Thermokinetic analyses of metal-sensitive reactions in a ceramic flow calorimeter

Abstract

Measuring the thermokinetic data of chemical reactions is an important part for chemical process development. However, some reactions are very sensitive to the presence of metals, limiting the use of standard materials for calorimeters. In this work we present a flow calorimeter employing a 3D printed ceramic reactor plate for the measurement of metal-sensitive reactions. The calorimeter was characterized by residence time measurements aided by mixing simulations, and was validated via a standard neutralization reaction, an aggressive nitration reaction, and a binary solvent system for mixing enthalpy, before being used for a nitrosylation reaction featuring a metal sensitive product.