Preparation of MCM-41 supported (Bu4N)4H3(PW11O39) catalyst and its performance in oxidative desulfurization

Highly ordered mesoporous material (Bu4N)4H3(PW11O39)/MCM-41 with 10, 18, and 25 wt.% (Bu4N)4H3(PW11O39) loadings was prepared by impregnation method in acidic media under reflux conditions, and characterized by XRD, HRTEM, Nitrogen adsorption/desorption, FT–IR, 31P CP–MAS NMR, XPS, SEM and TEM. The characterization results revealed that (Bu4N)4H3(PW11O39) was homogeneously dispersed on MCM-41 surface without effecting its mesoporous structure (even at high loadings). Nitrogen adsorption/desorption results showed that the material possessed high surface area (805–912 m2/g), pore volume (0.65–0.19 cm3/g) and pore diameter (2.2–3.0 nm). Wide angle XRD and 31P CP–MAS NMR results revealed that (Bu4N)4H3(PW11O39) was grafted onto silica surface through W–Si–O linkage and its structural integrity was maintained during preparation method. The material was found to be highly active and reusable catalyst for oxidative desulfurization (ODS) of organosulfur compounds and desulfurized almost 100% of Dibenzothiophene (DBT) and thiophene under mild reaction conditions. When the catalyst was applied for ODS of FCC cycle oil a sulfur removal of 97.2% was achieved.

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► We prepared and designed TBA–POM/MCM-41 mesoporous material.
► The characterization results revealed that (PW11O39)7− was grafted on MCM-41.
► The material was found to be highly efficient for catalytic oxidative desulfurization for model and actual oils.