Production of high-purity ethyl acetate using reactive distillation: Experimental 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 twofolds: (1) to realize the type-II RD process [Y.T. Tang, Y.W. Chen, H.P. Huang, C.C. Yu, S.B. Huang, M.J. Lee, Design of reactive distillations for acetic acid esterification with different alcohols, AIChE J. 51 (2005) 1683–1699] for EtAc production with a pilot plant, a complex two-column configuration with liquid phase split, (2) to study the initial charges to the column holdups and a start-up procedure for continuous production. This pilot-scale plant consists of one RD column (10 reactive trays plus structured packing for separation) and a downstream stripper with a decanter in between. The two columns are equipped with temperature, flow, and level measurements and a Delta-V process control computer. The industrial grade alcohol (89 mol% EtOH, 11 mol% H2O) and acid (96.75 mol% HAc and 3.25 mol% H2O) are used as reactants. A product that contains more than 99 mol% EtAc and less than 100 ppm HAc is required as specifications. The results from six experimental runs show that, with proper initial charges in the inventory holdups and a systematic start-up procedure, high-purity acetate can be produced in a straightforward manner.