The nanocomposites of poly(o-chloroaniline) with titanium dioxide have been prepared via chemical oxidative polymerization technique using o-chloroaniline monomer and titanium dioxide nanoparticles for photocatalytic application. The different composites were prepared by varying the load percentage of titanium oxide nanoparticles (TiO2 NPs) in polyorthochloroaniline (POCA) matrix. The synthesized composite materials were characterized by Scanning electron microscopy (SEM), X-Rays diffraction (XRD), and Fourier transform infrared spectroscopy (FTIR) techniques. The POCA/TiO2 nanocomposites were further applied to evaluate the photocatalytic degradation potential towards direct yellow 50 (DY50) dye in an aqueous medium under ultraviolet radiations.