Boreskov Institute of Catalysis of the Siberian Branch of Russian ...

OP-III-1212342.TS6.TS8.TS12.TS51.TS913767.TS81413.TS15Figure 1: Schematic description ofexperimental reactive-distillation systemwith integrated fixed-bed reactor1 – pump for equimolar EtOH/AAmixture, 2 – fixed-bed pre-reactor,3 – pre-heater, 4 – additional feed ofacetic acid surplus, 5 – reactivedistillation column, 6 – reaction zone,7 – rectification section, 8 – strippingsection, 9 – condenser, 10 – decanter,11 – organic phase, 12 – water phase,13 – reflux stream, 14 – reboiler,15 – bottom product3 Results and discussionThe results consist ofutilization of fixed-bedexperimental runs for the catalyst activity evaluation, determination of mass transferlimitation of the chemical reaction and also for adjustment parameters for process simulation.The data were used as an input for a design of reactive-distillation column and finally, thecomplex system including pre-reactor and reactive distillation column has been adopted forprocess scale up 2 .3.1 Fixed-bed reactorThe reaction mixture was fed at atmospheric pressure to the fixed-bed reactor, filled byion-exchanger. The outlet was analyzed by GC and/or by acetic acid determination usingtitration method. The results for catalyst loading between 2 and 10 g cat .h/mol at differentreaction temperatures are given in Fig. 2.121011Figure 2: Ethanol conversionfor equimolar feed at differentreaction temperatures as afunction of catalyst loadingFor lower temperatures of 60 and 70 °C, ethanol conversion is attacking its equilibriumlimitation of 78 mass %. Recalculated to equilibrium feed composition, the equilibrium EtAcconcentration in the product equals to 64 mass %. For temperature above 76 °C, the reaction113