© 2016 Wiley Periodicals, Inc. The preparation, characterization, and photocatalytic activity evaluation of three hybrid fibrous materials composed mainly by poly(methyl methacrylate) (PMMA), methyl methacrylate (MMA): 3-(trimethoxysilyl) propyl methacrylate (TMSPM): titanium butoxide (TBT), TiO2nanoparticles (NPTiO2), and TiO2nanowires (NWTiO2) is studied. Two types of fibeŕs structures were prepared, single and core-shell structures. Scanning electron microscopy (SEM) and transmission electron microscopy (TEM) analysis showed both structures, single and core-shell, as well as the inorganic phase were dispersed in the hybrid fibers. Infrared spectroscopic analysis (FT-IR) and thermal analysis showed the organic and inorganic components, as well as the weight percentage of the inorganic phase present in hybrid fibers. The photocatalytic activity of the hybrid fibers class I and II showed that the best photodegradative efficiency for methylene blue in aqueous solution (2.9 × 10−5M) was 95%, provided by PMMA—10 wt % NPTiO2. © 2016 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2016, 133, 44334.