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BACKGROUND: The triple‐column extractive distillation (TCED) process for the ternary multi‐azeotropic mixture of N‐hexane/acetone/chloroform is a significant step in waste recovery and purification. Given the common occurrence of feed disturbances in practical industrial production, a feasible dynamic control scheme should effectively resist feed disturbances and ensure product quality, enabling the process to run steadily and safely with a high efficiency. However, it is challenging to design a robust control scheme for separation processes accompanied by side‐stream capability. In this work, dynamic control schemes were designed for four separation processes: conventional and double side‐stream TCED processes with single and double entrainers. A multipoint temperature control scheme, composition‐temperature cascade control scheme and variable ratio control were combined to improve the dynamic performance of the control schemes. RESULTS: The results showed that the control schemes designed for the four extractive distillation processes are highly robust, resisting ±20% feed flow and composition disturbances. A variable ratio control combined with composition‐temperature cascade was found to be vital for double side‐stream TCED schemes. CONCLUSION: The conventional TCED with a single entrainer (CS‐TCED) is an optimal process for N‐hexane/acetone/chloroform separation both from control and economic perspectives. The designed control scheme is simple, low‐cost and easy‐to‐implement with a superior dynamic performance over other separation schemes. This study has a certain theoretical guidance for N‐hexane/acetone/chloroform separation in terms of economic benefits and practical production. © 2022 Society of Chemical Industry (SCI). [ABSTRACT FROM AUTHOR]