Nanocomposite fibers are one of the most fascinating materials with broad applications. In the present work,nanocomposite fibers were prepared by a low-cost, simple, and “green” process. The nanocomposite of cellulose acetate/TiO2was realized by combining the functional oxide material TiO2with the regenerating electrospun cellulose acetate fibers. The structural features were characterized by scan electron microcopy, transmission electron microscopy and infrared spectrum. The compositing mechanism was proposed. The surface functionalized hydroxyl by the regenerating process plays an important role for the formation of hybrid material.