A new post-synthetic approach, involving cold plasma treatment, was employed for the preparation of TiO2–Beta zeolite. Zeolite Beta nanoparticles were first subjected to plasma induced deposition of TiCly (with y ≤ 3), which were further converted into TiOx (with x ≤ 2) upon O2-plasma treatment. Different steps of the new elaborated plasma approach were monitored using in situ FTIR spectroscopy. D2O isotopic exchange was used in order to shed light on the formation of Si–O–Ti bonds induced by TiCl4-plasma followed by O2-plasma treatments. The obtained TiO2–Beta materials were studied by a set of complementary characterization techniques including FTIR, TEM, SEM-EDS, XRD, N2 sorption, NMR and UV-Vis. The silanol content and the acidic properties of TiO2–Beta composites were also studied. The elaborated materials were tested as photocatalysts for methanol photooxidation in the gas phase. TiO2–Beta presents a methanol photooxidation rate 8 times higher than a conventional P25-TiO2 catalyst under UV irradiation.