This work investigates the preparation of cadmium sulfde nanoparticles (CdS) embedded in the polymeric polyvinylchloride (PVC) matrix. PVC/CdS nanocomposite flms were prepared via sol–gel method with deposition by spin-coating on glass substrates. Efects of CdS nanoparticles on the structural, morphological, optical and photocatalytic properties of the synthetized nanocomposite were studied. Results of XRD and Raman analysis confrm the formation of CdS nanoparticles with hexagonal phase in the PVC matrix, with average crystallite size between 17 to 69 nm. The UV–vis spectroscopy reveals that the transmission is between 80 and 95% in the visible region, and a direct energy bandgap between 4.07 eV for 3.85 eV. The PL emission spectra indicate the interstitial cadmium defect states. In addition, the surface modifer (PVC) exert great infuence not only on the optical performance of the particles themselves but also on the size distribution of the particle in the PVC matrix. The photocatalytic study shows a good potential of PVC/CdS nanocomposites flms for MB degradation under UV light irradiation.