The coal gangue was activated by calcine activation, calcine activation + mechanical activation (MA) complex activation. From the results of O2-TPO-MS and Ar-TPR-MS, we can speculate the reactions occurred during the coal gangue calcine activation processing. Effects of calcine temperature, calcine activation + MA complex activation, kinds of acid on the extraction percent of Al were investigated. The results of the extraction percent of Al and particle size analysis show that calcine (400~600 oC) activation and calcine (400~600 oC) + MA complex activation can enhance the extraction percent of Al and decrease the particle size. Much higher extraction percent of Al can be obtained with H2SO4 as acid medium than with HCl as acid medium for the coal gangue activated with the same condition.