CN109069994A - 用于热气过滤的催化活性过滤器、制备该过滤器的方法和从气流中同时去除固体颗粒和不期望的化合物的方法 - Google Patents
用于热气过滤的催化活性过滤器、制备该过滤器的方法和从气流中同时去除固体颗粒和不期望的化合物的方法 Download PDFInfo
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Abstract
用于在热气过滤中从热气流中同时去除固体颗粒和一种或多种不期望的化合物的催化活性过滤器用合适的催化剂部分或完全浸渍。这些化合物选自HCN、砷、有机硫化合物和羰基化合物。过滤器通过以下制备:制备包含催化有效量的至少一种活性金属和氧化物载体的浸渍液,通过将过滤器基材浸入到液体中或用液体喷洒过滤器基材来控制液体的量以用浸渍液浸渍过滤器基材,以及干燥和任选地煅烧经浸渍的过滤器。
Description
本发明涉及用于热气过滤工艺的催化活性过滤器,和制备所述过滤器的方法。此外,本发明涉及从气流中,尤其是在诸如煤、石油焦、生物质、重油、精炼厂残渣和城市固体废物气化设备的气化单元中,同时去除固体颗粒和不期望的化合物(更具体地,一种或多种选自氰化氢(HCN)、砷、有机硫化合物和羰基化合物的化合物)的方法。
热气过滤(HGF)被定义为在高于260℃的温度下对气体流出物进行干法净化(Heidenreich,Fuel 104,83-94(2013))。近年来,HGF技术已用于许多应用,例如工业废物、化学废物、动物废物和医疗废物的焚烧、贵金属回收、土壤修复、金属加工、废物能源转化项目、水泥和砖工业以及木材和造纸业。
在气化设备中,煤或其他进料用空气或用通过使空气通过空气分离单元(ASU)得到的O2直接气化。在气化之后,在气体处理工段中部分地清洁产物气体,以通过在水洗涤器中洗涤或通过过滤(通常在烛式过滤器中)来去除固体。然而,一些杂质可能通过并到达下游工艺。通过合成气处理工段的最常见杂质是砷、羰基化合物、HCN和有机硫。
对于化学品和一些与碳捕获结合的整合气化循环(IGCC)中,特别是在仅与CO2捕获结合的那些中,将部分清洁的产物气体进料到一个或多个酸变换反应器,在其中发生以下反应:
CO+H2O<->CO2+H2+热量 (1)
COS+H2O<->CO2+H2S (2)
HCN+H2O<->NH3+CO (3)
根据以下反应式,也可以在高于400℃的温度下形成甲烷作为副产物。
CO+3H2<->CH4+H2O+热量 (4)
然而,甲烷的形成将受到高蒸汽含量和/或适当催化剂设计的限制。
在酸变换工艺中,通常使用包含钴和钼的催化剂。这种Co-Mo催化剂具有在中等温度下操作而不需要从进入酸变换工艺的进料气中完全去除硫的优点。
对于没有酸变换需要的设备,将部分清洁的合成气进料到酸性气体去除(AGR)上游的COS水解中,在酸性气体去除(AGR)中通过液体介质从合成气中去除硫和CO2。
迄今为止,诸如HCN、砷、有机硫化合物和羰基化合物的组分通常已经通过酸变换COS水解反应器或在下游AGR单元中被去除,这两者都非常麻烦并且需要昂贵的处理单元,并且还导致设备停车。
本发明基于以下事实:各种过滤器单元,尤其是烛式过滤器,可以通过以下来赋予其催化活性:用催化剂前体浸渍它们,随后将其干燥并任选地煅烧。目的是将催化剂前体的一种或多种金属化合物转化为它们的催化活性形式。在某些情况下,例如基于Co-Mo的催化剂,催化剂还需要被硫化以具有催化活性。
根据本发明,将过滤器单元用催化剂浸渍,该催化剂在一种或多种选自HCN、有机硫化合物、砷和羰基化合物的化合物的转化中具有活性。
术语“羰基化合物”应以其最广泛的含义解释,意味着它涵盖所有类型的羰基化合物,包括金属羰基化合物,例如Fe和/或Ni羰基化合物。
此外,本发明基于以下观点:将催化的过滤器单元放置在工艺设备的合成气处理工段中,以便在气体进入酸变换反应器或酸性气体去除工段之前从其中去除HCN、砷、有机硫化合物和羰基化合物。
用于热气过滤的各种方法和装置在本领域中是已知的。因此,US 6,863,868公开了一种包括容器的热气过滤装置,其中安装多个过滤器元件。每个过滤器元件具有多孔本体,在其表面上设置催化层。过滤器元件的多孔本体可以是例如多孔陶瓷整体式基体、连续纤维增强的陶瓷复合材料(CFCC)基体、金属基体、金属间基体、超合金或金属-陶瓷复合材料基体。用于颗粒去除的多孔膜可以定位在过滤器元件的一个或多个表面上。据称,该装置适合于催化气相反应的各种挑战,但它也具有相当复杂的结构。
US 9,108,134描述了一种催化过滤器系统,包括具有流体入口和流体出口的过滤容器、在过滤容器内部的用于将容器内部分成原料气体室和清洁气体室的分隔壁以及多个滤烛。流体入口与原料气体室为流体连通并且位于多个滤烛的上游,而流体出口与清洁气体室为流体连通并且位于多个滤烛的下游。该过滤器系统可以用于例如煤气化中的热气清洁。
在US 2004/0067175中公开了一种陶瓷过滤器元件,其具有载体材料和含有催化材料的粘合剂材料。它特别适用于从气体中去除氮氧化物。
最后,由WO 98/03249中已知一种滤烛形式的气体净化设备。在外侧,滤烛显示出超细碳化硅颗粒的膜层,以滤除灰尘颗粒。然后沿流动方向向内是催化有效的烧结碳化硅粉末层。作为催化转化器,使用钒-钛化合物,并且用所述化合物浸渍碳化硅过滤器。滤烛是通过随后对多孔元件的涂覆产生的,然而其缺点是多孔层不能完全均匀地施加在孔区域中,因此催化剂材料的分布不均匀。除此之外,所施加的层与碳化硅颗粒的粘附存在问题,由此增加的困难是,在热气过滤的区域中,发生温度波动应力,这可以促进涂层的分离。
使用烛式过滤器的热气过滤是一种已经开始在气化行业中获得市场份额的概念。滤烛形状的陶瓷过滤器在许多工业中用于从工艺气体中去除颗粒物质。它们构成可用的最有效的集尘器类型之一,并且它们可以使颗粒的收集效率达到高于99%。过滤器可以由各种陶瓷材料制成,所述陶瓷材料包括由碱金属和碱土金属硅酸盐或硅酸铝(aluminosilicate)制成的陶瓷纤维。
过滤器(例如烛式过滤器)除了具有从工艺气体中去除颗粒物质的能力之外,还可以使过滤器具有催化功能。因此,申请人开发了用于从烟道气或废气中同时除去CO和NOx以及用于去除在许多工业工艺中产生的VOC、CO和二英的催化陶瓷烛式过滤器和方法。
本发明涉及一种催化活性过滤器,其用于在热气过滤中从热气流中同时去除固体颗粒和一种或多种选自氰化氢(HCN)、砷、有机硫化合物和羰基化合物的化合物,所述过滤器用合适的催化剂部分或完全浸渍,由两个层或区域组成,其中首先面向气体的外层或外部区域是惰性的,并且用于从气体中去除固体颗粒,并且底层或底部区域用含催化剂的液体浸渍,并且用于从气体中去除一种或多种所述化合物。
本发明的催化活性过滤器优选是烛式过滤器。然而,本发明绝不限于烛式过滤器。
在烛式过滤器中,过滤器基材具有中空圆柱体的形式。催化剂可以通过以下负载在过滤器基材上:例如通过将过滤器浸入到液体中或通过从过滤器的外侧和/或内侧将液体喷洒到过滤器上,从而用包含负载在无机氧化物载体上的所选的催化剂的液体浸渍过滤器基材。一旦施加液体,就将所得过滤器干燥并任选地煅烧。这些浸渍和干燥过程可能相当具有挑战性,因为一旦润湿,陶瓷过滤器基材往往会失去其大部分机械性能,从而可能变得相当难以处理。
本发明还涉及制备用于热气过滤的催化活性过滤器的方法,所述方法包括以下步骤:
-提供具有气体入口表面和气体出口表面的适当形状的过滤器基材,
-制备浸渍液,其包含有效量的一种或多种催化剂金属前体,其本身或在活化时能够催化地去除一种或多种选自氰化氢(HCN)、砷、有机硫化合物和羰基化合物的化合物,
-用浸渍液浸渍过滤器基材,使得过滤器基材的限定部分被催化剂填充,以及
-干燥并任选地煅烧经浸渍的过滤器基材。
加载到过滤器上的催化剂的量直接影响所得过滤器的催化性能。可以靶向催化剂负载的事实还确保没有加载过量的催化剂,由此降低了催化过滤器的总生产成本。
可以通过将过滤器基材浸入到液体中或者从其内侧将液体喷洒到过滤器基材上来施加含有催化剂的液体。此外,所施加的液体量基于所需的催化性能来限定。过滤器可以被催化剂填充,至多到液体到达外表面的位置,但也可以将总过滤器厚度的外几毫米保持在非浸渍状态,即,保持外表面干燥。通过这样做,由于过滤器的该干燥外壳,在浸渍和干燥过程中过滤器的机械性能显著提高。
本文使用的术语“外侧”和“内侧”分别是指过滤器面向未过滤气体的流动侧和面向经过滤气体的流动侧。
根据本发明使用的催化剂中的活性材料取决于期望除去的选自氰化氢(HCN)、砷、有机硫化合物和羰基化合物的化合物类型的数量。适于去除所有化合物类型的催化剂通常含有钴、钼、镍和活性氧化铝。在煤气化设备的气化器中,热的(1000℃或更高)合成气进入废热回收工段,且热气过滤器处于约300-400℃的温度,在此从气流中去除颗粒。然后进一步调节合成气,以从气流中去除HCN、砷、有机硫化合物和羰基化合物。
用于根据本发明的方法的合适的催化剂是申请人的基于Co-Mo的SSK-10TM酸变换催化剂,其同样适用于高温变换、中温变换和低温变换应用。通常,它含有约3wt%的CoO和约12wt%的MoO3,余量为载体。
经浸渍和干燥的过滤器,优选烛式过滤器,是外表面完整的过滤器,使得它仍然可以从热气流中去除颗粒。典型的过滤器直径将为约10cm,内径将为约4cm。将过滤器从中心向外浸渍,并调节浸渍流体的量,使得过滤器的限定部分被催化剂填充。如上所述,过滤器可以被催化剂填充,至多到液体到达外表面的位置或与外表面有一定距离的位置。
本发明还涉及用于从气流中去除固体颗粒和一种或多种选自氰化氢(HCN)、砷、有机硫化合物和羰基化合物的化合物的方法,其中气流通过由两个层或区域组成的催化活性过滤器,其中首先面向气体的层或区域是惰性的,而另一层或区域用含催化剂的液体浸渍,并用于从气体中去除一种或多种所述化合物。
如果气流是来自气化设备的产物气体,则催化活性过滤器位于酸性气体去除单元的上游。具体地,催化活性过滤器位于气化设备中存在的酸变换反应器的上游。
催化活性过滤器单元也可以位于气化设备的合成气处理工段中,使得在气体进入酸变换反应器或酸性气体去除工段之前从其中去除一种或多种选自氰化氢(HCN)、砷、有机硫化合物和羰基化合物的化合物。
Claims (14)
1.一种催化活性过滤器,其用于在热气过滤中从热气流中同时去除固体颗粒和一种或多种选自氰化氢(HCN)、砷、有机硫化合物和羰基化合物的化合物,所述过滤器用合适的催化剂部分或完全浸渍,由两个层或区域组成,其中
-首先面向气体的外层或外部区域是惰性的,并且用于从气体中去除固体颗粒,并且
-底层或底部区域用含催化剂的液体浸渍,并且用于从气体中去除一种或多种所述化合物。
2.根据权利要求1所述的催化活性过滤器,其中催化剂包括钴、钼、镍和活性氧化铝。
3.一种制备用于热气过滤的根据权利要求1或2所述的催化活性过滤器的方法,所述方法包括以下步骤:
-提供具有气体入口表面和气体出口表面的适当形状的过滤器基材,
-制备浸渍液,其包含有效量的一种或多种催化剂金属前体,其本身或在活化时能够催化地去除一种或多种选自氰化氢(HCN)、砷、有机硫化合物和羰基化合物的化合物,
-用浸渍液浸渍过滤器基材,使得过滤器基材的限定部分被催化剂填充,和
-干燥并任选地煅烧经浸渍的过滤器基材。
4.根据权利要求3所述的方法,其中通过用液体喷洒过滤器基材或将其浸入到液体中来浸渍过滤器基材。
5.根据权利要求3或4所述的方法,其中过滤器基材是烛式过滤器。
6.根据权利要求3所述的方法,其中过滤器基材是金属过滤器。
7.根据权利要求4或5所述的方法,其中通过从中空中心喷洒来浸渍过滤器基材以控制液体的量,使得过滤器基材的限定部分被浸渍液填充。
8.根据权利要求7所述的方法,其中过滤器被浸渍液填充,至多到液体到达外表面的位置。
9.根据权利要求7所述的方法,其中过滤器被浸渍液填充,仅到达外表面保持干燥的位置。
10.根据权利要求4-9中任一项所述的方法,其中过滤器的外径为10-20cm,内径为4-15cm。
11.一种用于从气流中去除固体颗粒和一种或多种选自氰化氢(HCN)、砷、有机硫化合物和羰基化合物的化合物的方法,其中使气流通过根据权利要求1或2所述的催化活性过滤器。
12.根据权利要求11所述的方法,其中气流是来自气化设备的产物气体,并且其中催化活性过滤器位于酸性气体去除单元的上游。
13.根据权利要求12所述的方法,其中催化活性过滤器位于气化设备中存在的酸变换反应器的上游。
14.根据权利要求13所述的方法,其中催化活性过滤器单元位于气化设备的合成气处理工段中,使得在气体进入酸变换反应器或酸性气体去除工段之前从其中去除一种或多种选自氰化氢(HCN)、砷、有机硫化合物和羰基化合物的化合物。
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US4175928A (en) * | 1975-12-05 | 1979-11-27 | Conoco Methanation Company | Hydrodesulfurization purification process for coal gasification |
US4824526A (en) * | 1985-07-31 | 1989-04-25 | Amoco Corporation | System for continuously and catalytically removing arsenic from shale oil and regenerating the catalyst |
US6863868B1 (en) * | 2000-09-29 | 2005-03-08 | Siemens Westinghouse Power Corporation | Catalytically enhanced filtration apparatus |
CN103506006A (zh) * | 2012-06-29 | 2014-01-15 | 三菱重工环境·化学工程株式会社 | 负载有催化剂的袋滤器 |
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