In this research, structural, magnetic properties and photocatalytic activity of cobalt ferrite spinel (CoFe2O4) nanoparticles were studied. The samples were characterized by X-ray powder diffraction (XRD), energy dispersive X-ray (EDX), scanning electron microscopy (SEM), transmission electronic microscopy (TEM), Brunauer−Emmett−Teller (BET), Fourier transform infrared spectroscopy (FTIR), and UV-visible diffused reflectance spectroscopy (DRS) analysis. The XRD analysis revealed the formation of the single-phase CoFe2O4 with a cubic structure that is annealed at 500−700 °C in 3 h. The optical band gap energy for CoFe2O4 was determined to be in the range of 1.57−2.03 eV. The effect on the magnetic properties of cobalt ferrites was analyzed by using a vibrating sample magnetometer (VSM). The particle size and the saturation magnetization of cobalt ferrite nanoparticles increased with increasing annealing temperature. The photocatalytic activity of CoFe2O4 nanoparticles was investigated by using rhodamine B dye under visible light. The decomposition of rhodamine B reached 90.6% after 270 min lighting with the presence of H2O2 and CF500 sample.