The self-propagating high-temperature synthesis (SHS) of zirconium diboride followed by hydrochloric acid leaching was carried out in this study. In the SHS stage, the initial mixture of B2O3, ZrO2 and Mg powders were ignited and then a mixture of the ZrB2, MgO, Mg3B2O6 and Mg2B2O5 were formed. In the leaching step, the SHS product was leached in the acid solution to remove impurities i.e. MgO, Mg2B2O6 and Mg2B2O5. The effects of temperature and acid concentration on the selective leaching were investigated. The obtained products were characterized by using X-ray diffraction and SEM techniques.