Production of High-purity Ethyl Acetate using reactive distillation: Experimental Validation and Start-up procedure

The production of high-purity ethyl acetate (EtAc) using reactive distillation (RD) is studied experimentally in a pilot-scale plant. The objectives are two folds: (1) to validate the appropriateness of the type-II RD flowsheet, a complex two-column configuration with liquid phase split, developed by Tang et al. (2005) and (2) to provide a startup procedure for continuous operation. This pilot-scale plant consists of one RD column and a downstream stripper with a decanter in between. The two columns are equipped with temperature, flow, and level measurements and control is executed in a Delta-V process control computer. The alcohol feed is of industrial grade ethyl alcohol (95.5 wt%; below azeotropic composition) and the acid feed contains 99wt% of acetic acid with water as impurity. Very stringent specification on EtAc is required: 99.00 wt% EtAc with acetic acid less than 100 ppm. Five experimental runs were performed and the results show that, with a correct start-up procedure, high-purity acetate can be produced in a straightforward manner.