Oil palm mesocarp fiber (OPMF), a biomass waste product from palm oil production, is rich in polysaccharides that can be transformed into a value-added product. This work aims to evaluate the chemical, physical, and thermomechanical properties of these fibers after a multi-step alkaline treatment, with a view to their potential use as reinforcement in industrial materials. The alkaline treatment was carried out in several stages, with sodium hydroxide (NaOH) at different concentrations (3%, 4%, and 5%) as the main reagent, and a solution of hydrogen peroxide (H2O2) and potassium hydroxide (KOH) to optimize fiber extraction. The results, obtained by Fourier transform infrared spectroscopy (FTIR), revealed significant spectral changes at certain peaks characteristic of the constituent elements of the treated fibers (absorbance at 2859, 1263, and 1027 cm？1), thus demonstrating the partial removal of hemicellulose and waxy substances during the process. In addition to the increase in the crystallinity index, initially 27% for untreated OPMF fibers, which reached 56% for OPMF fibers treated with a 5% NaOH solution, derived thermogravimetric analysis (DTG) revealed an improvement in the thermal stability of the fibers treated at 3% and 4%. Scanning electron microscopy (SEM) highlighted a more friable, stable, and porous surface after pretreatment, indicating the presence of perforations in the cell walls and an alteration of the lignin structure. In this study, the alkaline treatment was limited to four steps to preserve the lignocellulosic nature of the fiber while improving its physical and thermomechanical characteristics. These results demonstrate that alkaline treatment optimizes the performance of OPMF fibers for applications in composite materials.
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