In recent year, the price of crude oil was dramatically increased up to $ 150/barrel. It is essential to recycle and reuse the solid wastes in order to recovery the used energy. Many countries around the world have devoted their efforts in studying the techniques of solid wastes recycle and reuse, especially for the pyrolysis process of polymers and practices into oil recovery. Therefore, this research aimed to study the efficiency of ultrasound assisted oxidative desulfurization (UAOD) process applied in diesel oil and the recovered oils from waste tires after pyrolysis process (pyrolysis oil). The experimental results indicated that the oxidation efficiency increased as the addition of transition metal catalyst amounts increased. Longer sonication time (25 min) also enhanced the oxidation process through the biphasic transfer of oxidants, which resulted in high yield of organic sulfur oxidation. Moreover, the best desulfurization efficiency was accomplished at 99.72% (2.67 ppm sulfur left) and 68.18% (2800 ppm sulfur left) for diesel and pyrolysis oil, respectively. The batch experiment results could reach the goals of waste energy recovery and investigations.