Development, Validation, and Application of a Custom-Made Mini-Reaction Calorimeter for Thermal Safety Screening

Abstract

Before scaling up to production, it is of high importance to evaluate the potential of a reaction to lead to an undesired thermal degradation event. The use of a large amount of compounds is usually required for a reliable calorimetry study. In this work, we report the development of a milliliter-scale reaction calorimeter for reaction screening applications. The setup was designed using laboratory equipment and characterized and validated with routine experiments. The results were sufficiently accurate enabling us to observe trends in the measured reaction enthalpies of a family of compounds reacting with strong bases as a function of the compounds' structures.. The use of the microscale tailor-made calorimeter is considered very valuable for potentially highly energetic reactions since reaction calorimetry studies can be performed accurately and safely with small amounts of valuable materials.

Thermal Safety and Structure-Related Reactivity Investigation of Five-Membered Cyclic Sulfamidates

“…Therefore, we developed in-house a mini-reaction calorimeter with a minimum volume of 300 μL (Figure ) that supports the systematic and reproducible recording of the reaction heat when mixing cyclic sulfamidates with bases (Figure ). The prototype was validated by two well-known model reactions, the hydrolysis of acetic anhydride and the dilution of H 2 SO 4 , and all further tests showed high repeatability and robustness . First, compound 1 that initiated this study was tested with different types of bases diluted in an appropriate solvent allowing for an homogeneous mixture (e.g., acetonitrile).…”