Resonant wave mixing is a promising technology based on employing non-linear waves to intensify heat and mass transfer and enhancing dispersion processes in mixed materials. In the present work, for the first time, resonant wave mixing was used to prepare film-forming dispersions based on gelatinized maize starch and spherical TiO2 nanoparticles (0.5–1.5 wt%) synthesized by sol–gel technique. Then, nanocomposite films were obtained by solution casting method. The dynamic viscoelastic properties, including relaxation spectra of the film-forming dispersions were investigated by oscillatory squeeze film rheometry, while the structure of the nanocomposite films was studied by X-ray diffraction, FTIR spectroscopy and scanning electron microscopy. The mechanical, water-related and UV-protective properties of the film materials were evaluated. It was shown that nanofiller incorporation enhanced the density of the 3D network structure of a gelatinized starch dispersion. The resonant wave treatment favored homogenous dispersion of the TiO2 nanoparticles in the nanocomposites. All nanocomposite film samples displayed higher tensile strength and lower water vapor permeability in comparison with starch films without the nanofiller. The obtained nanocomposites possessed UV-protective properties, which could be potentially applied to produce biodegradable packaging materials with improved functional characteristics.