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Non-precious metal catalysts (10 wt% loading) over activated carbon (AC) and TiO2–SiO2 supports preparedvia incipient wetness impregnation and spray pyrolysis were characterized using various analyticaltechniques. AC with a higher surface area displayed a better ability than TiO2–SiO2 in syringol conversionand hydrocarbon product selectivity. Compared to Fe and NiFe catalysts, the Ni catalyst showed moreeffective hydrodeoxygenation performance in terms of syringol conversion, selectivity, and the yield ofoxygen-free products (mainly alkylbenzenes via transalkylation reactions). The deoxygenation abilitywas confirmed via the moisture and COx release. The highest syringol conversion (99.91%) could beobtained using 10 wt% Ni/AC. Generally, syringol hydrodeoxygenation in a fixed-bed reactor followedthe main reaction pathway of the hydrogenolysis of CAr–OC(sp3) and CAr–OH rather than the hydrogenationof the benzene ring, producing p-xylene, phenol, and cresols as the major products. Besides metalliccatalysts and supports, the reaction temperature and the total flow rate of the H2/Ar mixture onhydrodeoxygenation performance were also investigated. Our study provides a promising potential inthe utilization of non-precious metals and biomass-derived AC to remove oxygen from bio-oil modelcompounds, contributing to the development of sustainable renewable energy.