In the present work, graft co-polymerization of acrylonitrile (AN) onto Saccharum cilliare fibre has been carried out in the presence of potassium persulphate and ferrous ammonium sulphate (FAS–KPS) as redox initiator. The reactions were carried out under pressure in an autoclave. Various reaction parameters such as pressure, time, pH, concentrations of initiator and monomer were optimized to get maximum graft yield (35.59%). Grafted and ungrafted Saccharum cilliare fibres were then subjected to evaluation of some of their properties like swelling behaviour in different solvents, moisture absorbance under different humidity levels, water uptake and resistance towards chemicals such as hydrochloric acid and sodium hydroxide. The characterization of the graft copolymers were carried out by FTIR spectrophotometer, X-ray diffraction (XRD) and scanning electron microscopic (SEM) studies.