Synthesis and physicochemical characterization of titanium oxide and sulfated titanium oxide obtained by thermal hydrolysis of titanium tetrachloride

Abstract

This work reports the synthesis of titanium oxide (TiO2) and sulfated titanium oxide (TiO2-SO4(2-)) obtained by thermal hydrolysis of titanium tetrachloride. Titanium hydroxide synthesized by this method was impregnated with a 1 N H2SO4 solution, to give amounts of sulfate ions (SO4(2-)) of 3 and 7 wt%. The synthesized samples were dried at 120 °C during 24 h and then calcined for 3 h at 400 °C. Thermal analyses, X-ray diffraction, nitrogen physisorption, infrared spectroscopy, potentiometric titration with n-butylamine, U.V.-visible diffuse reflectance spectroscopy and scanning electron microscopy were used to characterize the materials. The results of physicochemical characterization revealed that a mixture of crystalline structures, anatase, brookite and rutile developed in the titanium oxide, stabilizing the anatase structure in the sulfated titanium oxides, and coexisting with a small amount of brookite structure. The synthesized mesoporous materials developed specific surface areas between 62 and 70 m² g-1, without detecting an important influence of sulfation on this parameter. The presence of sulfate ions improved the acidity of titanium oxide and modified the characteristics of light absorption in the 425-600 nm region, which suggests the possibility of using these materials in reactions assisted by visible light.