VxTi1–xO2 (x = 5 and 10 mol %) solid solutions have been synthesized through supercritical drying in isopropanol at t = 250°C and p = 10 MPa. Their physicochemical properties and photocatalytic performance have been compared to those of an earlier synthesized ZnxTi1–xO2 aerogel containing 10 mol % Zn [1]. It has been shown that increasing the vanadium content of VxTi1–xO2 from 5 to 10 mol % leads to a decrease in hydrogen evolution rate in methanol/water splitting reaction under UV irradiation from 190 to 32 µL/(min gcatal), whereas in the case of the anatase-based aerogel solid solution containing 10 mol % Zn an opposite picture is observed: the hydrogen evolution rate in methanol/water splitting reaction under UV irradiation increases sharply to 700 µL/(min gcatal).