Mn/TiO_2系列低温SCR脱硝催化剂制备及其反应机理研究
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摘要
选择性催化还原(SCR)脱除烟气中NO_x是大气污染控制领域的一个重要课题。近年来，低温SCR由于具有明显的节能特点和潜在的工业应用价值，正成为研究热点。但就目前国内外的研究进展而言，低温范围内催化剂活性不高、活性物质分散性较差、反应机理不够明确等仍是低温SCR脱硝技术走向实际应用的主要障碍。本文针对以上主要问题，以Mn／TiO_2作为基础组分，进行了低温SCR脱硝技术研究。
本文首先对制备方法进行了筛选。对溶胶—凝胶法、浸渍法和共沉淀法三种不同方法制备得到的催化剂活性比较结果表明，溶胶—凝胶法制备得到的催化剂纳米结构更为丰富，活性物质分散性更好，对NO的脱除率更高。可见，溶胶—凝胶法是一种较为理想的低温SCR催化剂制备方法。
其次，针对上述溶胶—凝胶法制备的催化剂，系统研究了低温SCR的优化操作条件，主要包括催化剂Mn／Ti比、催化剂焙烧温度、反应空速、反应系统中O_2和NH_3的浓度，以及在瞬态反应中O_2和NH_3的作用。此外，分析了催化反应的动力学过程，确定了反应级数和反应速率常数，并由此得到了Mn(0．4)／TiO_2的表观反应活化能。
为缓解催化剂制备过程中活性物质的烧结团聚，将过渡金属元素引入到催化剂体系中制备成三元催化剂，结果表明过渡金属元素的掺杂能够大幅度提高催化剂的活性。结合BET、XRD、XPS、TEM等表征手段，发现经过渡金属元素掺杂后催化剂的纳米结构和活性物质的分散性均得到有效改善，能更有效地脱除NO。
基于以上研究结果，研究了催化反应过程及反应机理。发现由于过渡金属元素Fe的掺杂，增加了活性组分——配位态NH_3形成的可能性，并降低了催化剂表面硝酸盐的稳定性，使硝酸盐由活性位的侵占物质转化为反应的活性中间体，从而使反应从不同的途径发生，形成了双反应通道。
最后，本文开展了催化剂抗硫性能的探索研究。制备了含Zr的低温SCR催化剂，并采用TG-DSC、XPS、DRIFT等表征手段，研究了催化剂表面S的存在形式以及对反应过程的影响，得出了SO_2造成催化剂失活的反应机理。同时发现Zr的掺杂可在一定程度上缓解催化剂的SO_2失活现象。
The selective catalytic reduction (SCR) is an important commercial process to control NO_x from stationary sources. Recently, low-temperature SCR has attracted interests for its energy efficiency and potential application. However, the activity of the catalysts is still not very high in low-temperature range, and the dispersion of active component is not good enough. Furthermore, the reaction mechanism is not very clear. These disadvantages limit the industrial application of low-temperature SCR. In order to solve these problems, the low-temperature SCR system was investigated by using the catalysts base on Mn/TiO_2.
Firstly, to improve the dispersion of active component in the catalysts, sol-gel catatlyst preparing method was introduced. From the comparison of catalysts prepared by sol-gel, impregnation and coprecipitation methods, it was found that the nano-structure and the dispersion of active component of catalysts prepared by sol-gel method were both improved, leading to higher catalytic activity. Therefore, sol-gel method was a potential one to prepare low-temperature SCR catalyst.
Secondly, base on the catalysts prepared by sol-gel method, the operating parameters were investigated, including the ratio of Mn/Ti, the calcination temperature, O_2 concentration, NH3 concentratoin, and the transient effect of the O_2 and NH_3. Furthermore, the kinetic study of the reaction was carried out. The reaction order and the rate constant were determined, and the apparent activation energy was also calculated.
To retard the sintering of the active component, the transition metals were added to the catalysts. From the characterization of the catalysts by BET, XRD, XPS and TEM, it was found that the nano-structure of the catalysts and the dispersion of the active component were both improved, which contributed to higher NO removal.
Furthermore, the reaction process and the mechanism were studied. With the addition of transition metal Fe, the coordinated NH3 was easier to be formed. The stability of the nitrate decreased, and nitrate was transformed to be an active intermediate in the reaction. Thus, the reaction could take place in another way.
Finally, the resistance to SO_2 of the catalysts was also investigated. Zr was added to the catalyst. TG-DSC, XPS and DRIFT were used to investigate the state of S over the catalysts and its influence on the reaction. The mechanism of deactivation was studied. And it was found that the resistance to SO_2 of the Zr modified catalysts was enhanced.
本文首先对制备方法进行了筛选。对溶胶—凝胶法、浸渍法和共沉淀法三种不同方法制备得到的催化剂活性比较结果表明，溶胶—凝胶法制备得到的催化剂纳米结构更为丰富，活性物质分散性更好，对NO的脱除率更高。可见，溶胶—凝胶法是一种较为理想的低温SCR催化剂制备方法。
其次，针对上述溶胶—凝胶法制备的催化剂，系统研究了低温SCR的优化操作条件，主要包括催化剂Mn／Ti比、催化剂焙烧温度、反应空速、反应系统中O_2和NH_3的浓度，以及在瞬态反应中O_2和NH_3的作用。此外，分析了催化反应的动力学过程，确定了反应级数和反应速率常数，并由此得到了Mn(0．4)／TiO_2的表观反应活化能。
为缓解催化剂制备过程中活性物质的烧结团聚，将过渡金属元素引入到催化剂体系中制备成三元催化剂，结果表明过渡金属元素的掺杂能够大幅度提高催化剂的活性。结合BET、XRD、XPS、TEM等表征手段，发现经过渡金属元素掺杂后催化剂的纳米结构和活性物质的分散性均得到有效改善，能更有效地脱除NO。
基于以上研究结果，研究了催化反应过程及反应机理。发现由于过渡金属元素Fe的掺杂，增加了活性组分——配位态NH_3形成的可能性，并降低了催化剂表面硝酸盐的稳定性，使硝酸盐由活性位的侵占物质转化为反应的活性中间体，从而使反应从不同的途径发生，形成了双反应通道。
最后，本文开展了催化剂抗硫性能的探索研究。制备了含Zr的低温SCR催化剂，并采用TG-DSC、XPS、DRIFT等表征手段，研究了催化剂表面S的存在形式以及对反应过程的影响，得出了SO_2造成催化剂失活的反应机理。同时发现Zr的掺杂可在一定程度上缓解催化剂的SO_2失活现象。
The selective catalytic reduction (SCR) is an important commercial process to control NO_x from stationary sources. Recently, low-temperature SCR has attracted interests for its energy efficiency and potential application. However, the activity of the catalysts is still not very high in low-temperature range, and the dispersion of active component is not good enough. Furthermore, the reaction mechanism is not very clear. These disadvantages limit the industrial application of low-temperature SCR. In order to solve these problems, the low-temperature SCR system was investigated by using the catalysts base on Mn/TiO_2.
Firstly, to improve the dispersion of active component in the catalysts, sol-gel catatlyst preparing method was introduced. From the comparison of catalysts prepared by sol-gel, impregnation and coprecipitation methods, it was found that the nano-structure and the dispersion of active component of catalysts prepared by sol-gel method were both improved, leading to higher catalytic activity. Therefore, sol-gel method was a potential one to prepare low-temperature SCR catalyst.
Secondly, base on the catalysts prepared by sol-gel method, the operating parameters were investigated, including the ratio of Mn/Ti, the calcination temperature, O_2 concentration, NH3 concentratoin, and the transient effect of the O_2 and NH_3. Furthermore, the kinetic study of the reaction was carried out. The reaction order and the rate constant were determined, and the apparent activation energy was also calculated.
To retard the sintering of the active component, the transition metals were added to the catalysts. From the characterization of the catalysts by BET, XRD, XPS and TEM, it was found that the nano-structure of the catalysts and the dispersion of the active component were both improved, which contributed to higher NO removal.
Furthermore, the reaction process and the mechanism were studied. With the addition of transition metal Fe, the coordinated NH3 was easier to be formed. The stability of the nitrate decreased, and nitrate was transformed to be an active intermediate in the reaction. Thus, the reaction could take place in another way.
Finally, the resistance to SO_2 of the catalysts was also investigated. Zr was added to the catalyst. TG-DSC, XPS and DRIFT were used to investigate the state of S over the catalysts and its influence on the reaction. The mechanism of deactivation was studied. And it was found that the resistance to SO_2 of the Zr modified catalysts was enhanced.
引文
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