Abstract: Continuous distillation processes including three-tower，four-tower and five-tower for separation of methyl cyanoacetate were proposed to replace the conventional batch distillation process. The best separation technology，that is five-tower continuous distillation，was determined based on the process technological analysis. Optimization simulations of five-tower continuous distillation were performed with ASPEN PLUS software in which RADFRAC model and WILSON equation were used，and the optimum operating conditions and equipment parameters were determined. The industrial data showed that the five-tower continuous distillation can reduce energy consumption by 30%，increase product’ yield by 2.4% compared with the batch distillation. A new process scheme for continuous separation of methyl cyanoacetate was established.