Apparent kinetics study and efficient continuous-flow synthesis of tert-butyl hydroperoxide & tert-butyl peroxybenzoate in a microreaction system

This study advances the synthesis of tert-butyl hydroperoxide (TBHP) and tert-butyl peroxybenzoate (TBPB) using a continuous microreaction system, meticulously detailing kinetic behavior and optimization processes through over 1250 experimental data points. We have developed a platform capable of high-throughput kinetic experiments and precise reaction quenching, determining kinetic parameters and optimal conditions that significantly improve reaction efficiency and safety. Tailored microreaction strategies, including micro-mixers, plate microreactors, and micro-packed beds, were employed to manage exothermic reactions and enhance mass transfer for each peroxide. For TBHP, conditions were optimized to achieve a 99% conversion rate of tert-butanol and an 82% conversion of hydrogen peroxide, with product selectivity reaching 92%. For TBPB, under optimal conditions, benzoyl chloride conversion reached 99.5%, and TBHP conversion was 80%, with a product selectivity of 94%. The integration of the TBHP and TBPB synthesis processes into a single continuous-flow system demonstrates scalable, safe, and efficient production, highlighting significant potential for advancements in organic peroxide manufacturing.