CN101370583A - 陶瓷蜂窝体的催化涂覆方法 - Google Patents
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Abstract
本发明涉及陶瓷蜂窝体的催化涂覆方法,该方法使用在载液中包含固体和/或溶解形式的催化剂成分的涂覆悬浮体。该蜂窝体具有贯穿其中的平行流动通道。该流动通道的壁通常具有开放孔隙结构。为了用涂覆悬浮体涂覆通道壁和特别是孔隙的内表面,提出了将流动通道暂时交替封闭使该涂覆悬浮体强制通过通道壁的开放孔隙结构。然后涂覆被干燥和煅烧。为了封闭流动通道,可以使用热或化学可分解的或者可溶解的组分,其或者在煅烧中或者通过后续的化学处理可以被分解或溶解。该涂覆蜂窝体优选用作车辆废气的净化。
Description
技术领域
本发明涉及用涂覆悬浮体涂布陶瓷蜂窝体的方法,所述涂覆悬浮体在载液(carrier liquid)中以固体和/或溶解形式包含催化剂成分。该涂覆蜂窝体优选用于车辆废气的净化。
背景技术
以涂覆的形式向蜂窝体施加的催化剂已经用于车辆废气净化多年。蜂窝体具有用于废气通过其中的平行流动通道。陶瓷蜂窝体用高度难熔的材料制成。主要是用堇青石(一种镁-铝硅酸盐)制成。其它通常使用的陶瓷材料有金刚砂、氧化铝、氧化锆、锆高铝红柱石、高铝红柱石、氮化硅、钛酸钡和氧化钛。蜂窝体是以这些材料通过挤出制备的,并且通常具有开放孔隙结构。
流动通道从进口端面(end face)到出口端面穿过蜂窝体。这些通道通常具有方形截面并以紧密间隔的格子排列在蜂窝体的横截面上。每单位横截面区域的流动通道数量作为单元密度(cell density)可以是10-200cm-2。
蜂窝体的催化涂覆是分散体涂覆,所述分散体涂覆通常是用催化剂成分的水悬浮体施加到所述蜂窝体上。该涂层在下文中也被称为活化涂层(washcoat)。
该催化剂成分包括,例如,具有高比表面积的精细分离的载体材料,在其上施加有催化活性成分,通常是铂系贵金属铂、钯、铑、铱和钌。在催化剂悬浮体中的固体在应用到蜂窝体前通常通过湿磨匀化。研磨后,悬浮体的固体的平均粒度d50为3-5μm。
载体材料的实例有单一和混合氧化物,例如,活性氧化铝、氧化锆、氧化锡、氧化铈、或其它稀土元素氧化物、氧化硅、氧化钛、和硅酸盐例如硅酸铝或钛酸盐例如钛酸钡或钛酸铝以及沸石。已经发现过渡系列(transition series)的活性氧化铝的各种相(phase)(可以通过涂布氧化硅和氧化镧或者氧化锆和氧化铈稳定)作为耐热载体材料特别有用。
如果下面称用催化活性层涂覆蜂窝体涂覆,这是指流动通道的通道壁的涂覆。不需要涂覆蜂窝体的外壁。施加涂层的量通常基于蜂窝体的外部体积以g/L计。本领域技术人员非常熟悉通常进行这种涂布的方法。
为了满足所需要求,涂层的浓度需要取决于特定的任务。总的来说,浓度越大,涂层的活性越大并越耐老化。实际中,根据用途,需要10-300g/L。然而,由于多种原因,最大可达到的浓度可以低于催化所需浓度。因此,涂层的粘附力以及由此的层厚度随着浓度的增加而降低。此外,高的层厚度降低流动通道的水力直径,并因此增加催化剂的废气反压力(背压力)。
有些应用,例如发动机废气中烃类和一氧化碳的氧化(“发动机氧化催化剂”),其中反应所需的催化剂仅有相对低的量,为100-200g/L蜂窝体体积。在这种情况下,进一步增加催化剂的量同时保持总的贵金属含量与活性优势没有关系。在其它催化反应的情况下,例如氮氧化物的存储和降低(“氮氧化物存储催化剂”)或通过氨选择性催化降低氮氧化物(“SCR催化剂”),另一方面,需要增加活性材料的量,但是可以仅适当地增加,这是由于上述的涂覆粘附力和最终的催化剂的背压力问题。
为了降低高的背压力,US 5,334,570提出了在陶瓷蜂窝体的孔隙中重新设置催化涂层。用于该专利的陶瓷蜂窝体的开放孔隙率为30-45%以及平均孔径为3-10μm。由于这个原因,使用胶状粒径为0.001-0.1μm,优选0.001-0.05μm,并且当蜂窝体与相应的胶状涂覆分散体接触时渗入蜂窝体的孔隙中的催化剂材料作为催化涂层。根据该专利,将蜂窝体浸入涂覆分散体中,以将它们与涂覆分散体接触。以这种方式,90-95%的胶状活化涂层颗粒可以沉积在蜂窝体的孔隙中,使得流动通道的横截面几乎没有由于涂层而降低,并且因此背压力仅稍有增加。
近年来,已经开发了具有显著增加的60-65%的孔隙率和10-20μm平均孔径的陶瓷蜂窝体。这里的目的是使得通道壁能够渗入催化剂颗粒,使得颗粒能够不仅沉积在通道表面作为层而且沉积在壁的孔隙系统中。因此对于相当量的催化剂,可以获得较低的层厚,或者反过来,在相等的催化剂层厚下具有较高的负载浓度[Tao等,SAE 2004-01-1293]。
为了涂覆蜂窝体,通常将催化活性的、水不溶的、粉状组分悬浮在水或有机液体中并研磨,然后通过将蜂窝体浸入该悬浮体中、通过将悬浮体倾倒其上或者通过吸入或泵入悬浮体对蜂窝体进行涂覆。
如果这里使用上述的新开发的多孔蜂窝体,部分催化活性物质实际上渗入蜂窝体的孔隙系统并沉淀在此。然而,上述方法不能使得蜂窝体的孔隙完全填充和由此的最优利用。
发明内容
本发明的目的是提供涂布多孔蜂窝体的方法,该方法使得以定义的方式用催化剂涂布流动通道的几何表面以及通道壁的孔隙。该目的是为了增加蜂窝体的壁中的催化活性成分的量,以使得用等质量的催化剂涂覆后的背压力行为最优化,或者为了在涂覆后相当的背压力行为下增加活性质量。
该方法使用陶瓷蜂窝体,所述陶瓷蜂窝体具有从进口端面到出口端面贯穿其中的由通道壁彼此分隔的平行的流动通道,所述通道壁具有开放孔隙结构。使用含有悬浮在载液中的固体的催化剂悬浮体进行涂覆。该方法特征在于在进口端面和出口端面,流动通道是交替地暂时封闭,使得催化剂悬浮体从进口面到出口面通过蜂窝体,并且暂时关闭的流动通道随后重新打开。
为了实现本发明,术语蜂窝体是指其流动通道在两端打开的流通蜂窝体。根据本发明,这些流动通道在进口和出口端面暂时地交替封闭以进行涂覆。这与其流动通道在进口和出口端面是永久性地交替关闭的壁流蜂窝体不同。
与传统的蜂窝体涂覆方法不同,本发明方法在涂覆工艺中强制涂覆悬浮体流经通道壁材料的孔隙系统。以这种方式,孔隙表面以目标方式被涂覆。依赖于涂覆悬浮体中固体的粒度分布和蜂窝体的陶瓷材料的平均孔径,这导致涂覆悬浮体或多或少所谓的滤过。因此通过适当选择粒度分布,可以以定义的方式设定沉积在孔隙中的涂覆悬浮体与沉积在通道壁上的涂覆悬浮体的质量比率。然而,优选用催化剂组分尽可能完全地填充通道壁的孔隙,以使得在理想涂层浓度下,壁表面涂层尽可能少。在适当低的涂层浓度下,甚至可以在孔隙中容纳所有的催化剂组分。
催化剂悬浮体可以被抽吸通过或泵过蜂窝体。另外,可以将蜂窝体浸泡在催化剂悬浮体中或者将催化剂悬浮体倾倒其上,只要保证在该工艺中涂覆悬浮体通过通道壁。
利用已知的用于制备交替封闭的壁流过滤器的方法实现流动通道的暂时交替封闭。如在壁流过滤器的情况下,暂时封闭的厚度限制为几毫米。
密封组分(sealing composition)没有任何限制。它们仅需要能够通过已知的方法被引入流动通道中并在涂覆蜂窝体的通常工作温度下被固化。蜂窝体通常在室温下涂覆。合适的密封组分有,例如,能够被溶剂溶出或者可以热分解或化学反应的组分,其在升温下(优选大于80℃)熔化或蒸发。具体地,后者的种类包括能够或者被燃烧或者成灰的有机密封组分。这种类型的合适组分有,例如,可以燃烧的水不溶性的填料,例如天然或合成的蜡,特别是固体石蜡,或者聚合物如聚乙烯蜡。优选熔点大于80℃的蜡。
适合用于本发明方法的蜂窝体是通常具有开放孔隙率的完全多孔蜂窝体。依赖于平均孔尺寸,涂覆悬浮体的固体需要具有相应小的颗粒直径。在平均孔尺寸为3-10μm的情况下,优选使用具有在胶态范围的平均粒径(<1μm)。然而,平均粒度d50在3-5μm或1-3μm的固体也是适合的。然而,也可以使用具有宽粒度范围的固体或者具有多峰粒度分布的固体。然后,在涂布中发生过滤:具有小粒径的颗粒沉积在蜂窝体的孔隙中,而较大的颗粒沉积在通道壁上。
然而,优选使用孔隙率为30-90%和平均孔隙直径为10-50μm的高度多孔的蜂窝体。
与普通蜂窝体相比,在通道表面以相当的层厚或者以流动通道的相当的水压直径下,本发明的方法使得更多的催化活性组分施加到载体上。
附图说明
以下实施例以及附图1-5说明本发明,附图表示:
图1是基于按照对比实施例1的传统涂覆蜂窝体的横截面的照片的图;
图2是图1的部分II;
图3是基于按照本发明的实施例1涂覆的蜂窝体的横截面的照片的图;
图4是图3的部分IV;
图5是三种蜂窝体的作为流量函数的背压力:
A)未涂覆蜂窝体,
B)根据本发明涂覆的蜂窝体,
C)传统涂覆的蜂窝体。
具体实施方式
实施例1
用固体石蜡交替封闭堇青石蜂窝体的流动通道。该蜂窝体的直径为14.4cm,长为15.24并且单元密度为46.5cm-2,通道壁的厚度为0.3mm。材料的孔隙率为65%,平均孔隙直径为22μm。
蜂窝体用传统的包含其上沉积了1.5重量%的五氧化二钒和9.3重量%的钨的二氧化钛粉的SCR催化剂涂覆。为此,将氧化钛粉悬浮在水中并用Dyno磨研磨至平均颗粒直径d50小于1μm且d90小于3μm。将该悬浮体泵过蜂窝体并在过滤器后侧用真空装置吸掉多余的活化涂层。重复该步骤一次使得该蜂窝体涂布的催化剂量为240g/L蜂窝体体积。涂覆后,将蜂窝体干燥并煅烧使得流动通道的交替石蜡密封熔化并燃烧。
对比实施例1
为了对比,将没有流动通道的前期交替封闭的与实施例1相同的蜂窝体用催化剂悬浮体涂覆,干燥并煅烧。涂覆后的催化剂质量是234g/L。
为了检测层厚度分布,制备催化剂的横截面并在扫描电子显微镜下检测。相应照片的图显示于图1-4。
图1显示了以对比实施例1描述涂覆的蜂窝体(1)的横截面。图2显示了图1的部分II的放大。参考数字(2)表示蜂窝体的流动通道并且(3)表示其具有孔隙(4)的堇青石结构。事实上所有的催化剂材料作为涂层(5b)存在于通道壁上。仅小部分渗入到通道壁的表面区域(5a)的堇青石结构的孔隙中。
图3和图4显示了对于以实施例1描述的涂覆催化剂涂覆相应于图1和2的横截面。由于涂覆悬浮体被泵过界定流动通道的通道壁,在堇青石结构的孔隙中的通道壁的内部(5c)和通道壁的表面区域(5a)都充满了催化剂材料。由于全部催化剂材料不可能被容纳在通道壁的孔隙中,进一步的涂覆材料(5b)(以约240g/L的选定涂层浓度)存在于通道壁上。
实施例2
为了测量根据本发明的蜂窝体以及传统涂覆蜂窝体的背压力,两个另外的与上述实施例具有相同尺寸的蜂窝体用类似于实施例1和对比实施例1的方法用离子交换沸石涂覆。根据本发明的涂覆蜂窝体的涂覆浓度为330g/L蜂窝体体积,并在传统涂覆蜂窝体上的涂覆浓度为327.5g/L。
以作为经过该体的空气流量的函数测定这些蜂窝体引起的背压力。同样测量未涂覆蜂窝体以对比。这些测量的结果显示于图5。曲线A为未涂覆蜂窝体的背压力,曲线B为根据本发明涂覆的蜂窝体的背压力,曲线C为传统涂覆的蜂窝体的背压力。
根据本发明涂覆的蜂窝体显示了比传统涂覆的蜂窝体明显较低背压力。尽管在大于300g/L的选定的涂覆浓度下,仅小部分的涂覆组分可以被通道壁中的孔隙吸收,然而这对背压力具有非常积极的作用。
Claims (9)
1.陶瓷蜂窝体的催化涂覆方法,所述陶瓷蜂窝体具有从入口端面到出口端面贯穿于所述蜂窝体的由通道壁彼此分隔的平行流动通道,所述通道壁具有开放孔隙结构,其中利用包含悬浮在载液中的固体的催化剂悬浮体进行涂覆,其特征在于,所述流动通道在进口端面和出口端面交替地暂时封闭,使得所述催化剂悬浮体从进口面到出口面流经所述蜂窝体,并且随后所述交替封闭的流动通道被再次打开。
2.如权利要求1的方法,其特征在于,所述催化剂悬浮体被抽吸或泵过所述蜂窝体。
3.如权利要求1的方法,其特征在于,将所述蜂窝体浸入催化剂悬浮体或将所述催化剂悬浮体倾倒在所述蜂窝体上。
4.如权利要求2或3的方法,其特征在于,所述流动通道被密封组分交替封闭,所述密封组分在涂覆蜂窝体的通常工作温度下是固体,且在升温下熔化或蒸发,能够被溶剂溶出,能够被热分解或能化学反应。
5.如权利要求4的方法,其特征在于,用作密封组分的是具有大于80℃的熔点并在煅烧涂覆的蜂窝体的过程中燃烧的天然或合成蜡。
6.如权利要求1的方法,其特征在于,所述蜂窝体的孔隙率为30%-90%,并且平均孔隙直径为10μm-50μm。
7.如权利要求1的方法,其特征在于,所述悬浮体的固体的平均粒度d50为3μm-5μm。
8.如权利要求1的方法,其特征在于,所述悬浮体的固体的平均粒度d50为1μm-3μm。
9.如权利要求1的方法,其特征在于,所述悬浮体的固体的平均粒度d50为小于1μm。
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2005
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2006
- 2006-11-22 US US12/158,843 patent/US8278236B2/en not_active Expired - Fee Related
- 2006-11-22 WO PCT/EP2006/011152 patent/WO2007073807A2/de active Application Filing
- 2006-11-22 EP EP06818705.3A patent/EP1965917B1/de not_active Not-in-force
- 2006-11-22 CN CN200680049017XA patent/CN101370583B/zh active Active
- 2006-11-22 BR BRPI0620619-0A patent/BRPI0620619A2/pt not_active Application Discontinuation
- 2006-11-22 JP JP2008546160A patent/JP5049293B2/ja not_active Expired - Fee Related
- 2006-11-22 RU RU2008129724/04A patent/RU2412000C2/ru not_active IP Right Cessation
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- 2008-06-13 ZA ZA200805206A patent/ZA200805206B/xx unknown
- 2008-06-23 KR KR1020087015226A patent/KR101375553B1/ko active IP Right Grant
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Cited By (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102753267A (zh) * | 2010-02-09 | 2012-10-24 | 乌米科雷股份两合公司 | 涂覆方法和装置 |
CN104411403A (zh) * | 2012-06-12 | 2015-03-11 | 喜星触媒株式会社 | 载体空隙埋没型scr催化剂结构 |
CN103495346A (zh) * | 2013-10-09 | 2014-01-08 | 山东工业陶瓷研究设计院有限公司 | 含尘有毒高温气体处理用陶瓷膜及其制备方法 |
CN103495346B (zh) * | 2013-10-09 | 2015-09-02 | 山东工业陶瓷研究设计院有限公司 | 含尘有毒高温气体处理用陶瓷膜及其制备方法 |
CN108348852A (zh) * | 2015-11-02 | 2018-07-31 | 喜星触媒株式会社 | 载体界面孔隙集中埋没型scr催化剂结构体 |
CN110869124A (zh) * | 2017-07-06 | 2020-03-06 | 优美科股份公司及两合公司 | 涂覆设备和方法 |
CN110869124B (zh) * | 2017-07-06 | 2023-03-31 | 优美科股份公司及两合公司 | 涂覆设备和方法 |
Also Published As
Publication number | Publication date |
---|---|
DE102005062317A1 (de) | 2007-07-05 |
EP1965917B1 (de) | 2015-08-12 |
BRPI0620619A2 (pt) | 2011-11-16 |
WO2007073807A2 (de) | 2007-07-05 |
RU2008129724A (ru) | 2010-02-20 |
US20120321842A1 (en) | 2012-12-20 |
KR101375553B1 (ko) | 2014-03-24 |
KR20080080328A (ko) | 2008-09-03 |
RU2412000C2 (ru) | 2011-02-20 |
US8278236B2 (en) | 2012-10-02 |
US20090305874A1 (en) | 2009-12-10 |
ZA200805206B (en) | 2009-03-25 |
CN101370583B (zh) | 2010-06-16 |
JP2009521303A (ja) | 2009-06-04 |
DE102005062317B4 (de) | 2008-08-21 |
JP5049293B2 (ja) | 2012-10-17 |
WO2007073807A3 (de) | 2007-08-23 |
EP1965917A2 (de) | 2008-09-10 |
US9278347B2 (en) | 2016-03-08 |
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