Pt/分子筛催化剂上氢气选择催化还原NO的研究
摘要
氮氧化物(NOx)是大气的主要污染物。选择催化还原法(SCR)是消除大气中NOx的有效方法。近年来,H2以其清洁、低温高活性的特点逐渐引起人们的研究兴趣。本文以ZSM-35分子筛为载体,考察了金属负载型ZSM-35催化剂在氢气选择催化还原NO(H2-SCR)反应中的活性,并通过金属助剂添加、共结晶载体使用、快速SCR反应等提高催化剂的活性和选择性。同时利用多种表征手段深入探讨H2-SCR反应机理、金属助剂的作用以及快速SCR反应的优势。
在相同条件下比较了Pt基ZSM-35催化剂与ZSM-5、Beta催化剂的H2-SCR反应性能。120℃时,Pt/ZSM-35催化剂上的NO转化率达到80.8%,相应的N2选择性为68.5%,明显优于Pt/ZSM-5、Pt/Beta。XRD和NH3-TPD结果说明三种催化剂上均含有金属态的Pt物种；Pt引入未改变载体的骨架和晶体结构,但是降低了强酸中心数量。原位红外光谱结果说明反应条件下原位生成了吸附氨物种。进一步研究表明Pt负载量对Pt/ZSM-35催化剂H2-SCR反应活性有一定影响。XRD、TEM、XPS结果显示Pt/ZSM-35催化剂上80%的Pt物种以金属态存在,20%以Pt2+的氧化态存在；Pt含量的增加并未改变催化剂上Pt物种的组分,但使得金属态Pt物种发生团聚。不同气氛下的原位红外光谱结果表明吸附的硝酸盐物种和氨物种是H2-SCR反应的重要中间物种。
通过多种不同金属对Pt/ZSM-35催化剂进行改性。Cr的引入表现出引人瞩目的促进作用：NO最高转化率由原来的80.5%提高至94.7%,相应的N2选择性由64.2%提高至67.6%。进一步研究显示Cr的最佳负载量为1 wt%,最佳引入方式为Pt、Cr共浸渍。H2-TPR结果显示与Cr/ZSM-35相比Pt-Cr/ZSM-35催化剂上Cr物种的主要还原峰明显向低温移动,说明Pt与Cr物种之间存在一定的相互作用。此外,Cr物种引入后明显增加了NO-O2在催化剂表面的吸附,形成了新的表面含氮物种,Pt-NO和Pt-NOδ+物种；原位H2-SCR反应过程中,Pt-Cr/ZSM-35催化剂上氨物种的数量明显多于Pt/ZSM-35。这说明Cr的促进作用源于增加NOx物种的吸附以及氨物种的原位生成。
首次将共结晶分子筛作为催化剂载体应用于富氧条件下的氮氧化物消除反应。Pt基ZSM-35/MCM-49催化剂表现出较好的H2-SCR反应活性。进一步研究表明共结晶分子筛载体中ZSM-35与MCM-49比例的变化对催化剂的H2-SCR反应活性影响较小。XRD、H2-TPR、CO吸附红外结果显示Pt/35(x%)/49催化剂上的Pt物种主要以Pt0、Pt2+和Pt4+形式存在。原位漫反射红外光谱研究显示H2-SCR反应过程中Pt/35(x%)/49催化剂上形成的吸附物种基本相同；载体中ZSM-35与MCM-49的比例影响原位产生的氨物种的数量。
首次将“快速SCR”概念引入到H2-SCR反应中。分别以0.5%Pt/ZSM-35和Pd/Al2O3、Pd/SiO2、Pd/MgO为催化剂,比较研究了催化剂的快速和常规H2-SCR反应活性和选择性。结果发现与常规H2-SCR反应相比,快速H2-SCR反应明显提高了氮氧化物的消除效率。Pd/Al2O3和Pd/Si02催化剂表现出极好的快速H2-SCR反应活性,200℃以上NOx的转化率一直保持在100%。原位DRIFT研究显示：(1)常规和快速H2-SCR反应中催化剂表面形成的物种基本相同；(2)与常规H2-SCR反应相比,快速H2-SCR反应中催化剂表面形成了更多的吸附氨物种。
Nitrogen oxides (NOx) are the main air pollutants. Selective catalytic reduction (SCR) is the most promising way of NOx abatement. Recently, hydrogen with the advantage of clean and high activity at relatively low temperature attracts much attention. In this study, ZSM-35 zeolite is used as support. Metal based ZSM-35 catalysts are investigated in selective catalytic reduction of NO by hydrogen (H2-SCR). Metal additives, composite zeolites and fast SCR reaction are introduced to improve the activity and selectivity. Many characterizations are used to get deep insight into the reaction mechanism, the effect of additives and the advantage of fast SCR reaction.
The performance of Pt based ZSM-35, ZSM-5 and Beta in H2-SCR reaction is compared under the same reaction conditions. At 120℃, Pt/ZSM-35 catalyst exhibits attractive activity (80.8%) and selectivity (68.5%), which is better than those on Pt/ZSM-5 and Pt/Beta. XRD and NH3-TPD results suggest that metallic Pt species exist in all catalysts; the introduction of Pt does not influence the framework of zeolite support, but decreases the number of strong acid sites. Adsorbed ammonium species are formed during in situ H2-SCR reaction. The effect of Pt loading on catalytic activity is studied secondly. XRD、TEM、XPS results suggest that Pt species on Pt/ZSM-35 catalyst exist mainly in metallic (80%) and only 20% in+2 oxidation state, and the increase of Pt loading has no effect on the valance state of Pt, but causes the aggregation of metallic Pt. In situ IR results indicate that adsorbed nitrates and ammonia are key intermediates in H2-SCR reaction.
Several metals are used to modify Pt/ZSM-35 catalyst. An attractive enhancement of NO conversion from 80.5% to 94.7% is obtained at 120℃on Cr modified sample. Further studies show that 1 wt% is the optimal loading of Cr, and co-impregnation is the optimal introducing way. H2-TPR results suggest that comparing with Cr/ZSM-35, the main reduction peak of Cr species on Pt-Cr/ZSM-35 shifted to low temperature. Moreover, the introduction of Cr enhances (1) the adsorption of NO-O2 by forming new Pt-NOδ+ and NO species adsorbed on Pt were detected upon NO+O2 adsorption; (2) the formation of ammonia species under reaction condition. It indicates that the enhanced adsorption of NOx and formation of surface NH4+ species is the origin of promotional effect of Cr on Pt/ZSM-35 for H2-SCR reaction.
Composite zeolites are used firstly in NOx elimination under excess oxygen. Pt based ZSM-35/MCM-49 catalysts exhibit high activity in H2-SCR reaction. Further study suggests that the ratio of ZSM-35 and MCM-49 in composite zeolitic support has little influence on the catalytic activity. XRD and H2-TPR results, coupled with those in CO adsorption show that Pt species in Pt/35(x%)/49 catalysts are in metallic, +2 and+4 states. In situ IR results show that during H2-SCR reaction same surface species are formed on Pt/35(x%)/49 catalysts; the ratio of ZSM-35 and MCM-49 has some effect on the formation of ammonia species.
Fast SCR is introduced to H2-SCR reaction for the first time. The performance of 0.5%Pt/ZSM-35 and Pd/Al2O3, Pd/SiO2, Pd/MgO in standard and fast H2-SCR reaction is compared respectively. Results show that compared with the normal H2-SCR process, a significant enhancement of deNOx efficiency is achieved in the fast H2-SCR process. Pd/Al2O3 and Pd/SiO2 catalysts exhibited attractive activity and gave 100%NOx conversion above 200℃. In situ DRIFT results show that same surface species are formed during standard and fast H2-SCR reaction, and much more ammonia species are formed during fast H2-SCR reaction than those in standard one.
在相同条件下比较了Pt基ZSM-35催化剂与ZSM-5、Beta催化剂的H2-SCR反应性能。120℃时,Pt/ZSM-35催化剂上的NO转化率达到80.8%,相应的N2选择性为68.5%,明显优于Pt/ZSM-5、Pt/Beta。XRD和NH3-TPD结果说明三种催化剂上均含有金属态的Pt物种；Pt引入未改变载体的骨架和晶体结构,但是降低了强酸中心数量。原位红外光谱结果说明反应条件下原位生成了吸附氨物种。进一步研究表明Pt负载量对Pt/ZSM-35催化剂H2-SCR反应活性有一定影响。XRD、TEM、XPS结果显示Pt/ZSM-35催化剂上80%的Pt物种以金属态存在,20%以Pt2+的氧化态存在；Pt含量的增加并未改变催化剂上Pt物种的组分,但使得金属态Pt物种发生团聚。不同气氛下的原位红外光谱结果表明吸附的硝酸盐物种和氨物种是H2-SCR反应的重要中间物种。
通过多种不同金属对Pt/ZSM-35催化剂进行改性。Cr的引入表现出引人瞩目的促进作用：NO最高转化率由原来的80.5%提高至94.7%,相应的N2选择性由64.2%提高至67.6%。进一步研究显示Cr的最佳负载量为1 wt%,最佳引入方式为Pt、Cr共浸渍。H2-TPR结果显示与Cr/ZSM-35相比Pt-Cr/ZSM-35催化剂上Cr物种的主要还原峰明显向低温移动,说明Pt与Cr物种之间存在一定的相互作用。此外,Cr物种引入后明显增加了NO-O2在催化剂表面的吸附,形成了新的表面含氮物种,Pt-NO和Pt-NOδ+物种；原位H2-SCR反应过程中,Pt-Cr/ZSM-35催化剂上氨物种的数量明显多于Pt/ZSM-35。这说明Cr的促进作用源于增加NOx物种的吸附以及氨物种的原位生成。
首次将共结晶分子筛作为催化剂载体应用于富氧条件下的氮氧化物消除反应。Pt基ZSM-35/MCM-49催化剂表现出较好的H2-SCR反应活性。进一步研究表明共结晶分子筛载体中ZSM-35与MCM-49比例的变化对催化剂的H2-SCR反应活性影响较小。XRD、H2-TPR、CO吸附红外结果显示Pt/35(x%)/49催化剂上的Pt物种主要以Pt0、Pt2+和Pt4+形式存在。原位漫反射红外光谱研究显示H2-SCR反应过程中Pt/35(x%)/49催化剂上形成的吸附物种基本相同；载体中ZSM-35与MCM-49的比例影响原位产生的氨物种的数量。
首次将“快速SCR”概念引入到H2-SCR反应中。分别以0.5%Pt/ZSM-35和Pd/Al2O3、Pd/SiO2、Pd/MgO为催化剂,比较研究了催化剂的快速和常规H2-SCR反应活性和选择性。结果发现与常规H2-SCR反应相比,快速H2-SCR反应明显提高了氮氧化物的消除效率。Pd/Al2O3和Pd/Si02催化剂表现出极好的快速H2-SCR反应活性,200℃以上NOx的转化率一直保持在100%。原位DRIFT研究显示：(1)常规和快速H2-SCR反应中催化剂表面形成的物种基本相同；(2)与常规H2-SCR反应相比,快速H2-SCR反应中催化剂表面形成了更多的吸附氨物种。
Nitrogen oxides (NOx) are the main air pollutants. Selective catalytic reduction (SCR) is the most promising way of NOx abatement. Recently, hydrogen with the advantage of clean and high activity at relatively low temperature attracts much attention. In this study, ZSM-35 zeolite is used as support. Metal based ZSM-35 catalysts are investigated in selective catalytic reduction of NO by hydrogen (H2-SCR). Metal additives, composite zeolites and fast SCR reaction are introduced to improve the activity and selectivity. Many characterizations are used to get deep insight into the reaction mechanism, the effect of additives and the advantage of fast SCR reaction.
The performance of Pt based ZSM-35, ZSM-5 and Beta in H2-SCR reaction is compared under the same reaction conditions. At 120℃, Pt/ZSM-35 catalyst exhibits attractive activity (80.8%) and selectivity (68.5%), which is better than those on Pt/ZSM-5 and Pt/Beta. XRD and NH3-TPD results suggest that metallic Pt species exist in all catalysts; the introduction of Pt does not influence the framework of zeolite support, but decreases the number of strong acid sites. Adsorbed ammonium species are formed during in situ H2-SCR reaction. The effect of Pt loading on catalytic activity is studied secondly. XRD、TEM、XPS results suggest that Pt species on Pt/ZSM-35 catalyst exist mainly in metallic (80%) and only 20% in+2 oxidation state, and the increase of Pt loading has no effect on the valance state of Pt, but causes the aggregation of metallic Pt. In situ IR results indicate that adsorbed nitrates and ammonia are key intermediates in H2-SCR reaction.
Several metals are used to modify Pt/ZSM-35 catalyst. An attractive enhancement of NO conversion from 80.5% to 94.7% is obtained at 120℃on Cr modified sample. Further studies show that 1 wt% is the optimal loading of Cr, and co-impregnation is the optimal introducing way. H2-TPR results suggest that comparing with Cr/ZSM-35, the main reduction peak of Cr species on Pt-Cr/ZSM-35 shifted to low temperature. Moreover, the introduction of Cr enhances (1) the adsorption of NO-O2 by forming new Pt-NOδ+ and NO species adsorbed on Pt were detected upon NO+O2 adsorption; (2) the formation of ammonia species under reaction condition. It indicates that the enhanced adsorption of NOx and formation of surface NH4+ species is the origin of promotional effect of Cr on Pt/ZSM-35 for H2-SCR reaction.
Composite zeolites are used firstly in NOx elimination under excess oxygen. Pt based ZSM-35/MCM-49 catalysts exhibit high activity in H2-SCR reaction. Further study suggests that the ratio of ZSM-35 and MCM-49 in composite zeolitic support has little influence on the catalytic activity. XRD and H2-TPR results, coupled with those in CO adsorption show that Pt species in Pt/35(x%)/49 catalysts are in metallic, +2 and+4 states. In situ IR results show that during H2-SCR reaction same surface species are formed on Pt/35(x%)/49 catalysts; the ratio of ZSM-35 and MCM-49 has some effect on the formation of ammonia species.
Fast SCR is introduced to H2-SCR reaction for the first time. The performance of 0.5%Pt/ZSM-35 and Pd/Al2O3, Pd/SiO2, Pd/MgO in standard and fast H2-SCR reaction is compared respectively. Results show that compared with the normal H2-SCR process, a significant enhancement of deNOx efficiency is achieved in the fast H2-SCR process. Pd/Al2O3 and Pd/SiO2 catalysts exhibited attractive activity and gave 100%NOx conversion above 200℃. In situ DRIFT results show that same surface species are formed during standard and fast H2-SCR reaction, and much more ammonia species are formed during fast H2-SCR reaction than those in standard one.
引文
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