Separation of n-hexane–ethyl acetate mixtures by azeotropic batch distillation with heterogeneous entrainers

In this article, a systematic study of the separation of the n-hexane–ethyl acetate mixture with an entrainer by heterogeneous azeotropic batch distillation is performed. Based upon the thermodynamic behaviour of the ternary mixtures, potential entrainers partially miscible with one or two original azeotropic components are chosen. In all cases, the entrainer adds a heterogeneous binary or ternary azeotrope that is the lowest boiling point in the ternary diagram. Therefore, it leaves the column by the overhead stream which is subcooled to get two liquid phases in the decanter. The phase with the highest amount of the original component is removed as distillate product whereas the entrainer-rich phase is continuously refluxed to the column. Considering methanol, acetonitrile, water and nitromethane as heterogeneous entrainers, screening was performed based on the composition of the unstable heteroazeotropic mixture, the ratio of both liquid phases in the condensed top vapour and the purity of the distillate product determined by the liquid–liquid envelope at the decanter temperature. The process feasibility analysis is validated by using rigorous simulation with the batch process simulator ProSimBatch. Simulation results are then corroborated in a bench experimental column for the selected entrainer, showing several advantages of heterogeneous batch distillation (HBD) compared to homogeneous systems.