The development of more resistant and inexpensive materials were important for the emergence of composites, materials that are the result of the mixing of two or more distinct components with improved properties. Vegetable fibers reinforced polymer matrix composites help to reduce costs as well as to preserve product quality. Sisal fibers are important due to good impact resistance and availability. Thus, the characterization used infrared spectroscopy and UV-Vis diffuse reflectance. The main purpose was to adapt the methodology used, in order to improve fiber-matrix adhesion, but without risks of fiber defibrillation. Scanning electron microscopy was used to obtain the morphological characterization and the energy-dispersive X-Ray spectroscopy to describe the elemental chemical composition of the fibers. Chemical treatments using NaOH 2% and acetylation with acetic acid and acetic anhydride in the ratio (1:1,5) were important to observe the main changes such as the removal of impurities and the smaller amount of water absorbed in the acetylated fiber, which allows a better adhesion of the fibers with a polymer. After this, the fibers can be used to the production of polypropylene and polyethylene composites that are expected to apply in automotive parts such as bumpers, fuel tanks and internal coatings.