[en] Zr-benzendicarboxylate structure, UiO-66 was prepared in 1-L batch scale by using a unique sonochemical-solvothermal combined synthesis method. The produced UiO-66 showed uniform particles of ca. 0.2 µm in size with the BET surface area of 1,375 m²/g in high product yield (>95%). The UiO-66 showed 198 and 84 mg/g CO₂ adsorption capacity at 273 K and 298 K, respectively, with excellent CO₂ selectivity (CO₂:N₂=32:1) at ambient conditions. The isosteric heat of CO₂ adsorption varied from 33 to 25 kJ/mol as the adsorption progressed. The UiO-66 tested for xylene isomer separation in a liquid-phase batch mode confirmed preferential adsorption of the adsorbent for o-xylene over m-, and p-xylene