Ni metal nanoparticles were attached on the C/TiO2@MCM-41 (CTM-41) via facile and fast method based on dispersing of C/TiO2@MCM-41 in aqueous solution containing nickel ions by ultrasonic bath. Then, for the first time, the Ni ions were converted to Ni nanoparticles under UV light (photo-assisted deposition, PAD method), without using reducing agents and hydrogen gas. This process was carried out under the relatively mild conditions. The results showed that Ni (II) was reduced to Ni metallic nanoparticle in the size of about 2.7 nm on the surface of CTM-41 (Ni/CTM-41) with specific surface area of 754.37 m2 g1. The photocatalytic ultra-deep desulfurization of a fuel-like n-octane containing dibenzothiophene (DBT) was conducted over the Ni/CTM-41 nanophotocatalyst. Using this method, the total sulfur content efficiently decreased under mild conditions in one phase and without using an oxidant. The synthesized Ni/CTM-41 (3% Ni) exhibited the maximum photocatalytic desulfurization of DBT for all different ratios of Si/Ti. In contrast, the synthesized CTM-41 (without Ni) exhibited the maximum photocatalytic desulfurization of DBT only for minimum ratio of Si/Ti. The Ni/CTM-41 was characterized by several techniques including N2 adsorption–desorption isotherms, XRD, TEM, and atomic absorption spectroscopy techniques. The results confirmed that Ni was highly dispersed on the support phase. The GC–MS analysis confirmed the photocatalytic removal of DBT. Based on the experimental results, it is proposed that the hydroxyl radical and hole have key role in the photocatalytic desulfurization process.

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