Niobium-aluminum-based catalysts were synthesized by a sol-gel process and successfully applied to the reaction of acetalization of acetone with glycerol yielding 2,2-dimethyl-1,3-dioxolane-4-methanol (solketal) and 2,2-dimethyl-1,3-dioxan-5-ol. The synthesis procedure was developed using high throughput techniques and the materials prepared with molar ratio1 Metal (1Nb:xAl): 100H(2)O: 1.5NH(4)OH (in which x =1, 0.6, 0.3, 0.1 and 0.05) were selected to be further investigated. The obtained series of mixed oxides displayed high catalytic activity reaching glycerol conversion up to 84%, with 98% of selectivity towards solketal. The physicochemical properties of the investigated catalysts were characterized by N-2-adorption/desorption, thermal analysis, X-rays diffraction, FTIR and Raman spectroscopy, and by adsorption of pyridine monitored by FT-IR spectroscopy and TGA. The catalysts are truly heterogeneous and can be reused in consecutive runs without loss of activity. (C) 2016 Elsevier B.V. All rights reserved.