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CN101626832A - 钯-铑单层催化剂 - Google Patents

钯-铑单层催化剂 Download PDF

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CN101626832A
CN101626832A CN200880007401A CN200880007401A CN101626832A CN 101626832 A CN101626832 A CN 101626832A CN 200880007401 A CN200880007401 A CN 200880007401A CN 200880007401 A CN200880007401 A CN 200880007401A CN 101626832 A CN101626832 A CN 101626832A
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cerium
oxide
zirconium mixed
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R·克林曼
M·罗伊茨
D·林德尼尔
J-M·瑞切尔
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Abstract

本发明描述了一种用于净化内燃机废气并具有出色活性和温度稳定性的单层三效催化剂。所述催化剂包括活性氧化铝、第一铈/锆混合氧化物和第二铈/锆混合氧化物。第一铈/锆混合氧化物具有比第二铈/锆混合氧化物更高的氧化锆含量。第一铈/锆混合氧化物用铑活化并且第二铈/锆混合氧化物用钯活化。

Description

钯-铑单层催化剂
技术领域
本发明涉及三效催化剂，其对于净化内燃机废气具有出色的催化活性和老化稳定性。
背景技术
三效催化剂广泛应用于净化在基本化学计量条件下工作的内燃机的废气。它们能将三种来自发动机的重要有害物质，即烃类、一氧化碳和氧化氮同时转化为无害的组分。经常使用双层催化剂，其能实现不同催化过程的分离并由此达到两层中催化效果的最佳协调。这种催化剂例如描述于EP0885650和EP1046423中。
双层催化剂具有的缺点是它们的生产比单层催化剂更贵。此外，双层催化剂与单层催化剂相比，倾向于带来升高的废气背压，这以内燃机的功率和它的燃料消耗为代价。因此人们一直以来已试图通过单层催化剂来尽可能不打折扣地产生双层催化剂的良好催化特性。单层三效催化剂例如公开于WO98/09726、EP1138382和EP1541220。
发明描述
对于减少内燃机排放的不断增加的要求，需要催化剂在催化活性、老化稳定性和生产成本方面不断发展。因此本发明的目标是提供一种催化剂，其相对于现有技术的催化剂具有在更低生产成本下的进一步降低的起燃温度和改进的温度稳定性。
该目标由根据权利要求所述的催化剂实现。该催化剂在陶瓷或金属构成的惰性催化剂载体上具有单个催化活性层。该催化剂的特征是其包括活性氧化铝和第一和第二铈/锆混合氧化物，其中所述第一铈/锆混合氧化物用铑活化并具有比用钯催化活化的第二铈/锆混合氧化物更高的氧化锆含量。
在本发明的上下文中，“载体材料用催化活性元素活化”的表述表示将催化活性元素以高分散的形式被沉积在可通过浸渍进入的载体材料的表面上。
由于所述特性的组合，该催化剂具有很好的起燃性能并拥有很高的温度稳定性。此外，该催化剂具有低的废气背压并且其生产成本比相应的双层催化剂的生产成本更低。
活性氧化铝和铈/锆混合氧化物作为粉状固体引入到涂层。两种混合氧化物可以用至少一种选自下组的元素的氧化物来稳定化而改进其温度稳定性，所述元素选自铁、锰、锡、钛、硅、钇、镧、镨、钕、钐及其混合物。掺杂元素的量以氧化物计，优选1至15并且尤其是5至10重量％，基于经稳定化的混合氧化物的总重量。
所述第一铈/锆混合氧化物的氧化铈对氧化锆的重量比优选为0.5至0.1，所述第二铈/锆混合氧化物的氧化铈对氧化锆的重量比为0.8至1.2。优选这些材料的比表面积是50至100m2/g。
活性氧化铝可以用1至10重量％的氧化镧稳定化，基于氧化铝加氧化镧的总重量计。当活性氧化铝和铈/锆混合氧化物另外用氧化锶和/或氧化钡浸渍时可以使所述催化剂的温度稳定性得到进一步改进。
通常地，所述催化剂载体是具有体积V的蜂窝体，其具有平行的内燃机废气的流道，该流道壁面用催化剂涂覆并且基于蜂窝体的体积，钯浓度是0.1至10g以及铑的浓度是0.01至1g。在特定的催化剂实施方式中，所述第一铈/锆混合氧化物除了铑也可以用钯催化活化。在另一实施方案中，两种铈/锆混合氧化物也都可以用铂活化。
实际要使用的贵金属浓度取决于所需的有害物质转化率。本文报道的最高浓度值是为遵守SULEV-车辆的严格排放标准所必需的(SULEV＝特超低排放车辆)。
为了用催化活性层涂覆催化剂载体，必须制备涂覆悬浮液，其直接包括所期望的催化层的所有组分，或包括这些组分的前体且它们通过层的最后煅烧转化为它们的最终形式。
两种铈/锆混合氧化物可以用铑或钯的前体化合物通过已知的浸渍方法分别涂覆。优选使用水溶性化合物硝酸铑和硝酸钯。经如此预涂覆的材料随后可以和氧化铝一起悬浮在水中。在湿态下碾磨该悬浮液直到悬浮液的固体具有大约3至5μm的平均粒度。然后，用该悬浮液按照已知的方法涂覆蜂窝体，将其干燥并煅烧。该制备方法保证了钯和铑彼此分开地沉积于不同的载体材料上。
在本发明优选的实施方案中，首先将所述第一铈/锆混合氧化物悬浮于水中。向该悬浮液中加入铑的前体化合物溶液，优选硝酸铑。随后，用碱，例如四乙基氢氧化铵(TEAH)将该悬浮液的pH值升至大约6，以使硝酸铑沉淀。然后，将所述第二铈/锆混合氧化物悬浮于该悬浮液中并加入钯的前体化合物溶液。由此，悬浮液的pH值降低至强酸性范围。通过重新加入碱将pH值又回升至大约6并因此使钯沉淀至两种混合氧化物上。此后，向该悬浮液中加入氧化铝并如前所述地最后碾磨悬浮液并加载至催化剂载体上。如此制备的催化剂不包含任何碱土金属。
另选地，可以首先预置氢氧化钡和/或氧化锶的碱性溶液。将所述第一铈/锆混合氧化物加入该溶液并悬浮在该溶液中。此后，向该悬浮液中加入例如硝酸铑溶液，在此由于悬浮液的碱性使铑沉淀至第一铈/锆混合氧化物上。随后，将所述第二铈/锆混合氧化物加入该悬浮液，接着加入硝酸钯溶液。最后，向该悬浮液中加入氧化铝并且如前所述地碾磨悬浮液并将其加载至催化剂载体上。通过使用氢氧化钡或氢氧化锶作为使硝酸铑沉淀的碱，氧化钡或氧化锶在最后煅烧之后留在涂层中。
根据最后两种制备方案制得的催化剂中，铑和钯都存在于第一铈/锆混合氧化物的颗粒上。
下文根据实施例和附图详细地说明本发明。所述附图如下：
图1：现有技术的催化剂和根据不同实施方案的催化剂的起燃温度比较
图2：图1的催化剂的最大转化率
对比例
根据EP1541220制备催化剂。为此，首先制备硫酸钡的水悬浮液。向该悬浮液中加入1重量％的硝酸并由此将pH值降低至大约5。此后，加入用3重量％氧化镧稳定的γ-氧化铝，随后加入氧化锆含量为50重量％的铈/锆混合氧化物，并在加入过程中用硝酸使pH保持大致恒定。加入10重量％蔗糖之后，碾磨该悬浮液，随后加入硝酸钯和硝酸铑。熟化一小时后，用该悬浮液涂覆堇青石的蜂窝体，将其干燥并煅烧。该蜂窝体具有93cm-2的蜂窝(Zell-)密度，14.4cm的直径和10.2cm的长度。所得的催化剂包含下述涂覆量：
80    g/l用镧稳定的氧化铝
75    g/l铈/锆混合氧化物(70重量％的氧化锆)
0.18  g/l铑(在所有固体组分上)
0.88  g/l钯(在所有固体组分上)
实施例1
根据本发明的一种催化剂制备如下：
将富含锆的铈/锆混合氧化物(70重量％的氧化锆)悬浮在水中，随后将硝酸铑搅拌加入该悬浮液。用TEAH使该悬浮液的pH值回升至大约6。此后，将含有50重量％氧化锆的铈/锆混合氧化物加入该悬浮液，并将硝酸钯搅拌加入该悬浮液。向该悬浮液中加入用3重量％氧化镧稳定的γ-氧化铝之前，用TEAH将pH值再升至6。随后，碾磨该悬浮液并如对比例所述以此涂覆蜂窝体，将其干燥并煅烧。所得的催化剂包含下述涂覆量：
80    g/l用镧稳定的氧化铝
35    g/l第一铈/锆混合氧化物(70重量％的氧化锆)
40    g/l第二铈/锆混合氧化物(50重量％的氧化锆)
0.18  g/l铑(在第一铈/锆混合氧化物上)
0.88  g/l钯(在在第一和第二铈/锆混合氧化物上)
实施例2
根据本发明另一种催化剂制备如下：
将氢氧化钡溶于水。将含有70重量％氧化锆的铈/锆混合氧化物悬浮于该溶液，并向该悬浮液中加入硝酸铑。此后，将含有50重量％氧化锆的铈/锆混合氧化物分散于该悬浮液，并将硝酸钯搅拌加入该悬浮液。加入氧化铝后，用乙酸将pH值调整至6。最后，碾磨该悬浮液并如对比例所述以此涂覆蜂窝体，将其干燥并煅烧。所得的催化剂包含下述涂覆量：
80    g/l用镧稳定的氧化铝
2     g/l氧化钡
35    g/l第一铈/锆混合氧化物(70重量％的氧化锆)
40    g/l第二铈/锆混合氧化物(50重量％的氧化锆)
0.18  g/l铑(在第一铈/锆混合氧化物上)
0.88  g/l钯(在第一和第二铈/锆混合氧化物上)
催化剂的测试
测试前，使所有催化剂在炉中于985℃下经受热液老化处理持续16小时。
老化后，在发动机测试台上在起燃温度和最大转换率方面来检测催化剂。
图1显示了起燃温度的对比。两种根据本发明的催化剂在老化后比起对比例催化剂具有显著更低的转化有害物质HC(烃类)、CO(一氧化碳)和NOx(氮氧化物)的起燃温度。图2的图表显示采用催化剂所能达到的最大转化率。
所述催化剂在30℃气体温度和345kg/h空气质量流量时具有18.3毫巴背压。该背压低于可类比的双层催化剂的背压约15％。

Claims (9)

1、一种用于净化内燃机废气的三效催化剂，其由在由陶瓷或金属构成的惰性催化剂载体上的单催化活性涂层组成，其特征是，所述催化剂包括活性氧化铝和第一和第二铈/锆混合氧化物，其中所述第一铈/锆混合氧化物用铑活化并具有比用钯催化活化的所述第二铈/锆混合氧化物更高的氧化锆含量。
2、如权利要求1所述的三效催化剂，其特征是，另外用氧化锶或氧化钡在其表面上涂覆氧化铝和铈/锆混合氧化物。
3、如权利要求1所述的三效催化剂，其特征是，所述铈/锆混合氧化物各自用基于混合氧化物总重量计的1至15重量％的稀土元素氧化物稳定化，其中所述稀土元素氧化物在每种情形下选自铁、锰、锡、钛、硅、钇、镧、镨、钕、钐及其混合物。
4、如权利要求3所述的三效催化剂，其特征是，所述第一铈/锆混合氧化物的氧化铈对氧化锆的重量比是0.5至0.1，并且所述第二铈/锆混合氧化物的氧化铈对氧化锆的重量比是0.8至1.2。
5、如权利要求4所述的三效催化剂，其特征是，所述活性氧化铝在每种情形下用基于氧化铝总重量计1至10重量％的氧化镧稳定化。
6、如权利要求1所述的三效催化剂，其特征是，所述催化剂载体是具有体积V的蜂窝体，其具有平行的内燃机废气流道，该流道壁面用所述三效催化剂涂覆并且基于蜂窝体的体积，钯浓度是0.1至10g，以及铑的浓度是0.01至1g。
7、如权利要求6所述的三效催化剂，其特征是，所述第一铈/锆混合氧化物除了铑还用钯催化活化。
8、如权利要求7所述的三效催化剂，其特征是，所述第一和第二铈/锆混合氧化物除了钯还用铂催化活化。
9、前述权利要求之一所述的三效催化剂作为配备有汽油发动机的机动车的靠近发动机的起始催化剂或底盘区域中的主催化剂用于净化发动机废气的用途。
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