Research Of Process Of Preparation Of Bicyclopentadiene Dioxide By Peroxo Phosphotungstate

Aims to solve the problems of higher cost, complicated reaction process, product hydrolysis and ring-opening easily and environment pollution in industrial production of acid dicyclopentadiene dioxide (DCPDD), this paper used green, pollution-free hydrogen peroxide as the oxygen source, environmental friendly heteropoly acid as catalyst, discussed the catalytic effect of the three catalyst and determined the best catalyst and process conditions1.The peroxo phosphotungstate was synthesized and then used as to oxidize dicyclopentadiene into dicyclopentadiene diepoxide with H2O2. The optimal oxidation conditions at55℃for14h were as follows:hydrogen peroxide concentration was55%; acetone dosage was75mL; DCPD was0.14mmol; n (H2O2):n (DCPD) was1.85; catalyst amount was1.01mmol. Yield of target production and conversion of DCPD was82.23%and98.8%respectively. The catalyst was characterized by IR.2.When using MCM-41loaded peroxo phosphotungstate as catalyst and hydrogen peroxide as the oxygen source for DCPDDO preparation. The optimal reaction conditions were:55%hydrogen peroxide; tert-butanol120mL; DCPD0.18mmol; n (H2O2):n (DCPD)=2.0; catalyst dosage1.25; the loading35%; reaction at63℃for7h. The yield of DCPDDO is91.2%and conversion of DCPD is99.1%under optimal epoxidation conditions. The catalytic activity is still very good even after4times reaction. The catalyst was characterized by IR and XRD.3.When using activated carbon loaded peroxo phosphotungstate as catalyst and hydrogen peroxide as the oxygen source for DCPDDO preparation. The optimal reaction conditions were:1.35mmol catalyst with loading rate of25%; hydrogen peroxide concentration55%; DCPD0.20mmol; n (H2O2):n (DCPD)=2.2; reaction at68℃for5h. The yield of DCPDDO is88.2%and conversion of DCPDD is99.3%under optimal epoxidation conditions. The catalyst still had high catalytic activity even after5times reaction. The catalyst was characterized by IR.4.The activated carbon loaded peroxo phosphotungstate was synthesized and then used as to oxidize dicyclopentadiene into dicyclopentadiene diepoxide using continuous reacting unit. The optimal oxidation conditions at60℃for110h were as follows:flow was90mL/h; n(H2O2):n(DCPD) was2.6; volume ratio of solvent and DCPD was4.0. The conversion of DCPD was92.2%and yield was70.2%under optimal epoxidation conditions.