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Every year a considerable amount of olive husk was rejected in nature by different oil mills or incinerated. The valorization of these agricultural wastes by its incorporation as loading in the development of composite materials with polyvinyl chloride (PVC) is the object of this research. To improve the properties of the interface between the polymer matrix and olive husk flour (OHF), two chemical treatment methods were conducted. The first treatment consisted to use PVC-g-MA (maleic anhydride grafted on PVC) as a compatibilizer in composites; the second was a surface modification of olive husk flour by benzoylation. In this context, we prepared various formulations based on polyvinyl chloride/olive husk flour with different loading rates (10, 20, and 30%) using twin-screw extrusion. The Fourier transform infrared was used to study the chemical modification of the fiber. The composites were characterized by mechanical tests, thermogravimetric (ATG/DTG), mechanical dynamic analysis (DMA), and the physical characterization by the water absorption test. The thermogravimetric analysis revealed the improvement of the thermal stability of the composites with and without treatment compared to virgin PVC.