CN114984971A - 一种nh3与co协同脱硝催化剂及其制备方法以及制备装置 - Google Patents
一种nh3与co协同脱硝催化剂及其制备方法以及制备装置 Download PDFInfo
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- -1 transition metal cations Chemical class 0.000 claims description 2
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- MWUXSHHQAYIFBG-UHFFFAOYSA-N Nitric oxide Chemical compound O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 abstract description 16
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- SYBFKRWZBUQDGU-UHFFFAOYSA-N copper manganese(2+) oxygen(2-) Chemical compound [O--].[O--].[Mn++].[Cu++] SYBFKRWZBUQDGU-UHFFFAOYSA-N 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 229910052748 manganese Inorganic materials 0.000 description 2
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Abstract
本发明公开了一种NH3与CO协同脱硝催化剂及其制备方法以及制备装置,包括两种催化活性物质的制备以及催化活性物质的负载,采用挤压脱模制备催化剂载体,喷涂的方式负载催化活性物质,制备工艺简便易控,通过本方法制备的协同脱硝催化剂,使烟气中的CO与氮氧化物反应,实现烟气中污染物的相互反应,既消除了CO,又减少了NH3‑SCR反应NH3的喷入量,降低了NH3逃逸;同时,由于CO在反应放出大量热量,提高了烟气温度,降低了烟气再加热成本。
Description
技术领域
本发明涉及烟气催化脱硝技术领域,更具体的说是涉及一种NH3与CO协同脱硝催化剂及其制备方法以及制备装置。
背景技术
近年来,随着环境的日益恶化,生态环境越来越被人们所重视,相关部门也出台了一系列的政策以及法规来约束污染物的排放。众多的工业生产行业中产生的污染物以及对应的处理手段各不相同。焦化以及炼钢过程中所产生的污染物主要是氮氧化物和CO,针对氮氧化物和一氧化碳的处理过程,通常采用常规脱硝工艺进行处理,但是传统脱硝无法对CO进行充分利用,并且传统脱硝工艺中,采用氨气脱硝窗口温度过高,反应中易造成NH3逃逸等。
因此,如何以NH3为主要还原剂同时充分利用烟气中的CO协同高效还原氮氧化物是本领域技术人员亟待解决的问题。
发明内容
有鉴于此,本发明提供了一种NH3与CO协同脱硝催化剂的制备方法和制备装置,通过本方法制备的协同脱硝催化剂,使烟气中的CO与氮氧化物反应,实现烟气中污染物的相互反应,既消除了CO,又减少了NH3-SCR反应NH3的喷入量,降低了NH3逃逸;同时,由于CO在反应放出大量热量,提高了烟气温度,降低了烟气再加热成本,并且装置结构简单,制备工艺简便。
为实现上述目的,本发明采用如下技术方案:
一种NH3与CO协同脱硝催化剂的制备方法,包括以下步骤:
步骤一:活性成分液的制备
(1.1)将过渡金属氧化物溶于铝溶胶中,形成CO脱硝催化活性成分液;
(1.2)将偏钒酸铵在450℃下焙烧3h,产物溶于铝溶胶中,形成NH3脱硝催化剂活性成分液;
步骤二:载体浆液的制备
将基体材料加入至去离子水中充分搅拌形成浆液,之后向浆液中加入助催化剂的前驱体溶液和增强剂,得到固含量≥60%的载体浆液;
步骤三:催化剂的制备
将步骤二得到的载体浆液置于挤压机中挤出脱模同时向载体上喷涂步骤一得到的CO脱硝催化活性成分液和NH3脱硝催化剂活性成分液,出料后自然干燥12-72h后350-750℃烧制10-60h,得到NH3与CO协同脱硝催化剂。
优选的,步骤一中所述的过渡金属氧化物为铜氧化物、锰氧化物、铈氧化物、铁氧化物中的一种或多种。
进一步的,所述的过渡金属氧化物制备方法如下:
取过渡金属的硝酸盐溶液加入碱液共沉淀,充分沉淀后,过滤去离子水洗涤至中性,60-120℃烘干5-20h,之后以5℃/min的速率升温至300℃-600℃焙烧8-10h,得到过渡金属氧化物。
进一步的,所述碱液为碳酸钠,碳酸氢钠,氨水或氢氧化钠种的一种或几种,过渡金属阳离子与碱液阴离子摩尔比为1:(1.1~1.5),更优选为1:1.2。
优选的,步骤二中所述的基体材料为二氧化钛或氧化铝,所述的助催化剂为钼氧化物或钨氧化物,为载体的0.1wt%-10wt%;对应所述的助催化剂的前驱体为七钼酸铵或偏钨酸铵溶液。
优选的,步骤二中所述的增强剂为玻璃纤维、木质素、聚氧化乙烯、纤维素中的一种或者几种,所述增强剂加入量为载体的2wt%-20wt%。
优选的,步骤二中还加入硬脂酸与乳酸的任意比混合物,所述的硬脂酸与乳酸总加入量为载体的2wt%-20wt%。
优选的,步骤二中得到的载体浆液固含量为75%~80%。
优选的,步骤三中得到的NH3与CO协同脱硝催化剂中CO脱硝催化活性成分和NH3脱硝催化剂活性成分总量为催化剂的1wt%-30wt%,CO脱硝催化活性成分和NH3脱硝催化剂活性成分的重量比为(0.1-10):1,喷涂厚度0.01-1.5cm,喷涂厚度以及两种成分的喷涂量均通过调整喷涂时间来决定。
本发明还请求保护了采用如上技术方案制备得到的NH3与CO协同脱硝催化剂。
此外,本发明还提供了制备如上技术方案中所述的NH3与CO协同脱硝催化剂的装置,包括依次连接的载体浆液储罐、载体浆液输送管和成型模具,所述载体浆输送管中设置有加压挤出装置,所述成型模具连接有活性成分输送管;
所述活性成分输送管通过料管连接有活性成分液储罐一和活性成分液储罐二,所述料管与所述活性成分输送管连接处设置有换向阀,所述活性成分输送管上设置有增压泵;
所述成型模具具有蜂窝孔结构,蜂窝孔内设置有柱塞,所述柱塞内设置有喷嘴,所述喷嘴与所述活性成分输送管连通。
优选的,所述换向阀为电磁换向阀,所述载体浆液储罐与所述载体浆液输送管之间设置有料阀。
经由上述的技术方案可知,与现有技术相比,本发明公开提供了一种NH3与CO协同脱硝催化剂及其制备方法与制备装置,具有如下有益效果:
本发明同时解决了氮氧化物和一氧化碳对环境的影响,同时消除了几种污染物,协同脱硝催化剂,降低了氨气逃逸量,减少了污染;并且充分利用了CO氧化放热特性,提高了NH3反应部分温度,进而提高了效率;重要的是本发明采用简单的装置进行挤出喷涂负载制备催化剂,解决了传统负载方式负载厚度不均等缺点,且制备工艺简便易控,可依据不同组分的催化需求进行负载调整,具有广泛的应用价值。
附图说明
为了更清楚地说明本发明实施例或现有技术中的技术方案,下面将对实施例或现有技术描述中所需要使用的附图作简单地介绍,显而易见地,下面描述中的附图仅仅是本发明的实施例,对于本领域普通技术人员来讲,在不付出创造性劳动的前提下,还可以根据提供的附图获得其他的附图。
图1为本发明制备装置的整体结构图;
图2为模具结构图;
图3为柱塞和喷嘴结构关系图。
具体实施方式
下面将结合本发明的实施例对本发明的技术方案进行清楚、完整地描述,显然,所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。
如附图1-3所示,本发明提供的NH3与CO协同脱硝催化剂的装置,包括依次连接的载体浆液储罐8、载体浆液输送管9和成型模具5,所述载体浆输送管9中设置有加压挤出装置6,所述成型模具5连接有活性成分输送管11;
所述活性成分输送管11通过料管14连接有活性成分液储罐一1和活性成分液储罐二2,所述料管14与所述活性成分输送管11连接处设置有换向阀3,所述活性成分输送管11上设置有增压泵4;
所述成型模具5具有蜂窝孔结构,蜂窝孔内设置有柱塞12,所述柱塞12内设置有喷嘴10,所述喷嘴10与所述活性成分输送管11连通。
其中,所述换向阀3为电磁换向阀,可实现智能控制和操作,所述载体浆液储罐8与所述载体浆液输送管9之间设置有料阀7,便于控制下料进而控制制备进程。
采用上述的装置进行催化剂的制备如下实施例1-2的催化剂,具体的制备工艺如下:
实施例1
步骤一:活性成分液的制备
(1.1)铜锰摩尔比=1:1的比例配置两种金属的硝酸盐溶液,80℃下充分搅拌4h后降至室温,之后加入碳酸钠共沉淀,并保证溶液总体金属阳离子:碳酸根=1:2,充分沉淀后,过滤去离子水洗涤至中性,80℃烘干12h,之后以5℃/min的速率升温至500℃焙烧9h,得到铜锰氧化物,然后将铜锰氧化物溶于铝溶胶中,形成CO脱硝催化活性成分液,置于活性成分液储罐一1中;
(1.2)将偏钒酸铵在450℃下焙烧3h,产物溶于铝溶胶中,形成NH3脱硝催化剂活性成分液,置于活性成分液储罐二2中;
步骤二:载体浆液的制备
将二氧化钛加入至去离子水中充分搅拌形成浆液;配置氧化钼前驱体即钼的盐溶液,之后向浆液中加入七钼酸铵溶液,使产物中氧化钼占载体9wt%;再向浆液中加入载体20wt%的玻璃纤维和木质素任意比混合物以及占载体5wt%的硬脂酸和乳酸的任意比例混合物,得到固含量为78%的载体浆液,置于载体浆液储罐8中;
步骤三:催化剂的制备
开启设备,通过加压挤出装置6挤出载体浆液至模具5中,待模具的出料形态基本稳定后,判断该模具出料状态是否合格,合格后开启喷涂,通过控制电磁换向阀确定两种活性成分的喷涂时间和喷涂量,设定两者喷涂时间比例为1:1,喷涂厚度为0.1cm,出料后自然干燥24h后450℃烧制40h,得到NH3与CO协同脱硝催化剂。
其中,模具的蜂窝孔截面积为0.01平方米。
实施例2
步骤一:活性成分液的制备
(1.1)铜锰铁摩尔比=1:1:2的比例配置三种金属的硝酸盐溶液,60℃下充分搅拌4h后降至室温,之后加入氢氧化钠共沉淀,保证溶液pH=10,充分沉淀后,过滤去离子水洗涤至中性,80℃烘干12h,之后以5℃/min的速率升温至450℃焙烧10h,得到铜锰铁氧化物,然后将铜锰铁氧化物溶于铝溶胶中,形成CO脱硝催化活性成分液,置于活性成分液储罐一1中;
(1.2)将偏钒酸铵在450℃下焙烧3h,产物溶于铝溶胶中,形成NH3脱硝催化剂活性成分液,置于活性成分液储罐二2中;
步骤二:载体浆液的制备
将氧化铝加入至去离子水中充分搅拌形成浆液;配置氧化钨前驱体即钨的盐溶液,之后向浆液中加入偏钨酸铵溶液,使产物中氧化钨占载体2wt%;再向浆液中加入载体13wt%的玻璃纤维和纤维素任意比混合物以及占载体10wt%的硬脂酸和乳酸的任意比例混合物,得到固含量为75%的载体浆液,置于载体浆液储罐8中;
步骤三:催化剂的制备
开启设备,通过加压挤出装置6挤出载体浆液至模具5中,待模具的出料形态基本稳定后,判断该模具出料状态是否合格,合格后开启喷涂,通过控制电磁换向阀确定两种活性成分的喷涂时间和喷涂量,设定两者喷涂时间比例为1:2(NH3脱硝催化剂活性成分:CO脱硝催化活性成分),喷涂厚度为0.01cm,出料后自然干燥24h后450℃烧制40h,得到NH3与CO协同脱硝催化剂。
其中,模具的蜂窝孔截面积为0.02平方米。
本说明书中各个实施例采用递进的方式描述,每个实施例重点说明的都是与其他实施例的不同之处,各个实施例之间相同相似部分互相参见即可。对于实施例公开的装置而言,由于其与实施例公开的方法相对应,所以描述的比较简单,相关之处参见方法部分说明即可。
对所公开的实施例的上述说明,使本领域专业技术人员能够实现或使用本发明。对这些实施例的多种修改对本领域的专业技术人员来说将是显而易见的,本文中所定义的一般原理可以在不脱离本发明的精神或范围的情况下,在其它实施例中实现。因此,本发明将不会被限制于本文所示的这些实施例,而是要符合与本文所公开的原理和新颖特点相一致的最宽的范围。
Claims (10)
1.一种NH3与CO协同脱硝催化剂的制备方法,其特征在于,包括以下步骤:
步骤一:活性成分液的制备
(1.1)将过渡金属氧化物溶于铝溶胶中,形成CO脱硝催化活性成分液;
(1.2)将偏钒酸铵在450℃下焙烧3h,产物溶于铝溶胶中,形成NH3脱硝催化剂活性成分液;
步骤二:载体浆液的制备
将基体材料加入至去离子水中充分搅拌形成浆液,之后向浆液中加入助催化剂的前驱体溶液和增强剂,得到固含量≥60%的载体浆液;
步骤三:催化剂的制备
将步骤二得到的载体浆液置于挤压机中挤出脱模同时向载体上喷涂步骤一得到的CO脱硝催化活性成分液和NH3脱硝催化剂活性成分液,出料后自然干燥12-72h后350-750℃烧制10-60h,得到NH3与CO协同脱硝催化剂。
2.根据权利要求1所述的一种NH3与CO协同脱硝催化剂的制备方法,其特征在于,步骤一中所述的过渡金属氧化物为铜氧化物、锰氧化物、铈氧化物、铁氧化物中的一种或多种。
3.根据权利要求2所述的一种NH3与CO协同脱硝催化剂的制备方法,其特征在于,所述的过渡金属氧化物制备方法如下:
取过渡金属的硝酸盐溶液加入碱液共沉淀,充分沉淀后,过滤去离子水洗涤至中性,60-120℃烘干5-20h,之后以5℃/min的速率升温至300℃-600℃焙烧8-10h,得到过渡金属氧化物。
4.根据权利要求3所述的一种NH3与CO协同脱硝催化剂的制备方法,其特征在于,所述碱液为碳酸钠,碳酸氢钠,氨水或氢氧化钠种的一种或几种,过渡金属阳离子与碱液阴离子摩尔比为1:(1.1~1.5)。
5.根据权利要求1所述的一种NH3与CO协同脱硝催化剂的制备方法,其特征在于,步骤二中所述的基体材料为二氧化钛或氧化铝,所述的助催化剂为钼氧化物或钨氧化物,为载体的0.1wt%-10wt%;对应所述的助催化剂的前驱体为七钼酸铵或偏钨酸铵溶液。
6.根据权利要求1所述的一种NH3与CO协同脱硝催化剂的制备方法,其特征在于,步骤二中所述的增强剂为玻璃纤维、木质素、聚氧化乙烯、纤维素中的一种或者几种,所述增强剂加入量为载体的2wt%-20wt%。
7.根据权利要求1所述的一种NH3与CO协同脱硝催化剂的制备方法,其特征在于,步骤二中还加入硬脂酸与乳酸的任意比混合物,所述的硬脂酸与乳酸总加入量为载体的2wt%-20wt%。
8.根据权利要求1所述的一种NH3与CO协同脱硝催化剂的制备方法,其特征在于,步骤三中得到的NH3与CO协同脱硝催化剂中CO脱硝催化活性成分和NH3脱硝催化剂活性成分总量为催化剂的1wt%-30wt%,CO脱硝催化活性成分和NH3脱硝催化剂活性成分的重量比为(0.1-10):1,喷涂厚度0.01-1.5cm。
9.一种权利要求1-8任一项所述的NH3与CO协同脱硝催化剂。
10.一种权利要求1-9任一项所述的NH3与CO协同脱硝催化剂的制备装置,其特征在于,包括依次连接的载体浆液储罐、载体浆液输送管和成型模具,所述载体浆输送管中设置有加压挤出装置,所述成型模具连接有活性成分输送管;
所述活性成分输送管通过料管连接有活性成分液储罐一和活性成分液储罐二,所述料管与所述活性成分输送管连接处设置有换向阀,所述活性成分输送管上设置有增压泵;
所述成型模具具有蜂窝孔结构,蜂窝孔内设置有柱塞,所述柱塞内设置有喷嘴,所述喷嘴与所述活性成分输送管连通。
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