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There are three kinds of binary azeotropes and one kind of a near‐boiling compound with clamping zone characteristics in the triethylamine‐dichloromethane‐acetone‐water system, which belongs to complex quaternary systems. A four‐column distillation process of heterogeneous azeotropic extraction for the separation of the system was designed, simulated, and optimized to obtain more suitable process parameters and energy consumption distribution of each column. On this basis, taking the total annual cost (TAC) as the comprehensive economic evaluation index and CO2 emission as the environmental evaluation index, the thermal integration technology and mechanical vapor recompression (MVR) heat pump technology were applied to the energy‐saving research of the distillation process for the system. The results indicate that compared with the conventional four‐column heterogeneous azeotropic extractive distillation process, the thermal integration distillation process and single‐column MVR heat pump coupled thermal integration distillation process can save energy consumption and TAC, and it can reduce CO2 emission.

There is a constant concentration zone for acetone-water mixtures, and the average relative volatility of the two components in the constant concentration zone is only 1.41, so the energy consumption of the conventional distillation process is high. Two kinds of split mechanical vapor recompression (MVR) heat pump distillation processes, i.e., single-stage and two-stage compression processes, were proposed to separate acetone-water mixtures. The thermodynamic data of the mixture were calculated and modules of Aspen Plus were used to simulate the distillation column and steam compressor. Taking the minimum total annual cost as the objective function, the conventional MVR and the two split MVR heat pump distillation processes were simulated and optimized. Compared with the conventional process, the MVR heat pump distillation process had greater economic advantages, and the split heat pump distillation (SHPD) with two-stage compression was superior to the other MVR heat pump distillation processes.

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