In this study, the self-propagating high-temperature synthesis (SHS) and following acid leaching techniques were carried out to produce zirconium diboride (ZrB2) powder. In the SHS experiments, technical grade ZrO2 powder, and different amounts of B2O3 and Mg powders were used. The SHS products were obtained in the form of black, spongy solid. In the leaching step, the effect of different acid concentrations on selective leaching was investigated by using optimum SHS product to eliminate the impurities such as MgO, Mg3B2O6 and Mg2B2O5. The products obtained were characterized by using XRD, ICP and SEM techniques.