Abstract. In this study, zinc oxide (ZnO) was prepared via extrusion-dripping method through an ion exchange mediated process using sodium alginate. The samples were synthesized at 500 ˚C and 600 ˚C to study the effect of calcination temperature. The morphology, microstructure and optical activity of the calcined ZnO nanoparticles were analyzed by TGA, FESEM and XRD. It was found that ZnO nanoparticles synthesized at 600 ˚C was of higher purity with high crystallinity. To enhance the photocatalytic efficiency of zinc oxide, ZnO/NCC films were synthesized at varying ZnO loading fractions of 10 wt%, 15 wt%, 20 wt% and 25 wt% and were evaluated by photodegradation of Methylene blue dye and the highest dye percentage removal is found to be 96% which is obtained at ZnO loadings of 25 wt%. The usage of ionexchange process has shown promising results in producing ZnO of desirable characteristics.