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Polymers have exhibited a promising ability for the corrosion protection of metals. In the present study, poly(o-anisidine) (POA) nanoparticles and its nanocomposites with silicon dioxide (SiO2) like POA/SiO2 containing different compositions content of SiO2 (5%, 10% & 15% w/w) were prepared by chemical oxidative polymerization. FT-IR spectra of POA/SiO2 composites indicate the presence of SiO2 nanoparticles in the polymer nanocomposites. The X-ray diffraction (XRD) studies was showed more crystalline behavior of polymer nanocomposites and the particle grain size was calculated using Scherer’s formula and it was found to be within nano range. The surface morphology of the polymer composites were investigated by Scanning Electron Microscopy (SEM). Energy dispersive X-ray spectroscopy (EDS) confirms the incorporation of silicon and oxygen in the polymer nanocomposites. Further the synthesized polymeric composites were introduced into acrylic resin and the polymer/SiO2/acrylic hybrid materials were applied on the surface of mild steel sample. The corrosion efficiency and corrosion rate of the polymer nanocomposites were calculated for mild steel in 3.5% NaCl solution using Polarization curve and Electrochemical Impedance Spectroscopy (EIS).