Research Of The Novel Process Of The Preparation Of Bicyclopentadiene Dioxide

This thesis based on the actual industrial production, from the perspective of environmental protection, for the past over the traditional production of acid dicyclopentadiene dioxide (DCPDD) of the existence of serious corrosion of equipment, the reaction process more complicated, too acidic easily lead to the acidity of epoxide ring-opening led to an increase in by-products such as inadequate, the use of green, pollution-free hydrogen peroxide as the oxygen source, relatively small damage to the environment and good catalytic effect on the load-type heteropoly acid as a catalyst to discuss three catalytic effect, explore and study the suitable for industrial production of green catalytic synthesis of production processes. In determining the best catalyst and process conditions, the establishment of a continuous device DCPDD production.1. With titanium silicalite as a catalyst, hydrogen peroxide as the oxygen source of DCPD catalyzed epoxidation reaction:optimal conditions for the 10mlDCPD, 40ml50% hydrogen peroxide, tert-butanol as solvent, reaction at 65℃for 14 hours. DCPD conversion rate is 99% or more, DCPDD selectivity is 35%.2. With phosphotungstic acid as a catalyst, hydrogen peroxide as the oxygen source in the reaction system catalyzed DCPD Epoxy:The optimal conditions for the 10mlDCPD,20ml50% hydrogen peroxide, tert-butanol as solvent, reaction at 60℃for 12 hours. DCPD conversion rate is to 99% or more, DCPDD selectivity is to 90%. In the condition of absent solvent, the direct reaction of hydrogen peroxide and DCPD to get the product directly to the solid white precipitate, washed with distilled water and drying the product obtained by gas chromatography, the purity of 98% or more.3. The supported heteropoly acid as a catalyst, hydrogen peroxide as the oxygen source of the reaction catalyzed DCPD Epoxy:The optimal conditions for the 10ml DCPD,50ml 50% hydrogen peroxide, tert-butanol as solvent, reaction at 65℃for 12 hours under. DCPD conversion rate is 99% or more, DCPDD selectivity is 55%. Catalyst can be reused six times, and no significant reduction in catalytic capacity.4. Based on the obtained optimum conditions, the establishment of a continuous production of equipment for DCPDD. Get the best of raw materials into the amount of rate of 3ml/h, for 72 hours to achieve the best system, the reaction one week after the conversion of DCPD and DCPDD selectivity decreased gradually, through the analysis of major element content can be seen is due to the loss of W.