DEVELOPMENT OF A PROCESS MODEL FOR A BATCH REACTIVE DISTILLATION - A CASE-STUDY

This paper presents the development of a complex fine chemical process involving simultaneous reaction and fractionation. The synthesis of t he ethyl eater of pentenoic acid CPA) involves the successive substitu tion of allyl alcohol (AA) for ethanol (EA) on triethyl orthoacetate ( TEOA) followed by an in situ exothermic oxy-Claisen rearrangement of t he mixed ortho esters. In this case study scaling-up is carried out fr om laboratory to production. The emphasis of the work is application o f reaction engineering to a problem in reactive distillation. The use of data from automated reactor experiments to determine reaction kinet ics is described. The subsequent use of the kinetics in a comprehensiv e simulation of the reactive distillation for scale-up and to establis h safe, optimum production conditions is also described. The three imp ortant requirements for this process (i) a high conversion of triethyl orthoacetate to the pentenoic acid ethyl (PAEE) and allyl esters (PAA E), (ii) to achieve a high selectivity for the ethyl ester and (III) t o minimise the excess of allyl alcohol used in each batch. At the comm encement of the work, the selectivity for the desired ethyl ester was about 50 %, with similar yield of the unwanted allyl ester. At the end of the work, all the stated process requirements were met and the sel ectivity for the desired product was raised to> 98 % under production conditions. (C) 1998 Elsevier Science Ltd. All rights reserved.