Effect of synthesis conditions on the structure and optical properties of hybrid copolymers based on Ti(OPr i ) 4 and hydroxyethyl methacrylate was determined. Raising the concentration of the methacrylic monomer in the system leads to a longer hydrolytic polycondensation of titanium alkoxide and faster radical polymerization of the organic monomer. Copolymers containing poly(titanium oxide) with a nearly anatase structure were obtained in the conditions of a double-stage synthesis including successive stages of low-temperature hydrolytic polycondensation and polymerization. In the case of a single-stage synthesis at 70°C, which combines simultaneously occurring polycondensation and polymerization processes, the copolymer contains the anatase (75%) and rutile (25%) forms of poly(titanium oxide).In the last two decades, extensive studies have been carried out in order to obtain nanostructured organoinorganic materials because of their optimal combination of numerous useful functions that are inherent in each component and cannot be found simultaneously in any other material [1]. The most spectacular examples of hybrid materials are nanocomposites based on SiO 2 , TiO 2 , VO 2 , and ZrO 2 in polymeric media. These nanocomposites are used in various fi elds of modern technology: biomedicine and ecology [2-4] and manufacture of solar cell arrays [5][6][7], photo/electrochromic and membrane materials, sensors [8-10], and catalysts for various reactions used to remove contaminants from the environment [11][12][13][14].The following materials can be distinguished among those being presently developed: organo-inorganic materials based on TiO 2 dispersed in a polymeric matrix and gels of poly(titanium oxide) (-TiO-) n in organic media [15][16][17][18]. Materials of this kind posses unique optical properties because of being able to effectively absorb light in the UV spectral range, which results in charge separation at the Ti-O bond and leads to the following conversion: Ti 4+ + e ← → Ti 3+ [11][12][13][14]. This property largely determines the possibility of further application of the material. It should, however, be noted that (-TiO-) n gels with high charge-separation effi ciency [18][19][20] are unstable in the course of time because of the solvent evaporation and are form-unstable. When TiO 2 powders are dispersed in a polymeric matrix, it is diffi cult to provide a homogeneous distribution of its particles with the bulk of the material. In addition, the charge-separation effi ciency in dispersions is lower than that in gels because the a single-electron-transition reaction involves only atoms on the surface of a particle, and, moreover, coarse particles scatter UV light [21]. All these factors hinder the practical application of gels and polymeric composites of titanium dioxide. Therefore, a topical task is to develop solid materials based on poly(titanium oxide), which retains the charge-separation ability as in the form of gels.