Data-Oriented Process Development: Determination of Reaction Parameters by Small-Scale Calorimetry with in situ Spectroscopy

Abstract

The rapid and complete characterization of chemical reaction mechanisms and their associated heat production is of the utmost importance in terms of chemical understanding and process safety and efficiency. In this contribution a new small volume (25–50 ml) combined reaction calorimeter (CRC) will be described. With this reactor it is possible to make calibration free calorimetry measurements and in situ mid-IR measurements simultaneously as well as gas consumption/production measurements in pressure-proof versions. The application of this reactor to the industrially relevant solvent free esterification of 1-butanol by acetic anhydride followed using calorimetry and mid-IR spectroscopy (a common reaction in the synthesis of many solvents, pharmaceuticals and perfumes) will be demonstrated. The results for this chemical system are presented in conjunction with a description of data analysis techniques allowing kinetic model fitting simultaneously to the different types of in situ measurements.