Mechanical property changes, thermal stability, and water absorption capacity of poly(vinyl chloride) (PVC)/sisal fiber composites were assessed with respect to the effect of maleic anhydride chemical treatments of the sisal fiber, for five different sisal fiber contents, varying from 0 to 30% by weight in the composite. The composites prepared with the untreated sisal exhibited higher tensile modulus and hardness than the unloaded resin, while elongation and tensile strength were reduced. The deterioration in the mechanical properties of PVC blended with sisal fiber is attributed to the presence of moisture, interfacial defects at the fiber and polymer interface, and fiber dispersion in the PVC matrix. The amount of absorbed water is a function of the amount of fiber in the composite (F0 ¼ 0 phr, F5 ¼ 0.77 phr, and F20 ¼ 4.83 phr). The comparison of the results of characterization of F5, F20, and F30 formulations prepared with the untreated fibers and the treated ones showed a reduction in absorbed water after the chemical treatment of fiber with maleic anhydride (F0 ¼ 0 phr, F5 ¼ 0.28 phr, and F20 ¼ 2.99 phr), thus improving the mechanical properties of composites prepared with the treated sisal.