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Abstract: The Wastewater treatment process is an increasing serious challenge for the whole world. Due to this reason, the proficient treatment of wastewaters has attracted major attentions among researchers to solve the problem. Several methods for removal of the dye contaminants from wastewater including photocatalytic degradation, adsorption, coagulation/flocculation, advanced oxidation processes, ozonation, membrane filtration and biological treatments have been developed and use. Amongst which, photocatalytic degradation has been recognized as the most popular treatment process in aqueous solution with the advantages of high efficiency and simple operation. In the past two decades, photocatalytic degradation of organic pollutant by semiconductor oxide such as TiO2, ZnO, NiO, SnO2, Cu2O, and In2O3 has attracted due to their high photo-catalytic efficiency, low cost and low toxicity, high physical and chemical stability, especially, strong ability of fully decomposing organic pollutant into harmless species. In the present work, NiO nanoparticle were synthesized by a chemical precipitation method using nickel nitrate as precursors and Sodium hydroxide as precipitating agent. The NiO nanoparticles have been successfully used as a photocatalyst for degradation of Methylene Blue dye from the aqueous medium. The synthesized nanoparticles were studied by powder XRD, EDAX, UV and FTIR spectroscopy. The powder XRD result revealed that the obtained sample structure. The particle size and the morphology of NiO nanoparticles were studied by the SEM. The EDAX and FTIR analyses confirmed the formation of NiO nanoparticles. Further, NiO impregnated activated carbon (AC-NiO) was prepared for photocatalytic degradation studies. The Photocatalytic degradation study results revealed that the AC-NiO nanocomposite was potential photocatalyst in degradation of Methylene blue (75%) when compared with plain Nio (25%).