The present work mainly aimed to synthesize different weight percentages (0.25 Wt% - 1.00 Wt%) of Manganese (Mn2+) and Magnesium (Mg2+) bimetal ions doped TiO2 nanomarerial assisted with different weight percentages (5 Wt% - 15 Wt%) of Gemini Surfactant (GS) using sol-gel method. The bimetal doped and undoped TiO2 photocatalysts were characterized by XRD, SEM, EDX, FT-IR, UV Vis-DRS, TEM, BET and PL. Characterization results evinced that Mn2+/Mg2+ bimetal ions doping and encapsulation of GS on

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... iO2 nanoparticles promote the formation of mesoporous multi-particle anatase TiO2 nanocatalysts with narrowed band gap, less particle size and high surface area. The surface elemental composition of the MMT5-GS2 (after calcination) revealed the presence of both the metal dopants Mn2+ and Mg2+ along with the Ti and O and their chemical interactions were further confirmed by FT-IR results. The photocatalytic activity of these catalysts was assessed by the degradation of Methyl Red (MR) using visible light irradiation. To understand the effect of different reaction parameters on the photocatalytic activity of the nanocatalysts such as the dopant concentration, GS concentration, catalyst dosage, solution pH and initial dye concentrations were investigated and optimized to achieve best performance. The photoluminescence results conclude that OH radicals are the crucial reactive species responsible for oxidative photocatalytic degradation of MR.