Synthesis of dicetyl peroxydicarbonate of high assay in microreactorby using response surface methodology
Volume Title: 1
1Polymer Eng. And Color Tech. Dept., Amirkabir University of Technology, 424 Hafez Ave., POBox: 15875-4413, Tehran, Iran
2Department of Polymer Engineering and Color Technology, Amirkabir University of Technology
Dicetyl peroxydicarbonate, as a solid peroxide, is conventionally synthesized in a two-phase batch or semi-continuous reactors and contains 6-8 wt.% impurities due to side reactions. The present study aimed to use a flow-focusing microreactor to prepare this peroxide with high yield and purity from the reaction of cetyl chloroformate and hydrogen peroxide. The clogging problem of the microreactor with solid peroxy particles was solved by selecting an appropriate reaction temperature, enabling the synthesis of dicetyl peroxydicarbonate with very high yield (ca. 100%) and assay (>99.5%) in a very short time (<45 s) and safe conditions. We also evaluated the effects of some important process and formulation parameters on reaction yield, by using response surface methodology. The flow rate in the microreactor was determined to be the most significant effect on the reaction yield. Finally, the optimum values for the flow rate, surfactant concentration, and ethanol concentration were calculated as 290 µL/min, 2.6 wt.%, and 27 vol.%, respectively.
Solid dialkyl peroxydicarbonate; high assay; microreactor; flow-focusing; Response surface methodology