This study describes a hydrometallurgical process to investigate the cerium recovery from rare earth polishing powder waste (REPPW) containing main elements such as cerium, lanthanum, praseodymium, neodymium, calcium and aluminum. First, dissolution experiments on La 2 O 3 , Pr 2 O 3 , Nd 2 O 3 , CaO and Al 2 O 3 with 5 µm particle size in sulfuric acid solutions were carried out using a batch reactor with various acid concentrations (115 mol/dm 3 ) at different temperatures (30180°C). The effects of these two parameters on the dissolution reaction were studied. The obtained results showed that two sequential leaching steps were needed to separate cerium from the mixture of CeO 2 , La 2 O 3 , Pr 2 O 3 , Nd 2 O 3 , CaO and Al 2 O 3 . The total process for cerium recovery from REPPW via two-stage acid leaching was then developed through the collection of experimental results. Moreover, the dissolution rate of Al 2 O 3 was expressed by a shrinking core kinetics model. The variation of the dissolution rate constant with temperature obeyed the Arrhenius equation with activation energy of 130 kJ·mol ¹1 and reaction rate constant as a function of the acid concentration of C 0.41. On the basis of the above data, a k-T (reaction rate constant-reaction temperature) diagram for a CeO 2 Al 2 O 3 H 2 SO 4 H 2 O system that permits rational extraction of CeO 2 and Al 2 O 3 was devised.