富氢气体中CO选择性甲烷化新型催化剂研究
摘要
CO选择性甲烷化具有工艺简单，易于操作，反应产物对燃料电池Pt电极无毒副作用等优点，在燃料电池的富氢原料气中低浓度CO深度脱除方面具有着诱人的应用前景，且其相关研究对竞争加氢反应体系以及其它对反应温度极为敏感的反应过程具有重要理论参考意义。
本文首先对催化剂活性组分及载体进行了筛选，然后添加催化助剂Zr，成功制备出Ru-Zr/CNTs催化剂。催化剂性能评价结果显示350℃还原的Ru-Zr/CNTs催化剂具有优越的催化活性，可以在较宽的温度区间（180-240℃）内将CO出口浓度降至10ppm以下。XRD、XPS、TEM以及H2-TPR等分析结果表明：添加Zr可以弱化催化剂中Ru活性组分与载体CNTs之间的相互作用，促进催化剂活性粒子在碳纳米管表面的分散；此外，ZrO_2的存在使得活性Ru粒子表面易于发生氧化电荷转移，有利于CO分子在催化剂表面的活化。碳纳米管的结构差异（管壁数，管径以及石墨化程度等）对催化剂活性粒子的分散性以及粒子形态影响并不明显。
利用CVD法（甲烷为碳源）构建了综合碳纳米管和泡沫镍诸多特性的CNTs-泡沫镍复合结构载体。研究发现采用间接浸渍法可实现Ni活性粒子在SiO_2涂层上高度均匀分散，因而在650℃的反应温度下制得碳纳米管管径分布相对均一的碳纳米管-泡沫镍复合结构载体。提高制备温度和催化剂中Ni负载量的会加剧催化剂渗入碳后的Ni粒子（即NixCy亚稳固溶体）的聚集以及裂解过程，进而导致所制备的碳纳米管的管径增大，管径分布变宽。而改变反应空速，碳纳米管的管径大小及其分布几乎不变。制备过程中，碳纳米管一部分呈现出顶端生长机制，另一部分则为底端生长机制。拉曼光谱结果表明碳纳米管-泡沫镍复合载体中的碳纳米管为多壁碳纳米管。
选用CNTs-泡沫镍复合载体创制出新型Ru-Zr/CNTs-泡沫镍复合结构催化剂。在这种新型催化剂中，CNTs用来分散活性组分以获得高催化活性，而泡沫镍骨架则用来提供高的导热性和微型反应通道，以消除反应体系中局部热点问题，进而提高反应的CO选择性及稳定性。实验结果表明Ru-Zr/CNTs-泡沫镍复合结构催化剂可以在非常宽的温度范围内（200-300℃）将富氢气体中CO出口浓度降至10ppm以下，且保持较高的CO选择性（>60%）。与Ru-Zr/CNTs相比，Ru-Zr/CNTs-泡沫镍复合结构催化剂将CO出口浓度降至10ppm以下的温度区间更宽，且CO选择性更高。在低温段（<220℃），CO主要经解离吸附反应历程形成CH_4，而高温段时CO则主要经非解离吸附反应历程形成CH_4。
Selective CO methanation has been considered to be a promising strategy in thethorough removal of CO from H2-rich gases for fuel cell, because it is easy to operate, and theproduct is safe to the Pt anodes of the PEMFC. Additionally, many other reaction processesdevelopment such as the competitive hydrogenation reaction and the temperature-sensitivereaction can be benefit greatly from the research of selective CO methanation.
The Ru-Zr/CNTs catalyst was prepared by using Ru, carbon nanotubes (CNTs) and Zr asactive component, support and promoter, respectively, based on the theory analysis andexperimental results. It was found that the catalyst reduced at350℃presented excellentcatalytic activity, decreasing CO concentration to below10ppm from10000ppm by COselective methanation at the temperature range of180-240℃. Characterizations includingXRD, XPS, TEM and H2-TPR indicate that the Zr modification of Ru/CNTs results in theweakening of the the interaction between Ru and CNTs and a higher Ru dispersion.Additionally, the oxidized charge transfer to surface Ru became more easily, due to theexisitance of ZrO_2, which is benefit to CO activation on catalyst surface. No significantinfluences on the dispersion, structure and morphology of Ru-Zr/CNTs catalyst were found bychanging the CNTs features such as wall number, out diameter (OD) and the degree ofgraphitization.
The CNTs-Ni foam was configurated by chemical vapor deposition (CVD), in which themethane was employed as carbon source. It was found that the prepared active Ni particleswere well diapersed on the SiO_2coating by indirect impregnation method, leading to thefabrication of CNTs-Ni foam composite with narrow diameter distribution of CNTs at650℃.However, the diameter distribution of CNTs broadened with increasing reaction temperatureand Ni loading, due to the agglomeration and cracking of Ni particles. No significantdifferences in the CNT diameters were observed by changing weight hourly space velocity(WHSV). Some CNTs are formed via tip-mechanism, while the other formed viabottom-mechanism. Raman analysis indicates that the as-formed CNTs are multi-wall CNTs(MCNTs).
The new Ru-Zr/CNTs-Ni foam composite catalyst was synthesized by using CNTs-Nifoam composite as support. In this catalyst, the CNTs is employed to disperse the activecomponent in nanometer size, assuring a high catalytic activity, while the Ni foam skeletonoffers high thermal conductivity and micro-channels in the size of micrometer order, allowingfor rapid heat transfer and minimizing the possibility of localized hot spots caused by the high exothermic reactions. The performance test shows that Ru-Zr/CNTs-Ni foam compositecatalyst has excellent catalytic performance, decreasing CO concentration to below10ppm byselective CO methanation at the temperature range of200-300℃, and keeping the COselectivity higher than60%. Compared with the results of Ru-Zr/CNTs, the Ru-Zr/CNTs-Nifoam composite catalyst has a wider temperature window where the CO level is less than10ppm and higher CO selectivity. The methanation of CO occurs over Ru-Zr/CNTs-Ni foamcomposite catalyst via two distinct pathways including dissociative reaction pathway andassociative reaction pathway. The first one dominates at low reaction temperature (<220℃),while the second one dominates at high reaction temperature.
本文首先对催化剂活性组分及载体进行了筛选，然后添加催化助剂Zr，成功制备出Ru-Zr/CNTs催化剂。催化剂性能评价结果显示350℃还原的Ru-Zr/CNTs催化剂具有优越的催化活性，可以在较宽的温度区间（180-240℃）内将CO出口浓度降至10ppm以下。XRD、XPS、TEM以及H2-TPR等分析结果表明：添加Zr可以弱化催化剂中Ru活性组分与载体CNTs之间的相互作用，促进催化剂活性粒子在碳纳米管表面的分散；此外，ZrO_2的存在使得活性Ru粒子表面易于发生氧化电荷转移，有利于CO分子在催化剂表面的活化。碳纳米管的结构差异（管壁数，管径以及石墨化程度等）对催化剂活性粒子的分散性以及粒子形态影响并不明显。
利用CVD法（甲烷为碳源）构建了综合碳纳米管和泡沫镍诸多特性的CNTs-泡沫镍复合结构载体。研究发现采用间接浸渍法可实现Ni活性粒子在SiO_2涂层上高度均匀分散，因而在650℃的反应温度下制得碳纳米管管径分布相对均一的碳纳米管-泡沫镍复合结构载体。提高制备温度和催化剂中Ni负载量的会加剧催化剂渗入碳后的Ni粒子（即NixCy亚稳固溶体）的聚集以及裂解过程，进而导致所制备的碳纳米管的管径增大，管径分布变宽。而改变反应空速，碳纳米管的管径大小及其分布几乎不变。制备过程中，碳纳米管一部分呈现出顶端生长机制，另一部分则为底端生长机制。拉曼光谱结果表明碳纳米管-泡沫镍复合载体中的碳纳米管为多壁碳纳米管。
选用CNTs-泡沫镍复合载体创制出新型Ru-Zr/CNTs-泡沫镍复合结构催化剂。在这种新型催化剂中，CNTs用来分散活性组分以获得高催化活性，而泡沫镍骨架则用来提供高的导热性和微型反应通道，以消除反应体系中局部热点问题，进而提高反应的CO选择性及稳定性。实验结果表明Ru-Zr/CNTs-泡沫镍复合结构催化剂可以在非常宽的温度范围内（200-300℃）将富氢气体中CO出口浓度降至10ppm以下，且保持较高的CO选择性（>60%）。与Ru-Zr/CNTs相比，Ru-Zr/CNTs-泡沫镍复合结构催化剂将CO出口浓度降至10ppm以下的温度区间更宽，且CO选择性更高。在低温段（<220℃），CO主要经解离吸附反应历程形成CH_4，而高温段时CO则主要经非解离吸附反应历程形成CH_4。
Selective CO methanation has been considered to be a promising strategy in thethorough removal of CO from H2-rich gases for fuel cell, because it is easy to operate, and theproduct is safe to the Pt anodes of the PEMFC. Additionally, many other reaction processesdevelopment such as the competitive hydrogenation reaction and the temperature-sensitivereaction can be benefit greatly from the research of selective CO methanation.
The Ru-Zr/CNTs catalyst was prepared by using Ru, carbon nanotubes (CNTs) and Zr asactive component, support and promoter, respectively, based on the theory analysis andexperimental results. It was found that the catalyst reduced at350℃presented excellentcatalytic activity, decreasing CO concentration to below10ppm from10000ppm by COselective methanation at the temperature range of180-240℃. Characterizations includingXRD, XPS, TEM and H2-TPR indicate that the Zr modification of Ru/CNTs results in theweakening of the the interaction between Ru and CNTs and a higher Ru dispersion.Additionally, the oxidized charge transfer to surface Ru became more easily, due to theexisitance of ZrO_2, which is benefit to CO activation on catalyst surface. No significantinfluences on the dispersion, structure and morphology of Ru-Zr/CNTs catalyst were found bychanging the CNTs features such as wall number, out diameter (OD) and the degree ofgraphitization.
The CNTs-Ni foam was configurated by chemical vapor deposition (CVD), in which themethane was employed as carbon source. It was found that the prepared active Ni particleswere well diapersed on the SiO_2coating by indirect impregnation method, leading to thefabrication of CNTs-Ni foam composite with narrow diameter distribution of CNTs at650℃.However, the diameter distribution of CNTs broadened with increasing reaction temperatureand Ni loading, due to the agglomeration and cracking of Ni particles. No significantdifferences in the CNT diameters were observed by changing weight hourly space velocity(WHSV). Some CNTs are formed via tip-mechanism, while the other formed viabottom-mechanism. Raman analysis indicates that the as-formed CNTs are multi-wall CNTs(MCNTs).
The new Ru-Zr/CNTs-Ni foam composite catalyst was synthesized by using CNTs-Nifoam composite as support. In this catalyst, the CNTs is employed to disperse the activecomponent in nanometer size, assuring a high catalytic activity, while the Ni foam skeletonoffers high thermal conductivity and micro-channels in the size of micrometer order, allowingfor rapid heat transfer and minimizing the possibility of localized hot spots caused by the high exothermic reactions. The performance test shows that Ru-Zr/CNTs-Ni foam compositecatalyst has excellent catalytic performance, decreasing CO concentration to below10ppm byselective CO methanation at the temperature range of200-300℃, and keeping the COselectivity higher than60%. Compared with the results of Ru-Zr/CNTs, the Ru-Zr/CNTs-Nifoam composite catalyst has a wider temperature window where the CO level is less than10ppm and higher CO selectivity. The methanation of CO occurs over Ru-Zr/CNTs-Ni foamcomposite catalyst via two distinct pathways including dissociative reaction pathway andassociative reaction pathway. The first one dominates at low reaction temperature (<220℃),while the second one dominates at high reaction temperature.
引文
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