Synthesis of a zirconium-benzenedicarboxylate, UiO-66, was carried out in increasing production scales of 250 mL, 1 L and 5 L at 393 K. Investigation on the effect of synthesis parameters on the product yield and textural properties was carried out using autoclaves of 250 mL capacity, whereas systematic scale up works were conducted using glass reactors fitted with condensers under ambient pressure conditions. Finally, 100 L pilot scale synthesis of UiO-66 was carried out using commercial terephthalic acid as ligand with industrial-grade dimethylformamide solvent. The products were characterized by X-ray powder diffraction (XRD), scanning electron microscopy (SEM), and N-2 adsorption-desorption measurements. The pelletized UiO-66 using polyvinyl alcohol as a binder demonstrated excellent CO2/N-2 separation (36:1) with moderately high CO2 adsorption capacity (191 mg/g) at 20 bar room temperature conditions. UiO-66 also showed excellent catalytic activity in cycloaddition of CO2 to styrene oxide at 2.0 MPa and 373 K with close to 100% selectivity to carbonate. No appreciable particle size effect on the catalytic activity was observed, and UiO-66 could be reused 3 times without loss of catalytic activity. (C) 2014 Elsevier B.V. All rights reserved.