Pure cobalt aluminate (CoAl 2 O 4 ) nanoparticles were successfully synthesized by novel sol-gel method with the aid of Co(NO 3 ) 2 Á3H 2 O, Al(NO 3 ) 3 Á9H 2 O, and gelatin without adding external surfactant or template.Besides, the effect of the dosage of gelatin on the particle size of final product was investigated. Moreover, gelatin plays role as capping agent, reducing agent, and chelate agent in the synthesis CoAl 2 O 4 nanoparticles. The cobalt aluminate nanoparticles were characterized by using X-ray diffraction, scanning electron microscopy, ultraviolet-visible, Fourier transform infrared spectroscopy, and spectra energy dispersive analysis of X-ray techniques. To evaluate the catalytic properties of nanocrystalline cobalt aluminate, the photocatalytic degradation of methyl orange under visible light irradiation was carried out.