Research on polymer matrix composites has become increasingly important in both the academic and industrial sectors. The study of polymer-natural fiber composites, known for their eco-friendly properties, has gained significance. Sugarcane bagasse fibers, abundant as discarded agricultural byproducts, offer improved properties such as density, rigidity, strength, and cost-effectiveness, enhancing sustainability. As a result, experiments were performed on cellulose fibers pre-treated from sugarcane bagasse using 5% NaOH solution by simply soaking them for 4–5 h followed by washing with water. Further modifications involved esterification using phthalic anhydride and phthaloyl chloride via steam baths at 90 °C and oxidation using sodium percarbonate with a phase transfer catalyst (Adogen) at 80 °C. These chemically altered cellulose fibers exhibited significant peak changes in the FTIR spectra, a reduced crystallinity index in the XRD pattern, increased thermal stability as evidenced by TGA curve, and improved surface roughness in the SEM analysis. This paper emphasizes successful pretreatment procedures for isolating cellulose fibers from sugarcane bagasse and introduces three chemical treatments for surface functionalization which might find applications in the preparation of biocomposites.