Lu Group

The widely adopted synthesis route of EC is the cyclopropanation reaction between 2,5-dimethyl-2,4-hexadiene and ethyl diazoacetate(EDA) catalyzed by transition metal, but it suffers from low production efficiency, low utilization of hexadiene and hard-to-scale up. In this work, we introduce the flow synthesis technology into the synthesis of EC, whose characteristics include rapid mixing, enhanced heat and mass transfer, security and so on. The synthesis platform has been set up successfully to realize continuous synthesis of EC and the equimolar reaction of hexadiene and EDA. Combined with a variety of characterization methods, the experimental phenomena were explained to deepen the understanding of the kinetic characteristics of this reaction.

Homogeneous synthesis of hydroxylamine hydrochloride was established in this work by adding the by-product formic acid to reaction mixture. Based on the homogeneous system, stop-flow microtube reactor was used to investigate the hydrolysis reaction characteristics and to develop the corresponding semi-empirical kinetics equation. It was discovered that water and acid imposed different and complex effect on the hydrolysis reaction rate in two separate intervals of acid concentration. Kinetics models were established in this two regions respectively and showed a good agreement with experimental data. Under the optimized conditions, the reaction time was greatly shorten to four hours for reaching 90 % conversion of NM at 110 ^oC . The high consistence of stop-flow reactor and continuous flow reactor in reaction performances was experimentally confirmed.