CN105840273A - 组合式选择性催化还原催化剂和微粒过滤器 - Google Patents

组合式选择性催化还原催化剂和微粒过滤器 Download PDF

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Publication number
CN105840273A
CN105840273A CN201610245145.7A CN201610245145A CN105840273A CN 105840273 A CN105840273 A CN 105840273A CN 201610245145 A CN201610245145 A CN 201610245145A CN 105840273 A CN105840273 A CN 105840273A
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Prior art keywords
particulate filter
catalytic reduction
selective catalytic
combination type
microgranule
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CN201610245145.7A
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黄银燕
克里斯汀·凯·兰伯特
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Ford Global Technologies LLC
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Ford Global Technologies LLC
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Publication of CN105840273A publication Critical patent/CN105840273A/zh
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    • F01N3/00—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust
    • F01N3/02—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for cooling, or for removing solid constituents of, exhaust
    • F01N3/021—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for cooling, or for removing solid constituents of, exhaust by means of filters
    • F01N3/033—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for cooling, or for removing solid constituents of, exhaust by means of filters in combination with other devices
    • F01N3/035—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for cooling, or for removing solid constituents of, exhaust by means of filters in combination with other devices with catalytic reactors, e.g. catalysed diesel particulate filters
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    • F01N3/00—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust
    • F01N3/02—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for cooling, or for removing solid constituents of, exhaust
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Abstract

本发明公开了一种组合式选择性催化还原催化剂和微粒过滤器。在至少一个实施例中，组合式选择性催化还原催化剂和微粒过滤器包括：微粒过滤器，具有壁，所述壁包括结构亚基和NH3氧化合成物微粒，所述过滤器限定入口通道和出口通道，入口通道包括下游端盖，出口通道包括上游端盖和开口端，其中，所述壁具有在40体积％至85体积％的范围内的孔隙度；以及涂层，在出口端靠近所述壁，其中，涂层包括贵金属微粒且涂层的长度大约小于出口通道的长度的50％。

Description

组合式选择性催化还原催化剂和微粒过滤器
本申请是申请日为2011年11月3日、申请号为201110348638.0、题为“组合式选择性催化还原催化剂和微粒过滤器”的专利申请的分案申请。
技术领域
本发明的一方面涉及一种用于处理排放物的装置及其制造方法。
背景技术
法规关注的排放物包括氮氧化物。氮氧化物包括但不限于一氧化氮(NO)和二氧化氮(NO2)。按照美国环境保护署的规定，这些化合物通常被称为NOx。
已提出处理系统，以对来自柴油发动机的排放物中的NOx进行处理，但是一般来说，处理系统相对比较昂贵。
发明内容
在至少一个实施例中，组合式选择性催化还原催化剂和微粒过滤器(SCRF)包括具有壁的微粒过滤器。所述壁限定入口通道和出口通道，入口通道包括下游端盖，出口通道包括上游端盖和开口端，排放物穿过所述开口端。所述壁还限定多个孔。所述壁包括多个沸石-贱金属微粒。涂层的长度大约小于出口通道的长度的50％。涂层能够容纳贵金属微粒。
在可选实施例中，微粒过滤器具有壁，所述壁包括结构亚基和NH3氧化合成物微粒。过滤器限定入口通道和出口通道，入口通道包括下游端盖，出口通道包括上游端盖和开口端。所述壁具有在40vol.％至85vol.％的范围内的孔隙度。涂层的长度大约小于出口通道的长度的50％。涂层能够容纳贵金属微粒。
在另一实施例中，一种制造组合式选择性催化还原催化剂和微粒过滤器(SCRF)的方法包括经过离子交换而使贱金属离子进入到沸石中，以形成多个沸石-贱金属微粒。将沸石-贱金属微粒、粘合剂、成孔合成物混合，以形成可挤压的混合物。挤压可挤压的混合物，以形成具有壁的微粒过滤器，所述壁限定入口通道和出口通道，入口通道包括下游端盖，出口通道包括上游端盖和开口端。焚烧成孔剂，以形成具有40vol.％至85vol.％的孔隙度的微粒过滤器。涂覆涂层以使其长度大约小于出口通道的长度的50％。加热涂层，以干燥涂层。将贵金属涂于涂层。加热贵金属以使其干燥，从而完成SCRF。
附图说明
图1示意性地示出了根据特定实施例的排放物处理装置；
图2示意性地示出了组合式选择性催化还原(SCR)催化剂和微粒过滤器(SCRF)沿着图1的2-2轴的断开截面图；
图3示意性地示出了SCRF沿着图2的3-3轴的截面图；
图4示意性地示出了SCRF沿着图2的4-4轴的截面图；
图5图解式地示出了根据至少一个实施例的制造SCRF的方法。
具体实施方式
现在，将详细描述为发明人所知的本发明的构成、实施例及方法。然而，应该理解的是，公开的实施例仅仅是可以以各种和可选的形式实施的本发明的示例。因此，在此公开的具体细节不应该被解释为限制，而仅仅作为用于教导本领域的技术人员以各种方式应用本发明的代表性基准。
除非清楚地指示，否则在本说明书中指示材料的量或者反应和/或使用条件的所有数值量在描述本发明的最大范围时应该被理解为由词语“大约”修饰。在数值极限内开始的实践应该是期望的且被独立地实施。
对适合于与本发明相关的给定目的的一组或一类材料的描述意味着所述组或类中的任意两种或更多种成分的混合物也是合适的。
对化学术语中的成分的描述指的是在添加到本说明书中说明的任何化合物时的成分，且未必排除混合后的混合物的成分之间的化学相互作用。首字母缩略词或其他缩写词的第一定义应用于随后在此使用的所有相同的缩写词，且将必要的变通应用于最初定义的缩写词的正常语法变型。对于相同的特性来说，除非清楚地作相反说明，否则通过与之前或之后参考的技术相同的技术来确定所述特性的测量。
现在，参照图1，示意性地示出了示例性的处理装置。处理装置10接收来自发动机12的废气14。废气14在靠近发动机12的入口16处进入处理装置10。废气14在具有纵向轴的废气导管18(例如，管)中行进。导管18的一部分将入口16与组合式选择性催化还原(SCR)催化剂和微粒过滤器(SCRF)20连接。在示出的实施例中，还原剂26(例如，类似于尿素的还原剂)储存在储存容器28中，并通过导管32被传送到还原剂传送系统30。传送系统30通过位于SCRF 20的上游的孔被结合到导管18的一部分。
SCRF 20能够改善对CO、碳氢化合物以及NH3的控制，从而防止在发动机的各种瞬态操作模式期间这些气体从处理装置10意外逃脱。
与现有的处理系统相比，SCRF 20是集成式系统，该集成式系统使制造成本更低并使昂贵材料的使用减少，该集成式系统实现等效的处理控制所需要的处理装置的体积更小。
SCRF 20可通过直接挤压工艺形成，其中，在挤压成块之前，将贱金属-沸石选择性催化还原(SCR)催化剂合成物与粘合剂、成孔合成物以及支撑材料混合。在至少一个实施例中，由于与先前的处理系统相比SCRF 20具有更大的孔体积且具有更少的涂层堵塞孔，所以SCRF 20能够减小背压。
图2示出了SCRF 20沿着图1的2-2轴的断开截面图。基板40是微粒过滤器(例如，柴油机微粒过滤器)基板。当挤压基板40时，基板40形成拉长的通道48和52。在交替的端部利用塞子54堵住交替的通道，从而迫使气体排放物46(图3)从接收气体的入口通道(例如，通道48)经由壁50移动到气体作为处理后的气体68从其中离开的出口通道(例如，通道52)。
一般来说，基板40的壁50必须具有足够的孔隙度，以在从排放物46(图3)去除微粒物的同时使排放物46从入口通道48流动到出口通道52。在第5,069,697号美国专利中公开了用于形成基板40的实用的制造技术。该专利公开的全部内容通过引用被包含于此。在特定实施例中，基板40可以是由包括折射材料的合成物形成的蜂窝块(honeycombed monolith)。
如图3示意性地示出的，在至少一个实施例中，基板40可包括多个沸石和NO氧化合成物微粒(例如，沸石-贱金属微粒60)以及可选的粘合剂材料62的混合物。沸石-贱金属微粒60和粘合剂材料62限定贯穿壁50的多个孔58。在实施例中，在基板40被烧结(焚烧部分或全部粘合剂材料62)之前粘合剂材料62通常是存在的。粘合剂材料62的焚烧通常可使基板40中孔的体积增加。在特定实施例中，在基板40被烧结之前，成孔材料也是存在的。通常，在烧结余下的孔58期间焚烧成孔材料。
如图4示意性地示出的，在至少一个实施例中，在基板40中靠近出口通道52的壁50随后被涂覆有涂层64，涂层64具有贵金属微粒66(例如，微晶粒)。
在至少一个实施例中，涂覆涂层64以使其长度达到SCRF 20的总长的50％。在另一实施例中，SCRF的涂覆有涂层64的长度小于SCRF的总长的20％。在另一实施例中，涂覆涂层64以使其长度达到SCRF的总长的15％。
应该理解的是，在至少一个实施例中，贵金属微粒66可以位于SCRF的总长的10％至SCRF的总长的100％的范围内。在另一实施例中，贵金属微粒66可以基本上位于SCRF的总长的20％至SCRF的总长的50％的范围内。
在另一实施例中，贵金属微粒66可以基本上位于涂层64的长度的10％至涂层64的长度的150％的范围内。在另一实施例中，贵金属微粒66可以基本上位于涂层64的长度的50％至涂层64的长度的100％的范围内。
在至少一个实施例中，催化剂中的贵金属微粒的量在0.1wt.％至3wt.％(即，重量百分比)的范围内。在另一实施例中，贵金属微粒的量在0.5wt.％至1.5wt.％的范围内。
在另一实施例中，贵金属微粒66的量在0.5g/ft3至5g/ft3(即，克每立方英尺)的范围内。在另一实施例中，贵金属微粒的量在1g/ft3至4g/ft3的范围内。
贵金属微粒66可包括但不限于铂、钯、铑、金、铼、锇以及铱的微粒。优先选用钯和/或铂来抑制一氧化碳、碳氢化合物以及氨从SCRF 20逃脱。
在至少一个实施例中，钯的含量与铂的含量的比率在0.1至10的范围内。在另一实施例中，钯的含量与铂的含量的比率在0.2至5的范围内。
通常，壁50具有对允许排放物46穿过壁50有效的孔隙度，而不会产生比现有技术中已知的选择性催化还原(SCR)系统明显高的背压。作为孔隙度测量的非限制性示例，在至少一个实施例中，壁50产生的背压小于20英寸的水产生的背压。
在至少一个实施例中，壁50的孔隙度在40vol.％至85vol.％(即，体积百分比)的范围内。在另一实施例中，壁50的孔隙度在45vol.％至60vol.％的范围内。
在至少一个实施例中，壁50的孔的平均尺寸在直径为10微米至直径为30微米的范围内。在另一实施例中，壁50的孔的平均尺寸在直径为15微米至直径为25微米的范围内。在至少一个实施例中，孔的平均尺寸包括在互相连接的间隙中通道的有效宽度。在另一实施例中，孔的尺寸包括在用于制造壁50的沸石-贱金属微粒60的合成物的结构亚基(SSU)中的腔的平均有效通道宽度。
在至少一个实施例中，壁50包括沸石的至少一种合成物或者具有结构亚基(SSU)的其他合成物(例如，磷酸铝)。沸石包含独特的四面体MO4结构亚基，其中，M可以是硅、铝、磷、镓、硼或者铍。沸石可包括有限成分单元和无限成分单元。有限成分单元的非限制性示例包括有限结构亚基以及二级构造单元(SBU)，例如，四元环、五元环或者六元环。无限成分单元的非限制性示例是成分链(component chain)和成分层(component layer)。沸石成分链的非限制性示例包括曲折链、锯链、曲轴形链。成分层的非限制性示例包括单个三元环和/或四元环、双四元环、五元环、双六元环、非连接式六元环(ABC-6家族)、β和/或类β家族、包合物(clathrasils)以及笼形物(cage)。在至少一个实施例中，优先选用菱沸石，例如，CHA沸石、SSZ-62沸石、SAPO-34沸石、SAPO-44沸石。
在美国专利6,709,644中公开了形成适用于壁50的沸石的非限制性示例，该专利通过引用被包含于此。
在至少一个实施例中，硅与铝的比率在10至20的范围内。在另一实施例中，硅与铝的比率在12至15的范围内。
在至少一个实施例中，在经过离子交换变成沸石-贱金属微粒60之前，沸石的基于金属氧化物的I族和/或II族金属的平均含量在沸石的0.01wt.％至沸石的5wt.％的范围内。在另一实施例中，在经过离子交换变成沸石-贱金属微粒60之前，沸石的I族和/或II族金属的平均含量在沸石的0.1wt.％至沸石的2wt.％的范围内。
在至少一个实施例中，在离子交换变换之后，沸石包括平均含量小于0.5wt.％的基于金属氧化物的I族和/或II族金属，优选地，当开始时，基本上为氢离子的形式。
沸石-贱金属微粒60可包括至少一种沸石，所述至少一种沸石具有贱金属，该贱金属被引入到位于沸石中和/或沸石上的可进行离子交换的位置。在现有技术中(例如，在美国专利7,704,475中)已经公开了使贱金属离子进行离子交换的非限制性方法。
在至少一个实施例中，通过在现有技术中已知的离子交换方法去除存在于沸石中的I族和/或II族金属离子。I族和/或II族金属离子被贱金属离子或氢离子代替。可选地，在另一实施例中，在第二步骤中，氢离子被贱金属离子代替。应该理解的是，在不超过这里的实施例的范围和/或精神的情况下，在与沸石进行离子交换期间，可使用多于一种类型的贱金属离子。
适合于包含在沸石-贱金属微粒60中的贱金属包括但不限于用于将NO氧化成NO2的贱金属催化剂、过渡金属、能够在至少两种氧化状态之间交替的贱金属。优选地，用于包含在沸石-贱金属微粒60中的贱金属包括锰、钼、钛、钒、钨、铜、钴、铁和/或镍。
在至少一个实施例中，沸石-贱金属微粒的贱金属的平均含量在沸石-贱金属微粒的1wt.％至15wt.％的范围内。在另一实施例中，沸石-贱金属微粒的贱金属的平均含量在沸石-贱金属微粒的2wt.％至5wt.％的范围内。
在至少一个实施例中，粘合剂包括无机聚合物。在另一实施例中，粘合剂包括氧化铝、二氧化硅和/或氧化锆。在另一实施例中，粘合剂包括硅树脂和乳化硅(silicone emulsion)。在美国专利7,754,638中公开了粘合剂的非限制性示例。
沸石-贱金属微粒粘合剂与烧结块的比率在1至9的范围内。
在至少一个实施例中，成孔材料包括有机聚合物。在另一实施例中，成孔材料包括木质纤维聚合物和/或石墨聚合物。在另一实施例中，成孔材料包括淀粉和/或石墨。
挤出物的成分包括在表1中示出的下列各项(可独立选择)：
表1
在至少一个实施例中，在烧结挤出物之后，块的孔隙度在40vol.％至85vol.％的范围内。在另一实施例中，块的孔隙度在50vol.％至75vol.％的范围内。在另一实施例中，块的孔隙度在55vol.％至70vol.％的范围内。
优选地，沸石-贱金属微粒60中的贱金属包括具有氧储存能力、能够经历氧化还原反应和/或能够氧化NH3的贱金属半族(moiety)。应该理解的是，提高沸石-贱金属微粒60的活性的其他金属半族可包括在壁50的成分的特定实施例中。还应该理解的是，在不超过实施例的范围和精神的情况下，一种或多种贱金属可包括在壁50的成分中。
关于图5，一种制造用于处理排放物的装置的方法包括将沸石-贱金属微粒60、粘合剂材料62以及成孔材料混合，以形成可挤压的合成物(步骤100)。
在步骤116中，可通过使贱金属离子与最初位于沸石上的I族和/或II族金属离子直接进行离子交换来形成沸石-贱金属微粒60。在可选的实施例中，I族和/或II族金属离子通过与来自酸的氢离子进行离子交换而离开沸石。氢离子通过与贱金属离子进行离子交换而离开沸石。
在步骤102中，可挤压的合成物被挤压成蜂窝块，例如，每平方英寸10个穴的蜂窝块。在步骤104中，蜂窝块被暴露于超过700℃的温度条件下，以形成烧结的陶瓷合成物。
在步骤106中，蜂窝块的穴的交替的端部被堵住，以形成微粒过滤器。
在步骤108中，涂覆涂层以使其长度达到蜂窝块的长度的20％。涂层被涂到通道的端部(处理后的排放物从所述通道释放出来)。涂层的非限制性示例包括溶解在其PH在0.5至3的范围内的硝酸中的γ氧化铝。溶解的氧化铝形成浆液，然后可利用在现有技术中已知的工艺(例如，浸渍和真空淀积)使所述浆液作为涂层被涂覆。在至少一个实施例中，涂层64基本上与出口通道的开口端相邻。
在步骤110中，带涂层的块被暴露于80℃与200℃之间的温度条件下，以锻烧涂层64。
在步骤112中，将贵金属溶液涂于涂层。在步骤114中，包含贵金属溶液的涂层64被暴露于80℃和200℃之间的温度条件下，以形成贵金属微粒66。
虽然已经详细描述了用于实施本发明的最佳方式，但是熟悉与本发明相关的领域的技术人员将认识到用于实施由权利要求限定的本发明的各种可选设计和实施例。

Claims (7)

1.一种组合式选择性催化还原催化剂和微粒过滤器，所述组合式选择性催化还原催化剂和微粒过滤器包括：
微粒过滤器，具有壁，所述壁包括结构亚基和NH3氧化合成物微粒，所述过滤器限定入口通道和出口通道，入口通道包括下游端盖，出口通道包括上游端盖和开口端，其中，所述壁具有在40体积％至85体积％的范围内的孔隙度；以及
涂层，在出口端靠近所述壁，其中，涂层包括贵金属微粒且涂层的长度小于出口通道的长度的50％。
2.根据权利要求1所述的组合式选择性催化还原催化剂和微粒过滤器，其中，结构亚基和NH3氧化合成物微粒包括具有氧储存成分的合成物。
3.根据权利要求1所述的组合式选择性催化还原催化剂和微粒过滤器，其中，结构亚基和NH3氧化合成物微粒包括具有贱金属的合成物。
4.根据权利要求1所述的组合式选择性催化还原催化剂和微粒过滤器，其中，在离子交换之后，当开始时，结构亚基和NH3氧化合成物微粒基本上为氢离子的形式。
5.根据权利要求1所述的组合式选择性催化还原催化剂和微粒过滤器，其中，涂层基本上与开口端相邻。
6.根据权利要求1所述的组合式选择性催化还原催化剂和微粒过滤器，其中，贵金属微粒基本上与开口端相邻。
7.根据权利要求1所述的组合式选择性催化还原催化剂和微粒过滤器，其中，当表示为金属时，所述微粒包括1重量％至15重量％的贱金属。
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