Simple Procedure for Optimal Scale-up of Fine Chemical Processes. II. Nitration of 4-Chlorobenzotrifluoride

Abstract

In this work, a simple and general procedure for optimally scaling-up exothermic semibatch processes has been applied to the analysis of a nitration reaction performed in the agrochemical industry for the production of an important class of herbicides. Such a reaction is performed in indirectly cooled semibatch reactors in which the species to be nitrated is added to a mixture of sulfuric and nitric acid, forming a heterogeneous (liquid−liquid) system. Adiabatic calorimetric experiments performed in an ARC equipment showed that the reaction in question belongs to the most critical class of exothermic reaction processes, for which maximum attainable temperature due to synthesis reaction (MTSR) is, at the same time, higher than system decomposition temperature and lower than boiling temperature of the reaction mass. It has been verified, through reaction calorimetry experiments (performed in an RC1 equipment), that the optimization−scale-up procedure previously developed allows, with minimum calculation and experimental effort, both for a selection, at laboratory scale, of operating conditions characterized by a rapid coreactant consumption and for their safe scale-up, maximizing industrial reactor productivity.