Separation of ethyl acetate–isooctane mixture by heteroazeotropic batch distillation

Tom Ooms (1) , Steven Vreysen (1) , Guy van Baelen (1) , Vincent Gerbaud (2) , Ivonne Rodríguez-Donis (3)

1 Thomas More Kempen (BELGIUM)
2 LGC - Laboratoire de Génie Chimique
3 Instituto Superior de Tecnologías y Ciencias Aplicadas - INSTEC (La Havana, Cuba)

This paper studies the separation of an ethyl acetate–isooctane mixture by heterogeneous azeotropic distillation in a batch rectifying column. An initial list of 60 candidates was studied but only methanol and acetonitrile were obtained as potential heterogeneous entrainers. These entrainers form a low boiling heterogeneous azeotrope with isooctane. Experimental verification of the miscibility gap with isooctane was performed at 25 °C for each entrainer giving a smaller region for methanol than for acetonitrile. Feasibility of the heterogeneous azeotropic batch distillation was carried out experimentally in a laboratory batch distillation column having 44 theoretical equilibrium stages and using a high reflux ratio. Several distillate fractions were taken as a function of the temperature at the top of the column. For both methanol and acetonitrile, the main fraction was defined by the condensed vapor providing a liquid–liquid split of the isooctane/entrainer heteroazeotrope into the decanter. Ethyl acetate impurity was detected in both decanted phases, but in much lower amount when using acetonitrile as entrainer. The process with acetonitrile also resulted in a shorter operating time and higher purity and recovery yield of isooctane as the main distillate product. Pure ethyl acetate remained into the boiler at the end of each process.

Mots clés: Heteroazeotropic distillation; Solvent recovery; Batch distillation; Ethyl acetate–isooctane mixture; Entrainer selection; Methanol; Acetonitrile

Domaines: Génie chimique; Génie des procédés

Tom Ooms, Steven Vreysen, Guy van Baelen, Vincent Gerbaud, Ivonne Rodríguez-Donis. Separation of ethyl acetate–isooctane mixture by heteroazeotropic batch distillation. Chemical Engineering Research and Design, 2014, 92 (6), pp.995-1004. ⟨10.1016/j.cherd.2013.10.010⟩. ⟨hal-03521173⟩