Vanadium (V) and yttrium (Y) were extracted from coal fly ash by a leaching pro-cess utilizing sulfuric acid with assistance of ultrasonic and hydrogen peroxide.Response surface methodology was applied to optimize main factors includingsolid-to-liquid (S/L) ratio, H2SO4percentage, and H2O2percentage. Under opti-mal conditions recovery rates for V and Y were 100 % and 97 %, respectively. Amodified shrinking core model to study the kinetic leaching showed that the massdiffusion step controlled the reaction rate. The enthalpies for V and Y recoveryindicated that the process was endothermic. Gibbs energy for both metals wasnegative, i.e., the process was spontaneous. Field emission scanning electronmicroscopy was applied to determine the effects of acid concentration and ultra-sound on the surface of coal fly ash. Results demonstrated that the leaching agentcould degrade and diffuse to coal ash particles.