Chitosan-graft-polyacrylonitrile (Ch-g-PAN), polyacrylonitrile/sepiolite (PAN-Sep) nanocomposites, and Ch-g-PAN/sepiolite (Ch-g-PAN-Sep) nanocomposites were produced via free radical polymerization using persulfate-metabisulfite redox initiators. The nanocomposites of sepiolite-modified PAN containing as much as 1%, 3% and 5% of acrylonitrile levels in sepiolite were successfully produced in situ. Chitosan and sepiolite increased thermal resistance and sorption of water is more advantageous and has more coverage. These copolymers and nanocomposites were electrospun to produce Ch-PAN derivative-based nanofibers. Nanofibers were successfully produced by the electrospinning method from the copolymers and nanocomposites containing sepiolite moiety.