The technology of purifying of α-terpineol by batch vacuum distillation from terpineol fraction, a byproduct of eucalyptus oil, was studied. The material of terpineol fraction was analyzed by GC-MS. Based on effusing curves of the target α-terpineol and those of the main impurities of γ-terpinene, terpinen-4-ol, and trans-pinocarveol by batch vacuum distillation, effects of tower packing pretreated with water and four organic solvents on the separation of α-terpineol were investigated. In addition, reflux ratio for fractioning α-terpineol was optimized. Finally, the optimum conditions found were tower packing pretreated with water, distillation in a varied reflux ratio, and the reflux ratio kept at 6 whenα-terpineol effused, whereby α-terpineol obtained was at 129～132 oC/ 5.0 kPa in purity over 90% and recovery 50%.