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Process safety assesment using adiabatic and reaction calorimetry for sodium borohydride as reducing agent in methanol Sigurnosna procjena reaktanta natrij borhidrida kao reducensa u metanolu korištenjem adijabatske i reakcijske kalorimetrije Dario Klarić1, Sebastijan Orlić1, Franjo Jović1, Eugen Marcelić1 1 Pliva Hrvatska d.o.o., TAPI R&D, API Pilot [email protected] Process safety assesment is a key aspect of process development with a goal of safely transfering a process to production, without any kind of hazard or risk. The main focus of research was made on the thermal risk that comes out of unwanted, secondary reactions which occur when process conditions are uncontrolled, whether the cooling of the reactor has failed, or taking into account different rates of heat and mass transfer during the process scale-up. Reaction calorimetry (RC-1), adiabatic calorimetry (ARRST) and process simulators (Dynochem, Visimix) are usefull tools in obtaining data and process understanding. Reaction calorimetry is a technique for gathering valuable kinetic data of exothermic and endothermic events which give insight into process safety and hazard analysis by quantifying the enthalpy of the reaction. Adiabatic calorimetry is used for testing the process in conditions that are uncontrolled, by heating the reaction mixture with a constant heat ramp while monitoring exothermic events. In our research, exothermic reaction with significant pressure generation that occurs when using sodium borohydride as a reducing agent in methanol as a solvent was examined. Sodium borohydride is a commercially available reagent which is commonly used for the selective reduction of organic molecules. It is readily soluble in water and alcohols during which hydrogen and heat (ΔrH>300 kJ/mol) are being released. The reaction measurements were conducted using Mettler Toledo RC-1 reactor at 0-5oC under atmospheric pressure. Using adiabatic calorimetry it was concluded that no unwanted reactions occur which allowed the prediction of safe conditions in case of unstable reaction conditions. With the data obtained from those tools, process simulators are used to build reaction models that include wanted and unwanted reactions, allowing us to build scenarios that could bring the process into dangerous and unstable conditions.