In this paper, the mixture of dimethyl carbonate, ethyl methyl carbonate and diethyl carbonate was separated by middle-vessel batch distillation with feeding in middle-vessel and process control characteristics were researched. The steady state simulation results in Aspen Plus were exported to Aspen Dynamics. Then control effect of liquid level control with HighSelector, composition control (structure1, structure2) and temperature control (proportional action, proportional integration action) were proposed. Composition control structure 2 and temperature control with PI action were investigated to achieve a good control effect. (C) 2017 The Chemical Industry and Engineering Society of China, and Chemical Industry Press. All rights reserved.