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Photocatalytic oxidative desulfurization has attracted much attention in recent years due to the continuous tightening of the sulfur content requirements in motor fuels and the disadvantages of the industrial hydrodesulfurization process. This work is devoted to the investigation of the photocatalytic activity of Bi2WxMo1−xO6 solid solutions (x = 1, 0.75, 0.5, 0.25, 0) in the oxidative desulfurization of hydrocarbons under visible light irradiation using hydrogen peroxide as an oxidant. The synthesized photocatalysts were characterized in detail using XRD, SEM, EDS, low-temperature nitrogen adsorption–desorption, and DRS. It was shown that the use of solid solutions Bi2WxMo1−xO6 with x = 0.5–0.75 leads to the complete oxidation of organosulfur compounds to CO2 and H2O within 120 min. The high photocatalytic activity of solid solutions (x = 0.5–0.75) is attributed to their ability to absorb more visible light, the presence of the corner-shared [Mo/WO6] octahedral layers, which may promote the generation and separation of photogenerated charges, and the hierarchical 3D flower-like structure. The reaction mechanism of the desulfurization was also analyzed in this work.

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