In this research, the photocatalytic effect was studied for sol-gel synthesized Mn/Mg co-doped metal oxide (TiO2) nanoparticles (NPs), which are encapsulated with anionic Gemini surfactant. The physicochemical properties of Mn/Mg co-doped TiO2 were investigated using a variety of characterization techniques, FT-IR, UV Vis-DRS, XRD, SEM, EDX, TEM, BET and PL. Characterization results reveal that Mn/Mg dopants stabilize TiO2 in the form of anatase phase and reduce the bandgap energy. Presence of strong chemical bonding and functional groups at the interface of dopant and TiO2 NPs was confirmed with FT-IR. The photocatalytic activity of these catalysts was assessed by the degradation of Orange II (AO7) using visible light irradiation. Of the variable nanomaterials MMT5-GS2 showed remarkable results. The photoluminescence studies revealed that OH radicals are the reactive species and responsible for oxidative photocatalytic degradation of Orange II.