A portable nanostructured nanocomposite film, based on cobalt oxide nanoparticles (NPs) and gold NPs embedded in a polyvinyl alcohol structure (PVA), Au/Co3O4/PVA, was prepared via a novel way based on pulsed laser ablation to be applied as an effective catalytic degradation material for a hazardous chemical structure as nitro compounds, which investigated by UV–visible spectroscopy (UV-Vis), infrared spectroscopy (FT-IR), scanning electron microscope (SEM), and X-ray diffraction (XRD). From XRD, the decrease in crystallinity of PVA is attributed to the intermolecular hydrogen bonding between PVA and Au/Co3O4. In addition, there are five interplanar peaks, with three peaks shared by both phases and one unique peak for each phase of Au and Co3O4. From FT-IR, the modes observed at a 500-1200 cm-1 wavenumber range corresponded to the stretching vibration modes of Au/Co3O4. From UV-VIS, as the embedding of Co3O4 on Au-PVA structure increases, the energy band gap is shifted to a lower value. This is due to the impurity introduced into Co3O4 grains, which may have trapped electrons stimulated from the conduction band, leading to a narrowing of the band gap and a continuous energy level. From SEM, in the case of the embedding of PVA with Au NPs, the bright semi-spherical shape of the nanostructured materials has a bright semi-spherical light area. Moreover, in the case of the embedding of PVA with Co3O4 NPs, the faint semi-spherical form of the nanostructured materials is discernible. Besides, the catalytic activity performance was tested for the degradation of 4-nitrophenol, which revealed that the reaction followed first-order kinetics, as indicated by linear regression analysis. The results showed that the sample completely converted 4-nitrophenol to 4-aminophenol within 6 minutes.