Abstract: Utilizing the renewable waste biomass to procure advanced materials has been the aim of research. Various reaction parameters were optimized for the graft co-polymerization of Hibiscus sabdariffa cellulose fiber using binary vinyl monomeric mixture. The graft co-polymers thus obtained were characterized by XRD technique and the results received the supporting evidence by various other advanced analytical techniques. The percentage crystallinity and crystallinity index were found to decrease with increase in grafting while a reduction in moisture absorption was observed. There was an increase in physico-chemico-thermal resistance in the graft copolymers. These graft copolymer can be used in various scientific applications.