Three different samples of nickel aluminosilicate (NAS) nanocomposite for application as catalyst in transfer hydrogenation reactions were prepared by the incorporation of nickel nanoparticles into the mesoporous aluminosilicate framework obtained by a simple sol-gel method followed by calcinations at various temperatures without using any templates. The above prepared nanocomposites were characterized using thermal studies, Fourier transform infrared (FT-IR) spectroscopy, powder X-ray diffraction (XRD) analysis, scanning electron microscopy (SEM), energy dispersive X-ray analysis (EDAX), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS) and nitrogen adsorption-desorption (BET) analysis. Effect of calcination temperature of alumnosilicate support on the surface area and pore size of the nanocomposites was studied from BET analysis. Crystalline nature and particle size of nickel oxide present in the aluminosilicate framework was determined from powder XRD pattern. Surface morphology of the catalysts and their elemental compositions were obtained from SEM and EDAX techniques, respectively. Catalytic activity of the above prepared catalysts towards transfer hydrogenation (TH) of carbonyl compounds using isopropyl alcohol as hydrogen donor in presence of KOH was tested with wide range of carbonyl compounds. The yield of the products formed in TH reaction was monitored by gas chromatography (GC). (C) 2012 Elsevier B.V. All rights reserved.