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The traditional process of alumina production by acid method was to neutralize the aluminum chloride solution obtained by acid leaching for preparing aluminum hydroxide, and then calcined to produce alumina. This process not only had many processes, but also had high energy consumption. In this paper, the properties of alumina prepared by pyrolysis of aluminum chloride solution were studied by chemical composition analysis, XRD and SEM. Thermodynamics of the pyrolysis process was analyzed. The effects of temperature and time on the pyrolysis properties of aluminum chloride solution were investigated. The results showed that it would be completely feasible according to thermodynamic calculation of the pyrolysis reactions of aluminum chloride solution. Meanwhile with the increasing of temperature and pyrolysis time, the residual chlorine content decreased gradually, and the particle size of the product decreased and tended to be uniform. The prolongation of pyrolysis time promoted the pyrolysis process of aluminum chloride solution and contributed to the formation of Al2O3 phase.