Lanthanum (La) integration (at various nominal contents) in SBA-15 prepared under acidic medium was intended from corresponding direct nitrate addition during mesoporous silica formation. Materials were impregnated with Pt (1.5 wt%) and studied through several textural (N2 physisorption), structural (XRD, TG-DTG), and surface (FTIR, STEM-HAADF, SEM-EDS, NH3, and CO2 TPD) instrumental techniques. Pt-impregnated solids were tested in phenol hydrodeoxygenation (HDO, T = 250 °C, 3.2 MPa, batch reactor, n-decane as solvent). Catalytic activity (in pseudo-first-order kinetic constant, kHDO basis) was not directly related to Pt dispersion, which was not determined by nominal rare earth content. Determining the actual composition of modified SBA-15 materials is crucial in reaching sound conclusions regarding their physicochemical properties, especially when La modifier is directly added during mesoporous matrix formation, where efficient interaction among constituents could be difficult to get. Otherwise, results from some characterization techniques (N2 physisorption and FTIR, for instance) could be misleading and even contradictory. Indeed, extant modifier precursors, when under SBA-15 synthesis conditions, could affect the properties of prepared materials even though they were absent in obtained formulations. Performing simple compositional analysis could eliminate uncertainties regarding the role of various modifiers on characteristics of final catalysts. However, several groups have failed in doing so.
In this study, we prepared Al2O3-TiO2 (AT) mixed oxides to synthesize NiW catalysts for sulfur removal reactions. The AT support samples were prepared with various surfactants. Additionally, gallium atoms (2.4 wt%) were introduced as an additive to coat the outer surface layers of AT support that lacked Al3+ or Ti2+ cations. Characterization results showed substantial differences in textural properties, chemical composition, and surface acidity. The x-ray Photoelectron Spectroscopy (XPS) and High-Resolution Transmission Electron Microscopy (HR-TEM) results demonstrated that the NiW/AT-L-Ga sample has a better combination of dispersion, sulfidation, and promotion among materials. The sulfided NiW/AT-L-Ga catalyst had the highest catalytic activity. After incorporating Ga, XPS observed that the activity could be associated with an increase in the NiWS active phase; however, including a surfactant in the synthesis of the support allowed an increase in the amount of NiWS phase. The active phase was modeled considering the HR-TEM results for the slab length, revealing the atoms at the border susceptible to promotion.