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Morphological Investigation Of Nanostructured Como Catalysts

机译：纳米结构科莫催化剂的形态研究

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This work reports the morphological investigation of nanostructured sulfided CoMo catalysts by means of high-resolution transmission electron microscopy (HRTEM). The catalysts were supported on Ti-modified hexagonal mesoporous silica (HMS-Ti) and P-modified HMS-Ti (P/HMS-Ti) materials. The oxide precursors were characterized by specific surface area (S_(BET)), temperature-programmed reduction (TPR), diffuse reflectance infrared Fourier transform spectroscopy in the OH region (DRIFTS-OH) and X-ray photoelectron spectroscopy (XPS) in order to elucidate the influence of the impregnation sequence (successive vs. simultaneous) and the effect of P-incorporation into HMS-Ti material on the morphology of calcined CoMo catalysts. Both TPR and XPS measurements indicate that the catalysts prepared by successive impregnation possess well-dispersed MoO_3 and CoO phases, whereas their counterparts prepared by simultaneous impregnation additionally possess the CoMoO_4 phase. For all sulfided catalysts, the presence of MoS_2 phase with particle size in the range 3.3-4.4 nm was confirmed by HRTEM. Catalytic activity was evaluated in the reaction of hydrodesulfurization (HDS) of dibenzothiophene (DBT) carried out in a flow reactor at 593 K and hydrogen pressure of 5.5 MPa. P-incorporation into the HMS-Ti material led to an overall increase in HDS activity and the hydrogenation ability of the sulfided catalysts. All catalysts proved to be stable during 10 h time-on-stream (TOS) operation. The activity of sulfide catalysts in the target reaction depends linearly on the surface exposure of Co species in the oxide precursors, as determined by XPS, and on the morphology of the sulfide form of catalysts (surface density of MoS_2 particles and their sizes) as determined by HRTEM.
机译：这项工作通过高分辨率透射电子显微镜（HRTEM）报道了纳米结构硫化CoMo催化剂的形态研究。催化剂负载在Ti改性的六方介孔二氧化硅（HMS-Ti）和P改性的HMS-Ti（P / HMS-Ti）材料上。氧化物前体的特征在于比表面积（S_（BET）），程序升温还原（TPR），OH区的漫反射红外傅里叶变换光谱（DRIFTS-OH）和X射线光电子能谱（XPS）以阐明浸渍顺序（连续vs.同时）的影响以及将P掺入HMS-Ti材料中对煅烧CoMo催化剂形态的影响。 TPR和XPS测量均表明，通过连续浸渍制备的催化剂具有良好分散的MoO_3和CoO相，而通过同时浸渍制备的相应催化剂还具有CoMoO_4相。对于所有硫化的催化剂，通过HRTEM证实存在粒径为3.3-4.4nm的MoS_2相。在二苯并噻吩（DBT）的加氢脱硫（HDS）反应中，在流动反应器中于593 K和5.5 MPa的氢气压力下评估了催化活性。 P掺入HMS-Ti材料中导致HDS活性和硫化催化剂的氢化能力全面提高。事实证明，所有催化剂在10小时的运行时间（TOS）运行中都是稳定的。硫化物催化剂在目标反应中的活性与XPS测定的氧化物前体中Co种类的表面暴露量线性相关，与测定的硫化物形式的催化剂形态（MoS_2颗粒的表面密度及其大小）线性相关。由HRTEM。

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