Ce和La掺杂KIT-6中孔分子筛负载的Co基催化剂的费-托合成催化性能研究
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摘要
费-托合成反应是一种由气转液的技术,就是在催化剂的作用下将一氧化碳和氢气转化为燃油和化学品的技术。在费-托合成反应的催化剂中(Fe, Co, Ni和Ru),钴基催化剂具有活性高,稳定性好,使用寿命长,不易积碳和中毒,产物以长链正构烷烃为主,产物烃经加氢裂解和异构改质可以得到低硫、低氮含量的优质柴油,以及与铁相比较低的水煤气变化反应,和与钌相比较低廉的价格等优点。
在本文工作中,采用水热合成法合成一系列不同含量Ce或La掺杂的KIT-6分子筛作为载体。同时采用满孔浸渍法制备了Ce或La负载的载体。将制备好的载体同样采用满孔浸渍法负载15%的钴制成催化剂。采用X-射线粉末衍射(XRD)、透射电子显微镜(TEM)、固体紫外漫反射(DRS-UV-vis)、X-射线光电子能谱(XPS)、固体~(29)Si魔角旋转核磁共振(~(29)Si MAS NMR)、氮气物理吸附-脱附、氢气程序升温还原(H2-TPR)、氢气程序升温脱附-氧滴定(H2-TPD和O_2 titration)等技术对催化剂进行了表征,在固定床反应器上考察了催化剂的费-托合成反应活性和产物选择性。主要结论如下:
1)KIT-6的结构在掺杂Ce后保持不变。载体xCe-KIT-6的骨架中同时存在Ce~(3+)和Ce~(4+)两种离子。载体xCe-KIT-6和浸渍法制备的载体0.06Ce-KIT-6-I采用满孔浸渍法制备15%的钴基催化剂。催化剂15Co/xCe-KIT-6的还原度在低的Ce含量时呈增加趋势,在高的Ce含量时呈减小趋势。掺杂低含量Ce可以提高催化剂的费-托合成反应活性和C_(5+)的选择性,而掺杂高含量的Ce则使催化剂呈现低的反应活性和C_(5+)的选择性。同时,甲烷选择性呈现和C_(5+)的选择性相反的趋势。催化剂15Co/0.06Ce-KIT-6-I的活性比催化剂15Co/KIT-6低。
2)KIT-6的结构在掺杂La后保持不变。掺杂少量的La到分子筛骨架中负载催化剂可以增加催化剂的还原度,大量的La的掺入则会降低催化剂的还原度。而催化剂的分散度随着La掺杂量的增加呈现先增加后降低的趋势。少量的La可以增加钴催化剂的活性和C_(5+)的选择性。
3)同样量的Ce或La做为助剂时,将其掺杂到分子筛骨架中的KIT-6载体负载的催化剂活性比其在KIT-6表面做载体时的活性高。
Fischer-Tropsch synthesis (FTS) is a gas-to-liquid (GTL) technology, which catalytically converts carbon monoxide and hydrogen into transportation fuels and chemicals. Among typical FTS catalysts (Fe, Co, Ni and Ru), the cobalt catalyst is preferred due to its high selectivity for heavy hydrocarbons, lower activity for water-gas shift (WGS) reaction than iron catalysts and lower price than ruthenium.
In the present work, A series of Ce- or La- incorporated into the structure of KIT-6 mesoporous molecular sieves with different Ce or La contents were synthesized by a direct hydrothermal process. Samples of Ce- or La- loaded KIT-6 material were synthesized by the incipient wetness impregnation technique. Catalysts with 15 wt% Co loading on the above supports were also prepared by the impregnation method. The supports and catalysts were characterized by X-ray diffraction, transmission electron microscopy, diffuse reflectance UV-vis, X-ray photoelectron spectroscopy, solid-state ~(29)Si magic-angle spinning nuclear magnetic resonance, N2 physisorption, H2 temperature-programmed reduction, H2 temperature-programmed desorption and oxygen titration. The catalysts activity and selectivity were evaluated in a fixed-bed reactor under typical hydrocarbon synthesis conditions. The main results are as follows:
1) The structure of the KIT-6 support was well retained after Ce incorporation. The samples of xCe-KIT-6 have both Ce3+ and Ce4+ sites in the framework. Catalysts with 15 wt % Co loading on the xCe-KIT-6 and 0.06Ce-KIT-6-I were prepared by the impregnation method. The percentage reduction of the 15Co/xCe-KIT-6 increased slightly for catalysts with low Ce content and decreased significantly with high Ce content. Small amounts of Ce were found to improve the activity of cobalt catalysts, and increase the selectivity to C5+ hydrocarbons of the Co catalysts for Fischer–Tropsch synthesis, while larger amounts of Ce had the reverse effect. Meanwhile, methane selectivity shows an opposite trend to C5+ selectivity. Ce-loaded KIT-6 supported Co catalyst presented lower activity than KIT-6 supported Co catalyst.
2) The structure of the KIT-6 support was well retained after La incorporation. Small amounts of La incorporated into the framework of KIT-6 promoted the percentage reduction of catalysts, and the large amounts of La decreased it. The trend in the catalyst dispersion of the 15Co-yLa-KIT-6 increased and then decreased with increasing La content. Small amounts of La were found to improve the activity of cobalt catalysts, and increase the selectivity to C5+ hydrocarbons of the Co catalysts for Fischer–Tropsch synthesis.
3) The same amounts of Ce or La as a promoter, Ce or La incorporated into the framework of KIT-6 had a higher activity more than Ce or La loaded at the surface of KIT-6.
在本文工作中,采用水热合成法合成一系列不同含量Ce或La掺杂的KIT-6分子筛作为载体。同时采用满孔浸渍法制备了Ce或La负载的载体。将制备好的载体同样采用满孔浸渍法负载15%的钴制成催化剂。采用X-射线粉末衍射(XRD)、透射电子显微镜(TEM)、固体紫外漫反射(DRS-UV-vis)、X-射线光电子能谱(XPS)、固体~(29)Si魔角旋转核磁共振(~(29)Si MAS NMR)、氮气物理吸附-脱附、氢气程序升温还原(H2-TPR)、氢气程序升温脱附-氧滴定(H2-TPD和O_2 titration)等技术对催化剂进行了表征,在固定床反应器上考察了催化剂的费-托合成反应活性和产物选择性。主要结论如下:
1)KIT-6的结构在掺杂Ce后保持不变。载体xCe-KIT-6的骨架中同时存在Ce~(3+)和Ce~(4+)两种离子。载体xCe-KIT-6和浸渍法制备的载体0.06Ce-KIT-6-I采用满孔浸渍法制备15%的钴基催化剂。催化剂15Co/xCe-KIT-6的还原度在低的Ce含量时呈增加趋势,在高的Ce含量时呈减小趋势。掺杂低含量Ce可以提高催化剂的费-托合成反应活性和C_(5+)的选择性,而掺杂高含量的Ce则使催化剂呈现低的反应活性和C_(5+)的选择性。同时,甲烷选择性呈现和C_(5+)的选择性相反的趋势。催化剂15Co/0.06Ce-KIT-6-I的活性比催化剂15Co/KIT-6低。
2)KIT-6的结构在掺杂La后保持不变。掺杂少量的La到分子筛骨架中负载催化剂可以增加催化剂的还原度,大量的La的掺入则会降低催化剂的还原度。而催化剂的分散度随着La掺杂量的增加呈现先增加后降低的趋势。少量的La可以增加钴催化剂的活性和C_(5+)的选择性。
3)同样量的Ce或La做为助剂时,将其掺杂到分子筛骨架中的KIT-6载体负载的催化剂活性比其在KIT-6表面做载体时的活性高。
Fischer-Tropsch synthesis (FTS) is a gas-to-liquid (GTL) technology, which catalytically converts carbon monoxide and hydrogen into transportation fuels and chemicals. Among typical FTS catalysts (Fe, Co, Ni and Ru), the cobalt catalyst is preferred due to its high selectivity for heavy hydrocarbons, lower activity for water-gas shift (WGS) reaction than iron catalysts and lower price than ruthenium.
In the present work, A series of Ce- or La- incorporated into the structure of KIT-6 mesoporous molecular sieves with different Ce or La contents were synthesized by a direct hydrothermal process. Samples of Ce- or La- loaded KIT-6 material were synthesized by the incipient wetness impregnation technique. Catalysts with 15 wt% Co loading on the above supports were also prepared by the impregnation method. The supports and catalysts were characterized by X-ray diffraction, transmission electron microscopy, diffuse reflectance UV-vis, X-ray photoelectron spectroscopy, solid-state ~(29)Si magic-angle spinning nuclear magnetic resonance, N2 physisorption, H2 temperature-programmed reduction, H2 temperature-programmed desorption and oxygen titration. The catalysts activity and selectivity were evaluated in a fixed-bed reactor under typical hydrocarbon synthesis conditions. The main results are as follows:
1) The structure of the KIT-6 support was well retained after Ce incorporation. The samples of xCe-KIT-6 have both Ce3+ and Ce4+ sites in the framework. Catalysts with 15 wt % Co loading on the xCe-KIT-6 and 0.06Ce-KIT-6-I were prepared by the impregnation method. The percentage reduction of the 15Co/xCe-KIT-6 increased slightly for catalysts with low Ce content and decreased significantly with high Ce content. Small amounts of Ce were found to improve the activity of cobalt catalysts, and increase the selectivity to C5+ hydrocarbons of the Co catalysts for Fischer–Tropsch synthesis, while larger amounts of Ce had the reverse effect. Meanwhile, methane selectivity shows an opposite trend to C5+ selectivity. Ce-loaded KIT-6 supported Co catalyst presented lower activity than KIT-6 supported Co catalyst.
2) The structure of the KIT-6 support was well retained after La incorporation. Small amounts of La incorporated into the framework of KIT-6 promoted the percentage reduction of catalysts, and the large amounts of La decreased it. The trend in the catalyst dispersion of the 15Co-yLa-KIT-6 increased and then decreased with increasing La content. Small amounts of La were found to improve the activity of cobalt catalysts, and increase the selectivity to C5+ hydrocarbons of the Co catalysts for Fischer–Tropsch synthesis.
3) The same amounts of Ce or La as a promoter, Ce or La incorporated into the framework of KIT-6 had a higher activity more than Ce or La loaded at the surface of KIT-6.
引文
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