This work reports the successful solid state synthesis of ZnO/NiFe2O4 nanocomposite by calcinations of both green synthesized ZnO nanorods and NiFe2O4 prismatic nanorods at high temperature (850 degrees C) for ten hours. These nanomaterials were characterized for structural, functional groups and morphological studies using XRD, FTIR and SEM respectively. The photocatalytic activity of the catalysts was assessed through photodegradation of methylene blue (MB) dye. The photocatalytic studies reveal that the ZnO/NiFe2O4 nanocomposite exhibits high degradation efficiency under UV light. The study shows that in the removal of MB solution by ZnO/NiFe2O4 nanoparticles, (OH)-O-center dot and photoproduced holes h(+) are the main species. Preparation of ZnO/NiFe2O4 nanocomposite by coupling of NiFe2O4 with green synthesized ZnO in solid state method is the novelty of this report. The synthesized recyclable ZnO/NiFe2O4 nanocomposite has potential applications in the treatment of both domestic and industrial waste water.