Safety Management Safety Management DSC • Determination of: - Temperature of decomposition - Energy of decomposition - Material compatibility • Determination of: - Heat of reaction - Maximum Temperature of Synthesis Reaction - Thermal accumulation DSC Tp: Temperature of Process MTSR: Maximum Temperature for Synthesis Reaction TMRad: Time to reach maximal rate of decomposition ASSESSMENT PROCESS SAFETY PROCESS SAFETY If high energy of decomposition is detected, complementary tests are needed: • Thermokinetic modeling of decomposition reaction • Shock sensitiveness • Friction sensitivity • Sensitivity to intense heat under confinement... PROCESS DEVELOPMENT Safety report Meeting R&D, HSE, production Evaluation of customer process safety data PROCESS OPTIMIZATION SCALE-UP PRODUCTION TECHNICAL PACKAGE Safety data acquisition Transfer protocol Modeling Scale-up evaluation TD24: Temperature at which time to maximum rate is 24h (decomposition temperature) ΔTad: Adiabatic Temperature Rise CALORIMETRIC STUDIES CALORIMETRIC STUDIES Temperature / °C DSC / (W/g) Energy: 1637 J/g Onset: 111°C Peak: 140°C Power: 8.8 W/g 50 10 10 5 5 0 100 150 200 250 300 350 PREVENT MITIGATE OPERATE TIME TEMPERATURE Normal process Cooling failure t 0 T proess TMR ad MTSR t 2 t 1 Tad r Tad d Desired reaction Undesired reaction (Decomposition) SCALE-UP EVALUATION SCALE-UP EVALUATION • Criticality index assessment • Determination of temperature and feed rate • Cooling capacities assessment for an exothermic reaction • Evaluation of heat transfer at production scale • Risk analysis performed on site (HAZOP) • Definition of safety barriers during reaction, work-up, distillation, drying 55 50 45 40 35 30 25 20 15 10 5 0 -5 002:40:00 Ti (°C), Tr (°C) Acetic anhydride. Total Mass (g) Thermal Conversion (qr_hf)2(%) qr_hf(W) 16 24 32 20 28 38 18 26 34 36 22 30 40 28 26 24 22 20 18 16 14 12 10 8 6 4 2 0 -2 100 90 80 70 60 50 40 30 20 10 0 002:50:00 003:00:00 003:10:00 003:20:00 003:30:00 003:40:00 003:50:00 004:00:00 Thermal conversion Heat of reaction Reaction temperature Jacket temperature Reagent dosing RC1 Optimax Easymax