Pyridine functionalized carbon nanofibers (Py-CNFs) were synthesized, characterized and used for the grafting of oxo-rhenium complex i.e., methyltrioxorhenium (MTO) via acid-base ionic interaction. The grafting of MTO to Py-CNFs was confirmed by FTIR, UV-vis, SEM, TEM and TGA analyses. The determination of rhenium content by ICP-AES further suggested the successful immobilization of MTO to the support. The developed heterogeneous material i.e., MTO@Py-CNFs was found to be an efficient catalyst for the oxidation of various secondary as well as tertiary amines to corresponding nitrones or N-oxides, respectively by using hydrogen peroxide. The developed catalyst was readily recovered by centrifugation and reused for subsequent ten runs without any significant loss in catalytic activity. (C) 2015 Elsevier B.V. All rights reserved.