Batch distillation in a column with a cold middle vessel is studied experimentally and simulated by a constant molar holdup model. The experimental results agree well with those simulated. The middle vessel is improved by adding an inside heat exchanger, and the flow rate in the stripping section can be controlled by the pressure in the middle vessel. The liquid temperature in the middle vessel is analyzed by a simple method, and the analysis results show that the liquid temperature in the middle is greatly decreased by the inside heat exchanger. The feasibility of using such a kind of column to separate heat-sensitive compounds is analyzed, and the analysis results show that it is a competitive choice for batch distillation of heat-sensitive compounds.