ABSTRACT:The one-stage bitemplate synthesis method for obtaining mesoporous zeolite-containing materials was used to prepare Ti-aerosil (Ti-MZ). The formation kinetics and the textural features of this material were also studied. The products were characterized by IR spectroscopy (FT-IR), X-ray diffraction (XRD) and nitrogen adsorption methods. Hydrothermal processing (HTP) for relatively short time periods (ca. 8 h) led to the formation of zeolite nano-domains in the amorphous titanium-silica matrix exhibiting perfect twodimensional hexagonal packing without destruction of the mesopore framework. Increasing HTP time was accompanied by the formation of a highly crystalline zeolite framework in the titanium-silica matrix which exhibited increasing microporosity accompanied by the destruction of the mesoporous framework.