Aluminum sec-butoxide (ASB) was synthesized to a high purity grade from Al dross through dissolution reaction and vacuum distillation under the condition of 3 mol C4H9OH/mol Al as a stoichiometric reactant ratio and 10^(-3) mol HgI2/mol Al as a catalyst. The dissolution reaction proceeded for 24 hours, then pure ASB was recovered by vacuum distillation from the Al solution obtained after the dissolution. The ASB thus synthesized was quantitatively analyzed by a complexometric method for purity. This reaction gave a 99.2% purity and 28% yield. Characteristics of the synthesized ASB were analyzed by FT-IR, 27Al-NMR, and 1H-NMR. The result of analysis revealed that the crystalline structure between the synthesized ASB and commercial ASB was identical. Especially, the yield synthesized through this experiment corresponded to the total amount of Al metal existing in Al dross.