CN108698035B - 制备催化整料的方法 - Google Patents

制备催化整料的方法 Download PDF

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CN108698035B
CN108698035B CN201780011931.3A CN201780011931A CN108698035B CN 108698035 B CN108698035 B CN 108698035B CN 201780011931 A CN201780011931 A CN 201780011931A CN 108698035 B CN108698035 B CN 108698035B
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sol solution
face
substrate
colloidal
compounds
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CN108698035A (zh
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K·约翰森
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Topsoe AS
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Haldor Topsoe AS
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  • Chemical & Material Sciences (AREA)
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  • Catalysts (AREA)
  • Dispersion Chemistry (AREA)
  • Exhaust Gas Treatment By Means Of Catalyst (AREA)
  • Exhaust Gas After Treatment (AREA)
  • Processes For Solid Components From Exhaust (AREA)
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Abstract

一种通过将包含催化活性材料和金属氧化物催化剂载体或其前体的溶胶溶液毛细抽吸到整体式基材的孔中来制备催化整体式主体或催化颗粒过滤器的方法。

Description

制备催化整料的方法
本发明涉及催化的整体式基材。具体地，本发明提供了通过将包含催化活性材料和金属氧化物催化剂载体或其前体的溶胶溶液毛细抽吸到整体式基材的孔中来制备催化整体式基材(任选地催化颗粒过滤器)的改进的方法。
催化整料通常用于清洁发动机废气，以催化去除废气中的有毒化合物。为了在来自贫燃发动机的废气中以适度的过滤效率去除颗粒物质，催化整料用作流通式过滤器。
最典型地，用于机动车应用的具有高过滤效率的过滤器是由整体式蜂窝体组成的壁流式过滤器，其中颗粒物质被捕获在蜂窝结构的分隔壁上或其中。这些过滤器具有由透气分隔壁隔开的多个纵向流动通道。气体入口通道在其气体入口侧打开并在相对的出口端处封闭，而气体出口通道在出口端打开并且在入口端处封闭，使得进入壁流式过滤器的气流在进入出口通道之前被迫通过分隔壁。
除了捕获烟灰颗粒之外，颗粒过滤器通常用在燃烧烟灰和去除氮氧化物(NOx)、一氧化碳和未燃烧的烃中具有活性的催化剂催化，烟灰、氮氧化物(NOx)、一氧化碳和未燃烧的烃为代表健康和环境风险的化合物，且必须从废气中减少或去除。
在氧气或由一氧化氮形成的二氧化氮存在下燃烧掉烟灰并且进一步去除或减少NOx、一氧化碳和烃成无害化合物中具有活性的催化剂本身是本领域已知的。
专利文献公开了许多清洁***，其包括用于从发动机废气中去除有害化合物的单独的催化剂单元。
在本领域中还已知的是用催化剂涂布的废气颗粒过滤器，所述催化剂催化烃和颗粒物质的氧化以及通过与作为其本身或作为其前体加入到废气中的氨反应而将NOx选择性催化还原(SCR)。
整体式或蜂窝状整体式基材的洗涂通常是通过将浆料倾倒或泵送到整体式基材的通道中进而在基材中粘着浆料或通过将基材的一侧浸渍到洗涂浆料中并任选地在对侧施加真空来进行。可以通过加压空气或真空从一侧除去洗涂层的剩余物，但是将易于除去壁内部的洗涂层。
在用洗涂层涂布后，将基材干燥并最后煅烧以活化涂层中的催化组分。
洗涂基材的问题在于其影响催化组分在过滤器壁中、在壁上的洗涂层的厚度中和沿着整料的通道轴的浓度梯度。因此，其对成品催化剂的质量具有潜在影响。
用颗粒悬浮液洗涂壁流式过滤器特别难以控制，因为一些通道在端面关闭，并且用于确保均匀涂层分布的气刀受到过滤器壁的阻碍。
与已知技术相比，本发明提出了一种用于涂布整体式基材的更简单的方法，其通过使用包含作为催化剂载体前体和金属催化剂前体的所有催化剂成分的溶胶溶液，并通过毛细作用力将该溶胶溶液吸入整体式基材的壁的孔中。
在本发明的上下文中，溶胶溶液是固体颗粒在水溶性化合物溶液中的悬浮液的混合物。
本发明提供了一种用于制备催化整料的方法，包括以下步骤：
a)提供多孔整体式基材，其具有由透气分隔壁隔开的多个纵向流动通道，所述整体式基材具有第一端面和与第一端面具有一定距离的第二端面；
b)在容器中提供至少对应于透气分隔壁的孔体积的量的溶胶溶液，该溶胶溶液包含一种或多种催化活性化合物的水溶性或胶体前体和一种或多种金属氧化物催化剂载体化合物的水溶性或胶体前体，一种或多种前体中的至少一种是胶体，并且一种或多种前体中的至少一种是水溶性的；
c)将整体式基材基本上垂直放置在容器中，第一或第二端面浸入溶胶溶液中；
d)仅通过毛细作用力将溶胶从浸入溶胶溶液的端面吸入到可渗透分隔壁的孔中，在可渗透分隔壁中到达距离浸入溶胶溶液的端面的预定距离，而没有施加真空或压力；
e)随后将整体式基材翻转，并将整体式基材基本上垂直放置在容器中，使相对的端面浸入溶胶溶液中；
f)仅通过毛细作用力将溶胶从浸入溶胶溶液的相对的端面吸入到可渗透分隔壁的孔中，而没有施加真空或压力；和
g)干燥和煅烧如此涂布的整体式基材。
除了提供更容易的涂布方法之外，本发明的另一个优点是在干燥和煅烧之后仅涂布过滤器中的孔的表面，这导致以在催化整料上降低的压降下运行如此制备的催化整料，特别是当催化整料为壁流式过滤器时。
溶胶溶液通常由液体分散剂(通常是酸的水溶液)中的二氧化铈、氧化铝、二氧化钛、氧化锆、二氧化硅溶胶的金属氧化物前体与溶解的催化活性金属前体(优选钯、铂、铑、钒、钼、钨的化合物及其混合物)的组合来配制。对于不同的前体，pH可以是酸性的、碱性的或中性的，这取决于实际溶胶的pH稳定性。
溶胶溶液的制备涉及将单体转化为胶体溶液，其作为金属氧化物催化剂载体和催化活性金属化合物的离散颗粒的前体。典型的前体是金属硝酸盐和稳定化的金属氢氧化物或羟基氧化物。铵化合物是典型的稳定剂。将溶胶溶液的酸度调节至其中溶胶是稳定的并且不形成凝胶的pH值。
胶体前体的尺寸在1-1000nm之间，优选在1-100nm之间。胶体前体的尺寸显著小于整料壁中的孔径直径，即通常为1-30μm。
为了提供正确量的溶胶溶液，在通过本领域已知的常规方法涂布整体式基材之前测量整体式基材的孔体积。
通过根据本发明的方法，仅通过毛细作用力将溶胶溶液吸入并且吸附在整体式基材的孔中，在基材壁上从浸入溶胶溶液的端面向上到达整体式基材的一定距离或高度，而没有在端面上施加任何必须的辅助外力，如真空或压力。将溶胶溶液吸入到距离浸入溶胶溶液的端面的一定距离。基材的润湿长度为基材的润湿末端至润湿前端的距离，其取决于基材的孔隙率。润湿长度也与液体-空气表面张力成比例。液体-空气张力在温度升高时降低。因此，优选在低温下，最优选在15至30℃之间，进行润湿处理。
溶胶溶液的吸附速率随时间而降低。当吸附速率大幅降低或为零时，将基材翻转，并将与先前孔填充阶段的面相对的端面浸入溶胶溶液中。
为了确保整体式基材的基本上整个长度被润湿，即基材壁中的所有孔都用溶胶溶液填充，优选在半壁孔填充时翻转基材，其通过填充基材壁的一半长度中的孔所需的时间或通过计算填充基材壁的一半长度中的孔的溶胶溶液的所需量来确定。
吸入步骤可以重复一次或多次。
完成孔填充步骤后，将整体式基材干燥并从孔中蒸发水。
如上文已经描述的，干燥步骤将催化材料和载体材料的细颗粒的量基本上集中在整体式基材的孔表面上。
干燥优选通过施加微波来进行。
最后，通过煅烧将前体化合物转化为活性催化化合物和金属氧化物催化剂载体化合物来活化干燥的整体式基材。
如上文已经描述的，根据本发明的方法特别用于用溶胶溶液填充壁流式过滤器的壁中的孔。
在所有情况下，整体式基材可以由多孔陶瓷材料或多孔金属材料制成。
优选地，整体式基材由堇青石、钛酸铝、莫来石或碳化硅制成。
实施例
在稀硝酸中制备包含氧化铈、氧化锆、钯和铂的前体的水溶胶溶液。前体的含量和类型总结在下表1中。
表1
化合物 量/g
水 2343.3
Ce(NO<sub>3</sub>)<sub>3</sub>溶液 2167.4
Zr-溶胶 499.9
Pd(NH<sub>3</sub>)<sub>4</sub>(HCO<sub>3</sub>)<sub>2</sub> 0.97
Pt(NH<sub>3</sub>)<sub>4</sub>(HCO<sub>3</sub>)<sub>2</sub> 6.29
HNO<sub>3</sub>(65％) 0.9
总计 5018.7
总体积为17.03L、高度为30.5cm且孔体积为2810ml的壁流式过滤器堇青石基材
Figure BDA0001768317060000041
对应于3100g上述溶胶溶液，如对溶胶溶液的总密度(g/ml)和壁流式过滤器的总孔体积(ml)所计算的。
将3300g上述溶胶溶液装入盘中。然后，将壁流式过滤器的一个端面放入盘中，并通过重量监测盘的重量。在吸入一半量的溶胶溶液后，将壁流式过滤器翻转并将另一个端面放入盘中。在计算量的溶胶溶液被吸入后，将如此涂布的壁流式过滤器在120℃下干燥并在600℃的温度下煅烧。涂布过程在25℃的温度下进行。

Claims (13)

1.一种用于制备催化整料的方法，包括以下步骤：
a)提供多孔整体式基材，其具有由透气分隔壁隔开的多个纵向流动通道，所述整体式基材具有第一端面和与第一端面具有一定距离的第二端面；
b)在容器中提供至少对应于透气分隔壁的孔体积的量的溶胶溶液，该溶胶溶液包含一种或多种催化活性化合物的水溶性或胶体前体和一种或多种金属氧化物催化剂载体化合物的水溶性或胶体前体，一种或多种前体中的至少一种是胶体，并且一种或多种前体中的至少一种是水溶性的；
c)将整体式基材基本上垂直放置在容器中，第一或第二端面浸入溶胶溶液中；
d)仅通过毛细作用力将溶胶从浸入溶胶溶液的端面吸入到可渗透分隔壁的孔中，在可渗透分隔壁中到达距离浸入溶胶溶液的端面的预定距离，而没有施加真空或压力；
e)随后将整体式基材翻转，并将整体式基材基本上垂直放置在容器中，使相对的端面浸入溶胶溶液中；
f)仅通过毛细作用力将溶胶从浸入溶胶溶液的相对的端面吸入到可渗透分隔壁的孔中，而没有施加真空或压力；和
g)干燥和煅烧如此涂布的整体式基材。
2.如权利要求1所述的方法，其中预定距离是端面之间的整个距离的约一半。
3.如权利要求1所述的方法，其中预定距离对应于容器中溶胶溶液的量的约一半。
4.如权利要求1至3中任一项所述的方法，其中溶胶溶液的吸入在15至30℃的温度下进行。
5.如权利要求1至3中任一项所述的方法，其中整体式基材是壁流式过滤器。
6.如权利要求1至3中任一项所述的方法，其中一种或多种催化活性化合物的水溶性或胶体前体选自钯、铂、铑、钒、钼、钨的化合物及其混合物。
7.如权利要求1至3中任一项所述的方法，其中一种或多种金属氧化物催化剂载体化合物的水溶性或胶体前体选自铝、钛、铈、锆、硅的化合物及其混合物。
8.如权利要求1至3中任一项所述的方法，其中多孔整体式基材是金属的或陶瓷的。
9.如权利要求1至3中任一项所述的方法，其中多孔整体式基材是堇青石、钛酸铝、莫来石或碳化硅。
10.如权利要求1至3中任一项所述的方法，其中一种或多种催化活性化合物的胶体前体和一种或多种金属氧化物催化剂载体化合物的胶体前体的粒度为1-1000nm。
11.如权利要求10所述的方法，其中胶体前体的粒度为1-100nm。
12.如权利要求1至3中任一项所述的方法，其中将步骤d、e和f重复一次或多次。
13.如权利要求1至3中任一项所述的方法，其中步骤中的干燥通过施加微波来进行。
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