Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)In this work, organo-functionalized magnesium phyllosilicates were prepared via hydrothermal synthesis with four sources of silicon: 3-aminopropyltriethoxysilane (AMPTS), N[3-(trimethoxysilyl)propyl]-ethylenediamine (TMSPEDA), N-[3-(trimethoxysilyl)propyl]-diethylenetriamine (TMSPETA) and tetraethoxyorthosilane (TEOS). Microwave radiation (MW) was employed as heating source and the results were compared with the analogous materials synthesized by conventional heating in an oven (CE). The materials obtained were characterized using X-ray diffraction (XRD), Fourier transformed infrared spectroscopy (FTIR), solid state Si-29 and C-13 nuclear magnetic resonance (NMR), thermogravimetry (TG) and elemental analysis of carbon, nitrogen and hydrogen (CHN). The 2:1 type of trioctahedral phyllosilicate was confirmed by the presence of the 0601330 reflection, at 59.5 degrees 2 theta. The presence the organic modifier was proven by the bands at 2930, 2850, and 1490 cm(-1) and the typical features of the phyllosilicate were found at 3700 cm(-1) (Mg-OH) and 1014 cm(-1) (Si-O-Si). C-13-NMR showed that the organic chains were intact in the interlayer space (5-64 ppm). Thermogravimetry indicated that these pending groups were stable in this support until 200 degrees C when they begin to decompose. Silicon-29 NMR confirmed that the pending groups were bound directly to the silicon atoms by the resonance of Si-C bond at 48 and 55 ppm. The results showed the success of the procedure for all the proportions of the silicon sources used, with a reduction of reaction time in the range from 91% to 96% using microwave radiation in relation to the conventional heating oven. (C) 2014 Elsevier Inc. All rights reserved.190292300PETROBRASConselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)