The research of dimethylbenzene and butylacetate from industrial spent solvent oil by batch distillation was studied, and the batch distillation experiment was by pretreated material. The effects of separation temperature and reflux ratio on separation efficiency were investigated,and compared the new tower with the old one. The experimental results showed that: when the reflux ratio R was 3, Butyl acetate and Xylene product purity were low, the R ≥ 4, the purity of the product of Xylene and Butyl acetate were significantly increased; both yield were lower with the increase of reflux ratio. When R was 4, the top temperature of the distillation column was between 109 and 111.4 °C, before and after device upgrading, Butyl acetate product purity were 90.03% and 72.88% respectively.When the top temperature was above 120 °C, the device after upgrading Xylene product purity was 98% and 94.42% before the upgrading. Both of the purity and the yield improved after device upgrading.