,可有利地使用所谓的宽孔载体(例如氧化铝)作为用于贵金属的载体涂层载体(参见例如US6110862,即包含分散于耐火无机氧化物载体相上的铂族金属组分的催化材料,所述载体相包含第一载体材料,所述第一载体材料的孔径分布中,所述第一载体材料的约98%的孔容积由半径范围在约30-240 Å的孔提供。
用于将至少一种金属以较高的浓度定位于挤出固体表面的技术包括浸渍,优选稠化浸渍,即浸渍介质用流变改性剂增稠。干燥法也可用来使金属在挤出固体的表面浓缩。例如,所谓的"蛋壳技术",其中金属在表面浓缩可以通过以下获得:使浸渍的挤出固体相对缓慢地干燥,使得金属通过浸吸(wicking)沉积在表面。盐和pH条件的特定选择也可用于直接金属沉积,例如通过测定挤出固体的等电点然后使用正确的pH和金属盐组合来受益于金属盐中的阳离子或阴离子和挤出固体之间的静电引力。
合适的过渡金属包括IB族金属、IVB族金属、VB族金属、VIB族金属、VIIB族金属和VIII族金属。优选地,所述或各个过渡金属选自Fe、Ni、W、Cu、Ce、Hf、La、Mn、Pt、Au、Ag、In、V、Ir、Ru、Rh、Os和它们的任何两种或更多种的混合物;镧系金属可为La、Pr或Ce或它们的任何两种或更多种的混合物;碱金属包括K和Cs;和碱土金属可选自Ba和Sr。
以下各项的金属总含量可为0.1-20重量%,比如1-9重量%:遍及整个挤出固体而未与所述或各个分子筛组分结合;位于挤出固体的表面;和/或以较高的浓度在挤出固体的表面。
挤出固体的金属总含量(即包括与所述或各个分子筛结合的任何金属)可为0.1-25重量%,比如1-15重量%。
催化剂总体上(包括挤出固体表面上的一个或多个涂层)的金属总含量包含至少一种金属,可为0.1-30重量%,比如1-25重量%。
在实施方案(A)的具体实施例中,根据本发明的NOx吸收催化剂包含含有以下的挤出固体:
10-100重量%的堇青石、氮化物、碳化物、硼化物、金属间化合物、铝硅酸锂、任选掺杂的氧化铝、二氧化硅源、二氧化钛、二氧化锆、二氧化钛-二氧化锆、锆石和它们的任何两种或更多种的混合物;
0-80重量%的尖晶石;
0-90重量%的沸石分子筛、非沸石分子筛或它们的任何两种或更多种的混合物,各项任选含有一种或多种金属;
0-80重量%的任选稳定的二氧化铈;和
0-25重量%的无机纤维。
在实施方案(B)的具体实施例中,根据本发明的NOx吸收催化剂包含含有以下的挤出固体:
10-100重量%的堇青石、氮化物、碳化物、硼化物、金属间化合物、铝硅酸锂、任选掺杂的氧化铝、二氧化硅源、二氧化钛、二氧化锆、二氧化钛-二氧化锆、锆石和它们的任何两种或更多种的混合物;
0-80重量%的尖晶石;
5-80重量%的任选稳定的二氧化铈;和
0-25重量%的无机纤维。
所述至少一种粘合剂/基质组分的含量可为>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%。
所述尖晶石的含量可为>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%。
所述分子筛总含量的含量可为>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%、>75重量%、>80重量%、>85重量%或>90重量%。
所述任选稳定的二氧化铈的含量可为>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%。
所述无机纤维的含量可为>5重量%、>10重量%、>15重量%或>20重量%。
在特别适于使用氮还原剂还原氮氧化物的催化剂的实施方案中,挤出固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、金属间化合物、铝硅酸锂、尖晶石、任选掺杂的氧化铝、二氧化硅源、二氧化钛、二氧化锆、二氧化钛-二氧化锆、锆石和它们的任何两种或更多种的混合物;50-90重量%的沸石分子筛、非沸石分子筛或它们的任何两种或更多种的混合物,各项任选含有一种或多种金属;和0-25重量%的无机纤维。这种挤出固体可布置成流通式基底整料或其可用于制造壁流式过滤器。优选的实施方案含有无机纤维。
其它实施方案可使用基本上由以下组成的挤出固体:10-37重量%的堇青石、氮化物、碳化物、硼化物、金属间化合物、铝硅酸锂、任选掺杂的氧化铝、尖晶石、二氧化硅源、二氧化钛、二氧化锆、二氧化钛-二氧化锆、锆石和它们的任何两种或更多种的混合物;60-88重量%的沸石分子筛、非沸石分子筛或它们的任何两种或更多种的混合物,各项任选含有一种或多种金属;和0-20重量%的无机纤维;或:15-30重量%的堇青石、氮化物、碳化物、硼化物、金属间化合物、铝硅酸锂、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、锆石和它们的任何两种或更多种的混合物;2-20重量%的二氧化硅源;50-81重量%的沸石分子筛、非沸石分子筛或它们的任何两种或更多种的混合物,各项任选含有一种或多种金属;和2-10重量%的无机纤维。
在另一实施方案中挤出固体可基本上由以下组成:10-100重量%的堇青石、氮化物、碳化物、硼化物、金属间化合物、铝硅酸锂、任选掺杂的氧化铝、尖晶石、二氧化硅源、二氧化钛、二氧化锆、二氧化钛-二氧化锆、锆石和它们的任何两种或更多种的混合物;0-50重量%的沸石分子筛、非沸石分子筛或它们的任何两种或更多种的混合物,各项任选含有一种或多种金属;20-80重量%任选稳定的二氧化铈;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。
用于制造NOx捕集器或NOx捕集过滤器的特别优选的实施方案包含基本上由以下组成的挤出固体:10-100重量%的堇青石、氮化物、碳化物、硼化物、金属间化合物、铝硅酸锂、任选掺杂的氧化铝、二氧化钛、二氧化锆、二氧化钛-二氧化锆、锆石和它们的任何两种或更多种的混合物;0-20重量%的二氧化硅源;0-50重量%的铝酸镁尖晶石;20-80重量%的任选稳定的二氧化铈;和0-20重量%的无机纤维。也可期望将沸石包括在挤出固体内以便改善NOx转化,特别是继冷启动之后。优选的实施方案含有铝酸镁尖晶石和无机纤维。
在特定实施方案中,碱土金属(比如Ba和/或Sr)和/或碱金属(例如K和/或Cs)可在任选稳定的二氧化铈上喷雾干燥且得到的喷雾干燥产品用于形成挤出固体。
在开发用于根据本发明的NOx吸收催化剂的挤出固体中,我们遭遇了以下组合物的挤出固体缺乏强度:69重量%的CeO2,和23重量%的γ-Al2O3和8重量%的玻璃纤维。对于提高强度现在的建议包括预焙烧所述CeO2材料以减少焙烧"生料"挤出固体期间的表面损失;将氧化铝含量增加至50%+;变化氧化铝(例如从市售可得的Pural™到Disperal™)和/或任选稳定的二氧化铈的粒径;加入惰性粘合剂(例如粘土)来增强机械稳定性;使用不同的氧化铝,例如氧化铝溶胶;测试其它粘合剂体系,例如TiO2溶胶、CeO2溶胶;乙酸铈;乙酸锆;优化pH;和加入表面改性剂(例如铝盐或其它有机表面活性剂)。在初步测试中我们已发现二氧化硅的存在可影响NOx捕集性能。但是,研究正在继续并将进一步研究这种选择。但是,在一个实施方案中,会减少或完全除去二氧化硅源的含量。
根据本发明的NOx吸收催化剂实施方案(包括NOx吸收催化剂过滤器)的另一优势是催化剂涂层中的碱金属(比如钾)可与堇青石基底相互作用,削弱了基底和/或降低了催化剂活性。一种可能的原因是碱金属与堇青石中的硅酸盐相互作用。通过使用根据本发明的催化剂,可以降低或避免这种相互作用,特别是使用低二氧化硅含量时。
在特别适于NOx吸收催化剂和NOx吸收催化剂过滤器的另一实施方案中,挤出固体基本上由以下组成:10-50重量%的堇青石、氮化物、碳化物、硼化物、金属间化合物、铝硅酸锂、任选掺杂的氧化铝、二氧化钛、二氧化锆、二氧化钛-二氧化锆、锆石和它们的任何两种或更多种的混合物;0-10重量%的二氧化硅源;20-50重量%的铝酸镁;20-80重量%的任选稳定的二氧化铈;和0-10重量%的无机纤维。
其中将任何上述挤出固体制成壁流式过滤器时,壁流式过滤器的孔隙率可为30-80%,比如40-70%。
在根据本发明的更具体的实施例中,NOx吸收催化剂包含基本上由以下组成的挤出固体:10-100重量%的堇青石、氮化物、碳化物、硼化物、金属间化合物、铝硅酸锂、任选掺杂的氧化铝、二氧化钛、二氧化锆、二氧化钛-二氧化锆、锆石和它们的任何两种或更多种的混合物;0-40重量%的二氧化硅源;0-80重量%的铝酸镁尖晶石;0-80重量%的任选稳定的二氧化铈;0-25重量%的无机纤维;和0-20重量%的H2S吸气剂组分,所述挤出固体催化剂体用包含以下的组合物直接浸渍并用包含负载的铑的单层涂覆:碱金属、碱土金属、镧系元素或它们的两种或更多种的任意组合;铂、钯或铂和钯。在此实施方案中,所述H2S吸气剂组分可选自金属化合物,其中金属选自Ni、Fe和Mn。NOx吸收催化剂(NOx捕集器)可为壁流式过滤器的形式或为流通式结构。
根据另一方面,本发明提供根据前述权利要求任意一项的催化剂的制造方法,所述方法包含以下步骤:通过使以下粉末起始物料与任选的无机纤维混合,任选加入有机助剂,来形成固体挤出体:至少一种粘合剂/基质组分或它们的一种或多种的前体;任选的沸石分子筛、非沸石分子筛或它们的任何两种或更多种的混合物,所述任选的沸石分子筛、非沸石分子筛或沸石和非沸石分子筛的混合物任选与至少一种金属结合;任选的任选稳定的二氧化铈;和任选至少一种金属化合物;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/或捏合成塑性化合物进行处理来形成混合物;将所述混合物挤出成催化剂体,使所述催化剂体干燥并焙烧形成固体挤出体;选择起始物料的数量比例以使固体挤出体含有(A) 10-100重量%的至少一种粘合剂/基质组分;和5-90重量%的沸石分子筛、非沸石分子筛或它们的任何两种或更多种的混合物;或(B) 10-100重量%的至少一种粘合剂/基质组分;和5-80重量%任选稳定的二氧化铈;和用至少一种金属任选浸渍固体挤出体的表面和/或用含有至少一种金属的至少一个涂层任选涂覆固体挤出体的表面。
非常一般地,生产挤出固体,通过将粘合剂、提高粘度的有机化合物和用于通过共混成均一浆料而转化材料的液体加入粘合剂/基质组分或其前体和任选的分子筛、任选的任选稳定的二氧化铈、任选的无机纤维和任选的至少一种金属化合物,并将该混合物在混合或捏合设备或挤出机中压制。所述混合物具有有机添加剂,比如粘合剂、增塑剂、表面活性剂、润滑剂、分散剂作为处理助剂来增强润湿且因此产生均一的批料。然后特别使用挤压机或挤出机(包括挤出模)模塑得到的塑性材料,并将得到的塑模干燥和焙烧。所述有机添加剂在焙烧挤出固体期间"烧尽"。
所述至少一种粘合剂/基质组分选自:堇青石、氮化物、碳化物、硼化物、金属间化合物、铝硅酸锂、尖晶石、任选掺杂的氧化铝、二氧化硅源、二氧化钛、二氧化锆、二氧化钛-二氧化锆、锆石和它们的任何两种或更多种的混合物。可使用的氧化铝前体为氢氧化铝或勃姆石。在使用氧化铝时,为了保证与氧化铝的粘合,有利的是在加入其它起始物料之前,将可溶于水的金属盐的水溶液加入所述氧化铝或氧化铝的前体物质。
在实施方案中,所述二氧化硅源可选自:二氧化硅、二氧化硅溶胶、石英、熔融或无定形二氧化硅、硅酸钠、无定形铝硅酸盐、烷氧基硅烷、硅酮树脂粘合剂、粘土、滑石或它们的任何两种或更多种的混合物。
在特定的实施方案中,所述二氧化硅源为硅酮树脂粘合剂且用于硅酮树脂粘合剂的溶剂是异丙醇或二元酯。
根据本发明的方法的一个实施方案包含以下步骤:首先使任选掺杂的氧化铝或其前体与溶液混合,和随后混合沸石分子筛、非沸石分子筛或它们的任何两种或更多种的混合物和无机纤维。
用于根据本发明方法的有机助剂可为选自纤维素衍生物、有机增塑剂、润滑剂和水溶性树脂的一种或多种。合适的纤维素衍生物的实例包括选自以下的纤维素醚: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、羟丙基纤维素、甲基羟乙基纤维素、甲基羟丙基纤维素和它们的任何两种或更多种的组合。纤维素衍生物提高最终产品的孔隙率,所述孔隙率有利于固体催化剂体的催化活性。起初纤维素在水悬浮液中溶胀但是最终在焙烧过程期间被除去。
用于本发明方法的有机增塑剂选自:聚乙烯醇、聚乙烯醇缩丁醛、离聚物、丙烯酸类、乙烯/丙烯酸共聚物、聚氨酯、热塑性弹性体、相对低分子量的聚酯、亚麻子油、蓖麻油酸酯和它们的任何两种或更多种的组合。
所述水溶性树脂可为聚丙烯酸酯。
用于根据本发明方法的润滑剂选自以下至少之一:乙二醇、硬脂酸、硬脂酸钠、甘油和二醇。
取决于所述挤出物组合物的组成,pH可为酸性或碱性。在所述方法使用酸性水溶液时,溶液的pH值可为3和4之间。期望地,使用乙酸来使溶液酸化。
在所述方法使用碱性水溶液时,溶液的pH值可为8和9之间。氨可用来将pH调节至碱性侧。
根据另一方面,本发明提供使从车辆内燃机中排放的废气中的氮氧化物(NOx)转化的方法,所述方法包含使贫废气与根据本发明的NOx吸收催化剂接触来将NOx吸附于其上并使NOx吸收催化剂与富废气间歇地接触来使被吸附的NOx脱附并将NOx转化成N2。所述内燃机可为压缩点火发动机或主动点火发动机。主动点火发动机一般供以汽油燃料,但是可使用其它燃料,包括与含氧化物(包括甲醇和/或乙醇)共混的汽油燃料、液化石油气或压缩天然气。压缩点火发动机可供以柴油燃料、柴油燃料和生物柴油的共混物或Fischer-Tropsch衍生燃料、生物柴油本身或天然气本身。现代的压缩点火发动机包括称为稀释受控燃烧系统(Dilution Controlled Combustion System, DCCS)的那些,例如Toyota的无烟富燃烧(Smoke-less Rich Combustion)概念。也可处理来自均质充气压缩点燃(HomogeneousCharge Compression Ignition, HCCI)发动机的排放物。特别地,可以处理其中在燃烧开始之前将实质上所有用于燃烧的燃料都注入到燃烧室的现代发动机。
根据另一方面,本发明提供用于内燃机(任选如上文所定义)的排气系统,所述排气系统包含根据本发明的NOx吸收催化剂。
根据另一方面,本发明提供包含内燃机和根据本发明的排气系统的机动车。所述机动车一般包含,当使用时,根据按照本发明将从车辆内燃机中排放的废气中的氮氧化物(NOx)转化的方法来操作发动机的装置。
为了使本发明可更充分地被理解,仅仅通过说明的方式并参考附图提供了以下实施例,所述附图中:
图1是描绘了对于不同评价温度,根据本发明的NOx吸收催化剂样品和参比样品相比累积NOx效率低于70%(g/l)的点的图形;
图2是比较使用多种孔改性剂制备的多种V2O5/WOx-TiO2过滤材料相对于使用流通式结构的参比产品的孔容积和孔隙率的图形;和
图3是描绘相对于孔隙半径,许多孔改性剂相对于V2O5/WOx-TiO2参比和市售可得的壁流式过滤器基底的孔容积的图形。
实施例1-挤出固体
将适量的CeO2与玻璃纤维和粉末化合成勃姆石(Pural SB)混合并在pH值为3.5的醋酸水溶液中处理成可成形且可流动的条(slip),所述条含有1.2重量%的纤维素(CMC-QP10000H(Nordmann))和1.0重量%的有机助剂PEO Alkox(聚环氧乙烷)。选择起始物料的数量比例,其方式使得成品固体催化剂体的活性材料含有69重量%的CeO2和23重量%的γ-Al2O3和8重量%的玻璃纤维。将所述可成形的混合物挤压成具有连续通道和圆形截面的蜂窝催化剂体,其显示的胞孔密度为300 cpsi(胞孔每平方英寸)。随后,根据WO 2009/080155(其全部内容通过引用并入本文)中描述的方法使催化剂体在2mbar下冷冻干燥1小时并在580℃的温度下焙烧来形成固体催化剂体。所述挤出整料基底具有直径为大约14 cm的流入区域和大约19 cm的流通长度。从此样品上切下1英寸x3英寸的芯用于催化剂制备。
实施例2-催化剂制备
通过总吸附法使实施例1的1英寸x3英寸芯用Pt和Pd浸渍:将硝酸Pt(0.988g,Pt试验10.08%)和硝酸Pd(1.037g,Pd试验1.94%)稀释在脱矿质水中来得到50ml溶液。将所述固体放入此溶液中以使其充分浸没,然后使之放置总共24小时。从溶液中除去所述固体(过量的溶液用压缩空气流除去),然后在100℃下在空气流中干燥。然后使所述固体在500℃下焙烧1小时(坡道升温4℃/min)。对剩余的溶液进行ICP分析并证实剩余<1%的Pt/Pd。通过浸入浸渍加入钡:将乙酸钡(8.88g)溶于脱矿质水来得到50ml的溶液(55.3g)。将所述芯浸没在所述溶液中1分钟,然后通过压缩空气流除去过量的溶液。被芯吸收的溶液的质量=9.70g。如上所述将所述芯干燥并焙烧。
如下制备参比芯:将硝酸Pt(540g,Pt试验10.07%)和硝酸Pd(73g, Pd试验15.14%)搅拌加入氧化铝浆料(4494 g的γ氧化铝,44.5%坩埚固体)中。使得到的载体涂层放置1小时,此后顺次搅拌加入二氧化铈(2083g)、乙酸钡(861g)和乙酸铈(565g)。加入脱矿质水来获得42.5%的坩埚固体含量,随后加入0.5重量%的羟乙基纤维素增稠剂。使用WO 99/47260(其全部内容通过引用并入本文)中公开的方法将得到的载体涂层投料在标准陶瓷整料(4.66英寸x3英寸,400cpsi,千分之六英寸壁厚)上,在100℃下在空气流中干燥并在500℃下焙烧1小时。从得到的催化剂中取出和实施例1样品等体积的芯。
实施例3-NOx储存测试
催化的挤出固体和实施例2的参比样品两者都代表充分配制的NOx吸收催化剂的底层。在充分配制的NOx吸收催化剂中,两者样品将用包含负载于氧化铝或稳定的二氧化锆上的铑的附加层涂覆。充分配制的NOx吸收催化剂的底层设计成用于储存NOx,因此其用于储存NOx的活性可独立于附加层而评价。
在实验室合成催化剂活性试验(SCAT)设备上,在NOx储存试验中测试上述样品。使用的气体混合物在表1中给出。
表1:用于NOx储存试验的气体混合物
* 2:1丙烯:丙烷。
本测试包括预处理步骤来清洁具有任何储存NOx的催化剂,随后是储存步骤。这用六个不同的评价温度重复:125、150、175、200、250和300℃。所述预处理步骤包括坡道升温至450℃(40℃/min,在N2中),温度一旦稳定,随后在富气体混合物中120秒。然后使所述样品在N2中冷却至测试的评价温度。引入贫气体混合物(无NO)并使之稳定,然后储存期随着将NO引入气流中时开始。在储存期进行时监测累积NOx效率。此累积效率定义为:
。
继续NOx储存期直到累积NOx效率低于70%。在这一点储存的累积NOx(g/L)为NOx储存70%或“NS70”值,其可对不同的评价温度绘制。
对未老化的(或“新鲜的”)样品的初期试验之后,使所述样品在800℃下在空气中烘箱老化24小时并再测试老化的样品。
评价的结果显示在图1中,在所述图中根据本发明的样品称作“挤出的LNT”。可以看出,根据本发明的浸渍的挤出固体与新鲜的和老化的参比两者相比,在175-300℃(包括)之间的所有温度下显示了更好的NOx储存活性。
实施例2制品的一个优势是,当充分配制成包括含铑层时,催化剂总体上包含涂覆了一个层的挤出固体。相比之下,所述参比样品包含具有两层的基底整料。所述两层可减小流体通道的截面,导致增加了背压或,如果背压通过负载较少的载体涂层(g/in3)解决,可降低催化剂的总体活性。
实施例4-挤出的V2O5/WOx-TiO2过滤器
类似于实施例1和5通过将如表1所列出的组分A、B、F和S与水共混制造可捏合的浆料而制备参比挤出的V2O5/WOx-TiO2固体。加入添加剂H(孔改性剂)并将所述材料捏合10 min来分散孔改性剂。如实施例1和5所述将得到的组合物挤出、干燥并焙烧。应注意到,最终焙烧的制品中存在的无机固体的百分比数量是100%。提供的在焙烧期间通过燃烧除去的添加剂(此处H和S)的量是相对于100%无机固体含量的重量%。
表2
A1 = TiW(98,9%, MC 10/晶体)
A2 = 来自AMV的V2O5(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(Vetrotex 4,5 mm/Saint Gobain)
H1 =纤维素(QP10000H/Nordmann)
H2 = PEO(Alkox/Alroko)
H3 = Zusoplast(Zschimmer&Schwarz)
S1 = MEA(Imhoff & Stahl)
S2 = NH3
S3 = C3H6O3(Fauth)。
使用下列孔改性剂而不是表2中的挤出添加剂H1、H2和H3,其中显示的量是相对于表2的配方中的无机固体的总重量。
表3
。
孔隙率和孔容积和孔半径可例如使用压汞孔隙率测定法测量。
表3条目(包括孔容积和孔隙率)的结果也描绘于图2。由这些结果可见,参比的孔隙率和孔容积可通过适当选择孔改性剂提高,使得使用这些孔改性剂制造的挤出固体可用于制造壁流式过滤器。
这些结果通用于增大孔隙率、孔容积等性质,与固体挤出体的活性组分无关。即,虽然使用V2O5/WOx-TiO2活性材料说明了此实施例6的增大孔隙率和孔容积等,但是此实施例6中公开的增大孔隙率和孔容积等的原理适用于任何活性材料的挤出,例如用于包含三效催化剂的汽油烟尘过滤器的挤出固体,因为所述孔改性剂在焙烧过程中被烧尽,留下活性材料和填料等作为无机固体。
图3比较了不同参比与使用表2中列出的其它孔改性剂制备的固体挤出V2O5/WOx-TiO2材料,也与市售可得的壁流式过滤器(NGK)比较的孔容积。从图中可见,包括孔改性剂改善了参比挤出固体的孔隙率和孔容积,使得所述材料具有接近那些市售可得的壁流式过滤器的性质。
实施例5-挤出的壁流式NOx吸收催化剂过滤器
这是预言性实施例。可由实施例1的可成形和可流动的条制备挤出整料基底,除了可加入孔改性剂Rettenmaier BC200、天然纤维素材料和聚丙烯腈(PAN)纤维的总共13重量%的混合物来制造所述可成形和可流动的条。可选择起始物料的数量比例,其方式使得成品固体催化剂体的活性材料含有69重量%的CeO2和23重量%的γ-Al2O3和8重量%的玻璃纤维。一般地,期望得到的产品将具有大约10μm的平均孔径。
焙烧的挤出整料基底可使用公开于WO99/47260(其全部内容通过引用并入本文)的方法用增稠的浸渍介质浸渍,所述浸渍介质包含硝酸铂、硝酸钯和乙酸钡。然后可干燥并灼烧得到的浸渍的基底。可将包含稳定的二氧化锆和硝酸铑的载体涂层涂覆于浸渍的基底上。然后可将这种浸渍的,然后涂覆的装置干燥并灼烧。铂和钯的总负载可为大约100gft-3,Pt5:Pd,和钡大约在800ft-3。铑可存在大约10gft-3。
所述包含多个通道的挤出的流通式整料基底可制造成壁流式过滤器布置,由此多个第一通道在上游端被堵塞且上游端未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通过在通道端以根据EP 1837063(其全部内容通过引用并入本文)期望的模式插入实质上不透气的塞子,使得横向和竖直相邻的通道在相对端以棋盘的外观被堵塞。这种过滤器排列也公开于SAE 810114(其全部内容通过引用并入本文)。浸渍焙烧产物。
为了避免任何疑惑,本文引用的任何和所有文献的全部内容通过引用并入本文中。
Claims (10)
1.一种NOx吸收催化剂,其包含含有以下的挤出固体:
10-100重量%的至少一种粘合剂/基质组分;和5-80重量%任选稳定的二氧化铈,所述催化剂包含以下的至少一种金属:(a)至少一种贵金属;和(b)至少一种碱金属或至少一种碱土金属,其中:
(i) 所述至少一种碱金属或至少一种碱土金属存在于整个挤出固体中;
(ii) 大部分的所述至少一种碱金属或至少一种碱土金属位于挤出固体的表面;
(iii) 所述至少一种碱金属或至少一种碱土金属携带于挤出固体表面上的一个或多个涂层;
(iv) 所述至少一种碱金属或至少一种碱土金属存在于整个挤出固体且在挤出固体的表面也以较高的浓度存在;
(v) 所述至少一种碱金属或至少一种碱土金属存在于整个挤出固体且也携带于挤出固体表面上的一个或多个涂层;或
(vi) 所述至少一种碱金属或至少一种碱土金属存在于整个挤出固体,在挤出固体的表面以较高的浓度存在且也携带于挤出固体表面上的一个或多个涂层。
2.根据权利要求1的NOx吸收催化剂,其中存在于以下各项的至少一种金属不同于存在于其它位置的至少一种金属:(a) 整个挤出固体;(b) 以较高的浓度存在于挤出固体的表面;和(c) 携带于挤出固体表面上的一个或多个涂层。
3.根据权利要求1或2的NOx吸收催化剂,其中所述至少一种贵金属负载于挤出固体表面上的一个或多个涂层,其中所述或各个涂层包含以下一种或多种:任选稳定的氧化铝、二氧化硅、二氧化钛、任选稳定的二氧化铈、任选稳定的二氧化锆、氧化钒、氧化镧、尖晶石和它们的任何两种或更多种的混合物。
4.根据权利要求3的NOx吸收催化剂,其包含两个或更多个涂层,其中第一底层包含任选稳定的二氧化铈和尖晶石的混合物。
5.根据权利要求4的NOx吸收催化剂,其中覆盖第一底层的第二层包含负载在一种或多种氧化铝和任选稳定的二氧化锆上的铑。
6.根据权利要求5的NOx吸收催化剂,其中覆盖第二层的第三层包含负载在块体可还原氧化物上的沸石或铂和/或钯,所述可还原氧化物实质上不含碱金属和碱土金属。
7.根据权利要求3的NOx吸收催化剂,其包含一个或多个涂层,其中铂和/或钯位于挤出固体的表面且其中第一底层包含负载在一种或多种氧化铝和任选稳定的二氧化锆上的铑。
8.根据权利要求7的NOx吸收催化剂,其中覆盖第一层的第二层包含负载在块体可还原氧化物上的沸石或铂和/或钯,所述可还原氧化物实质上不含碱金属和碱土金属。
9.根据权利要求6或8的NOx吸收催化剂,其中所述块体可还原氧化物选自氧化物、复合氧化物和包含选自以下的一种或多种金属的混合氧化物:锰、铁、锡、铜、钴或铈和它们的任选稳定的类似物。
10.根据权利要求9的装置,其中所述至少一种可还原氧化物包含MnO2、Mn2O3、Fe2O3、SnO2、CuO、CoO和CeO2。
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CN113507973A (zh) * | 2019-02-27 | 2021-10-15 | 禹泰荣 | 利用光催化剂预敷涂层的玻璃及铝结构体空气过滤器及其制造方法 |
CN113507973B (zh) * | 2019-02-27 | 2023-03-28 | 禹泰荣 | 利用光催化剂预敷涂层的玻璃及铝结构体空气过滤器及其制造方法 |
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