There are several methods for the synthesis of nanomaterials such as sol-gel, deposition, hydrothermal, solvothermal and etc. In this thesis, aluminum and titanium oxides with high surface area and large pore volumes were prepared by a facile method. This method provides the possibility to design nanoparticles with controlled morphology, high specific surface area and high purity. One of the advantages of this method is the utilization of green and safe materials environmentally. Nanoparticles of aluminum oxides, boehmite (AlOOH) and alumina (Al 2 O 3 ), were prepared by aluminum alkoxide as precursors. These nanoparticles with high surface area and large pores were synthesized using sol-gel method via an easy and environmentally safe method in a short time. Also, for evaluation of the effect of chain length of alkoxide precursors on the product, aluminum propoxide (Al(OC 3 H 7 ) 3 ), aluminum butoxide (Al(OC 4 H 9 ) 3 ) and aluminum pentoxide (Al(OC 5 H 11 ) 3 ) was used. The application of these nanomaterials in the removal of heavy metals from water was studied and nanoboehmites were used to remove copper from aqueous solution. These nanoparticles were characterized by FT-IR, XRD, TGA, DTA, FE-SEM and TEM techniques. N 2 adsorption- desorption analyses were used for determination of the specific surface areas and pore volumes of the synthesized materials. In addition, nanoparticles of titanium oxide (TiO 2 ), using titanium alkoxide as a precursor by sol-gel method were also prepared and the effect of chain length on the product of alkoxide precursors was studied. Tetraethyl titanate (Ti(OC 2 H 5 ) 4 ), tetra-isopropyl titanate (Ti(OC 3 H 7 ) 4 ) and tetra-butyl titanate (Ti(OC 4 H 9 ) 4 ) were used as preliminary precursors. These nanoparticles were characterized by FT-IR, XRD, TGA, DTA, FE-SEM and TEM techniques. N 2 adsorption- desorption analyses were used to evaluate the specific surface area and pore volume of the prepared samples.