ZnS, Fe2O3 and ZnS/ Fe2O3 nanoparticles were prepared by Chemical and sol gel method under optimal conditions and characterized using XRD, TEM and UV-Visible spectroscopic techniques. As-synthesized nanomaterials were used as a photocatalysts for the degradation of Victoria Blue-B dye. Effects of photo-catalyst load and substrate initial concentration on degradation of the dye in aqueous solution have been investigated. Maximum degradation (97.2 %) of Victoria Blue-B was observed using catalyst load (Fe2O3) : 1.0g/250ml of 25 mgL-1. Photocatalytic degradation of the dye follows pseudo first order kinetics. Using Victoria Blue-B initial concentration, 100mg/lit., the dye degradation rate constant under visible radiation and photocatalyst load, was 5.33 x 10-3 min-1.