乙炔在ZSM-5和ferrierite基催化剂上选择还原氮氧化物的机理研究
摘要
汽车尾气中的氮氧化物对大气环境造成了越来越严重的污染,它的有效去除受到世界的广泛关注。烃类选择催化还原氮氧化物法(HC-SCR)是消除稀燃发动机尾气中NO_x的最有效方法。本论文从探索稀燃条件下乙炔和氮氧化物在ZSM-5和ferrierite(FER)分子筛基催化剂上的吸附规律,及其与乙炔选择还原氮氧化物反应(C_2H_2-SCR)活性之间的关系出发,研究开发了具有低温高活性的C_2H_2-SCR反应催化剂,并探讨了其反应机理。
对于1600 ppm NO+800 ppm C_2H_2+10%O_2+N_2体系,研究发现250℃在HFER分子筛上,氮氧化物的消除转化率为70%,是HZSM-5的3倍。
为探索上述与HZSM-5相比,HFER活性高的原因,用原位红外光谱研究比较了这两种分子筛上NO+O_2共吸附生成硝酸根的相对速率,发现(1)上述两种分子筛上吸附NO_x生成硝酸根的速率,正比于C_2H_2-SCR反应中其上氮氧化物的转化率;(2)在C_2H_2-SCR原位反应稳态红外光谱中,这两种分子筛上未出现硝酸根物种的红外吸收峰(1629和1598 cm~(-1))。基于这些实验结果,提出并论证了C_2H_2-SCR反应的控速步骤为硝酸根物种在分子筛表面上的生成。与HZSM-5相比,HFER分子筛上硝酸根物种的形成能力较强,是其低温活性高于HZSM-5的主要原因。
通过原位红外光谱对C_2H_2-SCR反应的跟踪,排除了前人诸多文献提出乙酰胺为反应活性中间物种的可能性。提出并论证了甲酰胺为分子筛上C_2H_2-SCR反应的重要活性中间物种。甲酰胺物种来源于硝酸根与C_2H_2的反应,并对NO+O_2(及硝酸根)有相当高的反应活性。由此,提出了HFER和HZSM-5基催化剂上的C_2H_2-SCR反应机理。
在HZSM-5和HFER分子筛中担载2%Zr,显著促进了催化剂上硝酸根物种的生成。相应地,显著提高了分子筛对C_2H_2-SCR反应的活性:在250℃使氮氧化物转化率分别由原来的20%提高至53%(HZSM-5)以及70%到78%(HFER)。
研究发现,当Zr原子同晶取代分子筛骨架上的Al原子后,所得催化剂的C_2H_2-SCR反应活性显著低于HFER,表明Zr原子处于分子筛孔道与处于分子筛骨架对分子筛C_2H_2-SCR反应的影响显著不同。相应的,Zr原子同晶取代HFER中的Al原子后未在其上的C_2H_2-SCR原位反应稳态红外光谱中发现甲酰胺物种的生成,这与所得催化剂的低C_2H_2-SCR反应活性相对应。
The elimination of nitrogen oxides has received much attention all over the world due to the more and more serious pollution caused by the pollutant gases being contained in automobile exhaust. Selective catalytic reduction of NO by hydrocarbons (HC-SCR) has been believed to be the most effective way to remove nitrogen oxides from the exhaust gas of lean-burn engines. The thesis aimed to research the active catalyst for selective catalytic reduction of NO_x by C_2H_2 (C_2H_2-SCR) at low temperature and investigate the reaction mechanism. The feature of zeolites for adsorbing acetylene and nitrogen oxides was studied firstly, which are the main reactants for the aimed reaction.
It was found that the NO_x conversion over HFER is as 3 times high as that of HZSM-5 under the reaction conditions of 1600 ppm NO + 800 ppm C_2H_2 + 10 % O_2 in N_2 at 250℃.
The nitrate species formation over the zeolites by the co-adsorption of NO+O_2 was investigated by in situ FT-IR and the following results were obtained. (1) The activity of the zeolites for C_2H_2-SCR can be well correlated with the relative rate of the nitrate species formation. (2) The bands at 1629 and 1598 cm~(-1) due to nitrate species, which were sharply appeared when the catalyst was exposed to NO+O_2, could not be observed in the in situ FT-IR spectra when the catalysts were exposed to C_2H_2+NO+O_2. Based on the results above, it was proposed that the rate-determining step of C_2H_2-SCR was nitrate species formation over the catalysts. It is the main reason for the high activity of HFER at low temperature in C_2H_2-SCR that the formation rate of nitrate species on HFER was higher than that on HZSM-5.
Based on the in situ FT-IR investigation, acetamide, which was supposed to be an intermediate of HC-SCR in series of reaction systems, was excluded in C_2H_2-SCR over the zeolites based catalysts. It was proposed for the first time that formamide species was a crucial intermediate for C_2H_2-SCR. The formamide species produced by the reaction of nitrate species with C_2H_2 are quite high reactive towards NO+O_2 (and nitrate species). Accordingly, the mechanism of C_2H_2-SCR over HFER and HZSM-5 was proposed.
The nitrate species formation on the catalysts was dramatically improved by loading 2 % Zr on HZSM-5 and HFER. Accordingly, the activity of the catalysts for C_2H_2-SCR were significantly enhanced, leading to the sharp increase of NO_x conversion from 20 % to 56 % (HZSM-5) and 70 % to 78 % (HFER) at 250℃, respectivly.
The activity of Zr/HFER towards the aimed reaction influenced by present state of zirconium was also investigated. It was found that Zr isomorphous substituted Al in the framework of HFER is unfavorable for C_2H_2-SCR although the loading of zirconium on the zeolite could significantly enhance the aimed reaction. Correspondingly, no band at 1691 cm~(-1) due to formamide species appeared in the in situ FT-IR spectra in steady state of C_2H_2-SCR over the catalyst in which part of Al in the framework of HFER was isomorphous substituted by Zr, which is in line with the much low activity of the catalyst for C_2H_2-SCR.
对于1600 ppm NO+800 ppm C_2H_2+10%O_2+N_2体系,研究发现250℃在HFER分子筛上,氮氧化物的消除转化率为70%,是HZSM-5的3倍。
为探索上述与HZSM-5相比,HFER活性高的原因,用原位红外光谱研究比较了这两种分子筛上NO+O_2共吸附生成硝酸根的相对速率,发现(1)上述两种分子筛上吸附NO_x生成硝酸根的速率,正比于C_2H_2-SCR反应中其上氮氧化物的转化率;(2)在C_2H_2-SCR原位反应稳态红外光谱中,这两种分子筛上未出现硝酸根物种的红外吸收峰(1629和1598 cm~(-1))。基于这些实验结果,提出并论证了C_2H_2-SCR反应的控速步骤为硝酸根物种在分子筛表面上的生成。与HZSM-5相比,HFER分子筛上硝酸根物种的形成能力较强,是其低温活性高于HZSM-5的主要原因。
通过原位红外光谱对C_2H_2-SCR反应的跟踪,排除了前人诸多文献提出乙酰胺为反应活性中间物种的可能性。提出并论证了甲酰胺为分子筛上C_2H_2-SCR反应的重要活性中间物种。甲酰胺物种来源于硝酸根与C_2H_2的反应,并对NO+O_2(及硝酸根)有相当高的反应活性。由此,提出了HFER和HZSM-5基催化剂上的C_2H_2-SCR反应机理。
在HZSM-5和HFER分子筛中担载2%Zr,显著促进了催化剂上硝酸根物种的生成。相应地,显著提高了分子筛对C_2H_2-SCR反应的活性:在250℃使氮氧化物转化率分别由原来的20%提高至53%(HZSM-5)以及70%到78%(HFER)。
研究发现,当Zr原子同晶取代分子筛骨架上的Al原子后,所得催化剂的C_2H_2-SCR反应活性显著低于HFER,表明Zr原子处于分子筛孔道与处于分子筛骨架对分子筛C_2H_2-SCR反应的影响显著不同。相应的,Zr原子同晶取代HFER中的Al原子后未在其上的C_2H_2-SCR原位反应稳态红外光谱中发现甲酰胺物种的生成,这与所得催化剂的低C_2H_2-SCR反应活性相对应。
The elimination of nitrogen oxides has received much attention all over the world due to the more and more serious pollution caused by the pollutant gases being contained in automobile exhaust. Selective catalytic reduction of NO by hydrocarbons (HC-SCR) has been believed to be the most effective way to remove nitrogen oxides from the exhaust gas of lean-burn engines. The thesis aimed to research the active catalyst for selective catalytic reduction of NO_x by C_2H_2 (C_2H_2-SCR) at low temperature and investigate the reaction mechanism. The feature of zeolites for adsorbing acetylene and nitrogen oxides was studied firstly, which are the main reactants for the aimed reaction.
It was found that the NO_x conversion over HFER is as 3 times high as that of HZSM-5 under the reaction conditions of 1600 ppm NO + 800 ppm C_2H_2 + 10 % O_2 in N_2 at 250℃.
The nitrate species formation over the zeolites by the co-adsorption of NO+O_2 was investigated by in situ FT-IR and the following results were obtained. (1) The activity of the zeolites for C_2H_2-SCR can be well correlated with the relative rate of the nitrate species formation. (2) The bands at 1629 and 1598 cm~(-1) due to nitrate species, which were sharply appeared when the catalyst was exposed to NO+O_2, could not be observed in the in situ FT-IR spectra when the catalysts were exposed to C_2H_2+NO+O_2. Based on the results above, it was proposed that the rate-determining step of C_2H_2-SCR was nitrate species formation over the catalysts. It is the main reason for the high activity of HFER at low temperature in C_2H_2-SCR that the formation rate of nitrate species on HFER was higher than that on HZSM-5.
Based on the in situ FT-IR investigation, acetamide, which was supposed to be an intermediate of HC-SCR in series of reaction systems, was excluded in C_2H_2-SCR over the zeolites based catalysts. It was proposed for the first time that formamide species was a crucial intermediate for C_2H_2-SCR. The formamide species produced by the reaction of nitrate species with C_2H_2 are quite high reactive towards NO+O_2 (and nitrate species). Accordingly, the mechanism of C_2H_2-SCR over HFER and HZSM-5 was proposed.
The nitrate species formation on the catalysts was dramatically improved by loading 2 % Zr on HZSM-5 and HFER. Accordingly, the activity of the catalysts for C_2H_2-SCR were significantly enhanced, leading to the sharp increase of NO_x conversion from 20 % to 56 % (HZSM-5) and 70 % to 78 % (HFER) at 250℃, respectivly.
The activity of Zr/HFER towards the aimed reaction influenced by present state of zirconium was also investigated. It was found that Zr isomorphous substituted Al in the framework of HFER is unfavorable for C_2H_2-SCR although the loading of zirconium on the zeolite could significantly enhance the aimed reaction. Correspondingly, no band at 1691 cm~(-1) due to formamide species appeared in the in situ FT-IR spectra in steady state of C_2H_2-SCR over the catalyst in which part of Al in the framework of HFER was isomorphous substituted by Zr, which is in line with the much low activity of the catalyst for C_2H_2-SCR.
引文
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