CN108136372B - 整料式蜂窝状氧化催化剂及其制备方法 - Google Patents
整料式蜂窝状氧化催化剂及其制备方法 Download PDFInfo
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- 230000003647 oxidation Effects 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title abstract description 3
- 239000000463 material Substances 0.000 claims abstract description 27
- GNTDGMZSJNCJKK-UHFFFAOYSA-N divanadium pentaoxide Chemical compound O=[V](=O)O[V](=O)=O GNTDGMZSJNCJKK-UHFFFAOYSA-N 0.000 claims abstract description 26
- 229910052751 metal Inorganic materials 0.000 claims abstract description 22
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- 239000002002 slurry Substances 0.000 claims description 15
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 14
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- 238000000576 coating method Methods 0.000 claims description 9
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- 229910002651 NO3 Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
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- TXKMVPPZCYKFAC-UHFFFAOYSA-N disulfur monoxide Inorganic materials O=S=S TXKMVPPZCYKFAC-UHFFFAOYSA-N 0.000 description 1
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- XTQHKBHJIVJGKJ-UHFFFAOYSA-N sulfur monoxide Chemical compound S=O XTQHKBHJIVJGKJ-UHFFFAOYSA-N 0.000 description 1
- 229910001935 vanadium oxide Inorganic materials 0.000 description 1
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Abstract
本发明涉及一种整料式蜂窝状氧化催化剂及其制备方法，该蜂窝状氧化催化剂具有多个由壁限定的流通式通道，该壁由涂覆有包含惰性粘土材料的芯层的惰性材料构成，该芯层涂覆有顶层，该顶层包含选自铂族金属的至少一种金属和五氧化二钒。
Description
本发明涉及一种用于氧化来自包括燃气轮机和发电厂的固定烟道气源的废气和烟道气中的一氧化碳和挥发性有机化合物(VOC)的整料式蜂窝状催化剂。
本发明特别涉及一种整料式蜂窝状氧化催化剂，该整料式蜂窝状氧化催化剂具有涂覆在整料式蜂窝状基底上的包含惰性粘土材料的芯层和包含一种或多种铂族金属(PGM)的顶层，用于去除在化石燃料如天然气、煤或石油的燃烧中在固定源中形成的烟道气中的一氧化碳和VOC。
本发明还涉及一种制备氧化催化剂的方法，该氧化催化剂具有涂覆在整料式蜂窝状基底上的惰性粘土材料的芯层和在CO和VOC的氧化中有活性的催化材料的顶层。
通过催化氧化去除CO和VOC的方法在本领域中是公知的。
对于诸如CO和VOC氧化的应用，在来自固定源的烟道气清洁中所采用的最典型的氧化催化剂组合物是基于氧化铝负载的铂。
还已知的是，钯促进的氧化钒催化剂提供非常高的CO和VOC氧化活性，以及高的耐硫性。
当存在暴露于高含硫烟道气的风险并且必须使高的硫酸盐排放物和下游设备的结垢和/或使催化剂失活的风险最小化时，这些催化剂是特别优选的。
基于钯的氧化催化剂的优点是，这些催化剂具有相对低的硫氧化活性，这在用于清洁含硫氧化物的烟道气时特别重要。
为了用于来自固定源的气体清洁，将催化剂在整料式蜂窝状基底上形成修补基面涂层(washcoat)，该整料式蜂窝状基底通常由堆叠的陶瓷材料的波纹状片材或非织造玻璃纤维构成，形成具有多个平行的流通式通道的整料式蜂窝状结构。
上述类型的整料式蜂窝状催化剂通常通过用含有催化剂载体材料的修补基面涂层来涂覆整料式蜂窝状基底并用催化活性的金属氧化物的前体的溶液浸渍经涂覆的基底来制备。或者，修补基面涂层也可以含有前体。
通常通过将浆料倾倒入基底的通道中而将浆料捕获(pickup)到基底中，通过将基底一侧浸入修补基面涂层浆料中并任选地在相反侧施加真空，或者通过将修补基面涂层浆料泵送至通道中并任选地施加真空，来进行整料式蜂窝状基底的修补基面涂层的施加。
在涂覆修补基面涂层之后，将基底干燥并最后煅烧以活化涂层中的催化组分。
众所周知，在典型的氧化反应条件下，氧化反应比CO和某些VOC到催化剂壁中的扩散要快得多，并且因此在将昂贵的PGM催化剂材料的分布降低或限制在仅在整料式蜂窝状基底的壁或壁涂层的外表面时，在成本节约方面是有利的。
在通过上述涂覆方法制备的已知氧化催化剂中，PGM催化剂遍布整个壁横截面。因此，分布在壁表面下方的PGM催化剂不参与催化CO和反应性VOC的氧化。
通过本发明，当向基底的壁提供惰性粘土材料的芯层并且在芯层的表面上施加包含PGM的修补基面涂层时，解决了该问题。
我们还发现，当降低PGM在基底上的扩散速率时，PGM的扩散可被消除或大大降低。与将PGM的前体化合物溶解在水性浸渍液体中不同，将前体化合物加入到含有钒化合物的水性浆料中，该钒化合物充当PGM的载体并用于在基底上涂覆惰性粘土芯层。在该水性浆料中，PGM化合物被吸附在经负载的钒化合物颗粒上，并且因此不溶于水性浆料的水相中，否则其会导致不希望的到基底的壁和/或粘土芯层中的扩散。
根据上述发现，本发明提供了一种整料式蜂窝状氧化催化剂，其具有多个由壁限定的流通式通道，该壁由任选地设置有扁平衬里的惰性材料的一个或多个波纹状片材构成，并且涂覆有包含惰性粘土材料的芯层，该芯层涂覆有顶层，该顶层包含选自铂族金属的至少一种金属和五氧化二钒。
根据本发明的催化剂具有这样的优点，其显示出至少与常规整料相同的良好结构稳定性，因为整料式壁的总厚度由于惰性粘土芯层而保留。
本发明额外降低了每单位体积整料的催化剂负载，导致SO2的氧化减少。
根据本发明的催化剂的具体特征是单独的以下特征或其组合：
顶层还包含钨的氧化物和二氧化钛；
选自铂族金属的至少一种金属是钯；
惰性材料的一个或多个波纹状片材和任选的扁平衬里包含缠结的非织造纤维；
缠结的非织造纤维包含玻璃纤维；
惰性粘土材料选自高岭土类、含水硅酸铝、绿泥石类、叶腊石类(pyrophillite)、膨润土或其混合物；
顶层包含0.1至10重量％的五氧化二钒；
顶层包含100至30000ppm重量的钯；
本发明的另一方面是用于制备整料式蜂窝状氧化催化剂的方法，其包括以下步骤：
(a)通过堆叠或卷起任选地设置有扁平衬里的惰性材料的一个或多个波纹状片材来提供具有多个由壁限定的流通式通道的惰性整料式蜂窝状基底；
(b)用包含惰性粘土材料的芯层来涂覆整料式蜂窝状基底；
(c)提供包含选自铂族金属的至少一种金属和五氧化二钒的修补基面涂层；
(d)通过施加步骤(c)中制备的修补基面涂层而用顶层来涂覆芯层；和
(e)煅烧经涂覆的整料式蜂窝状基底。
根据本发明的方法的具体特征是单独的以下特征或其组合：
通过以下步骤制备步骤(c)的修补基面涂层：
(i)粉碎包含五氧化二钒的成品SCR催化剂产物；
(ii)将粉碎的催化剂产物分散在水中并形成浆料；
(iii)添加选自铂族金属的至少一种金属的水溶性前体；
修补基面涂层还包含二氧化钛和钨的氧化物；
包含五氧化二钒的成品SCR催化剂产物还包含二氧化钛和钨的氧化物；
铂族金属是钯；
惰性材料的一个或多个波纹状片材和任选的扁平衬里包含缠结的非织造纤维；
缠结的非织造纤维是玻璃纤维；
惰性粘土材料选自高岭土类、含水硅酸铝、绿泥石类、叶腊石类、膨润土或其混合物；
顶层包含0.1至10重量％的五氧化二钒；
顶层包含100至30000ppm重量的钯；
应当理解，在上文或在以下说明书和权利要求书中使用的术语“惰性材料”和“惰性粘土材料”是指该材料不具有催化活性。
实施例
如下制备在惰性粘土芯上的基于Pd-V2O5-WO3-TiO2的氧化催化剂。
通过将基底浸入高岭土和丁醇的浆料中而用高岭土的芯层来涂覆整料式蜂窝状基底，直到经涂覆的基底的壁厚度为0.4mm，该整料式蜂窝状基底由玻璃纤维制成的多个波纹状片材来制造，每个波纹状片材设置有扁平衬里。然后使如此制备的整料式蜂窝状基底排水10分钟，干燥三天并在N2气氛中在550℃下煅烧两个小时。
具有高岭土芯层的基底用如下制备的修补基面涂层进行涂覆：
通过添加氨水溶液将200g在水中的经破碎和研磨的V2O5-WO3-TiO2SCR催化剂(25质量％)调节至8.5的pH值。向所得浆料中添加以金属计为100ppmw的Pd硝酸盐溶液，直至浆料中达到以干物质计为1000ppmw的Pd。充分混合所得浆料，同时使用氨水溶液将pH调节为8.5，然后添加多糖至浓度为0.1质量％。
将如上制备的具有高岭土的惰性芯层的整料式蜂窝状基底浸入浆料中1.5分钟，然后使浆料从基底排出15分钟。然后将所得的整料式蜂窝状催化剂在400℃下煅烧2小时。
Claims (13)
1.一种整料式蜂窝状氧化催化剂，其具有多个由壁限定的流通式通道，所述壁由任选地设置有扁平衬里的惰性材料的一个或多个波纹状片材构成，并且涂覆有包含惰性粘土材料的芯层，所述芯层涂覆有顶层，所述顶层包含吸附在五氧化二钒上的选自铂族金属的至少一种金属，其中所述顶层包含0.1至10重量％的五氧化二钒和100至30000ppm重量的钯。
2.根据权利要求1所述的整料式蜂窝状氧化催化剂，其中所述顶层还包含二氧化钛和钨的氧化物。
3.根据权利要求1或2所述的整料式蜂窝状氧化催化剂，其中所述选自铂族金属的至少一种金属为钯。
4.根据权利要求1或2所述的整料式蜂窝状氧化催化剂，其中所述惰性材料的一个或多个波纹状片材和任选的扁平衬里包含缠结的非织造纤维。
5.根据权利要求4所述的整料式蜂窝状氧化催化剂，其中所述缠结的非织造纤维包含玻璃纤维。
6.根据权利要求1或2所述的整料式蜂窝状氧化催化剂，其中所述惰性粘土材料选自高岭土类、含水硅酸铝、绿泥石类、叶腊石类、膨润土或其混合物。
7.用于制备整料式蜂窝状氧化催化剂的方法，其包括以下步骤：
(a)通过堆叠或卷起任选地设置有扁平衬里的惰性材料的一个或多个波纹状片材来提供具有多个由壁限定的流通式通道的惰性整料式蜂窝状基底；
(b)用包含惰性粘土材料的芯层来涂覆所述整料式蜂窝状基底；
(c)提供包含选自铂族金属的至少一种金属和五氧化二钒的修补基面涂层；
(d)通过施加步骤(c)中制备的修补基面涂层而用顶层来涂覆芯层；和
(e)煅烧经涂覆的整料式蜂窝状基底，其中通过以下步骤制备步骤(c)的修补基面涂层：
(i)粉碎包含五氧化二钒的成品SCR催化剂产物；
(ii)将经粉碎的催化剂产物分散在水中并形成浆料；
(iii)添加选自铂族金属的至少一种金属的水溶性前体，
其中所述顶层包含0.1至10重量％的五氧化二钒和100至30000ppm重量的钯。
8.根据权利要求7所述的方法，其中所述修补基面涂层还包含钨的氧化物和二氧化钛。
9.根据权利要求7所述的方法，其中包含五氧化二钒的成品SCR催化剂产物还包含二氧化钛和钨的氧化物。
10.根据权利要求7至9中任一项所述的方法，其中所述铂族金属是钯。
11.根据权利要求7至9中任一项所述的方法，其中所述惰性材料的一个或多个波纹状片材和所述任选的扁平衬里包含缠结的非织造纤维。
12.根据权利要求11所述的方法，其中所述缠结的非织造纤维是玻璃纤维。
13.根据权利要求7至9中任一项所述的方法，其中所述惰性粘土材料选自高岭土类、含水硅酸铝、绿泥石类、叶腊石类、膨润土或其混合物。
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| EP0385164A2 (de) * | 1989-02-28 | 1990-09-05 | Degussa Aktiengesellschaft | Katalysator zur selektiven Reduktion von Stickoxiden mit Ammoniak |
| CN1628906A (zh) * | 2003-10-15 | 2005-06-22 | 赫多特普索化工设备公司 | 催化剂载体，由其制备的催化剂以及处理烟道气的方法 |
| CN1978568A (zh) * | 2005-11-29 | 2007-06-13 | 大荣C&E株式会社 | 选择性催化还原氧化氮的组合物、催化组件元件和催化组件 |
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