三环戊二烯的合成研究

The Research on Synthesis of Tricyclopentadiene

以双环戊二烯(DCPD)为原料,在高温下与解聚生成的环戊二烯(CPD)发生Diels-Alder双烯加成反应,制备非晶型环烯烃(COC)光学材料单体三环戊二烯(TCPD)。考察了反应温度、压力和时间对加成反应的影响,确定较佳的工艺条件为:反应温度150℃,反应压力0.2 MPa,反应时间6 h。在此条件下,TCPD产品收率为82.5%(以原料DCPD计),质量分数为99.5%[面积归一化法(GC)]。产物结构经过~1H NMR和MS表征。

Tricyclopentadiene (TCPD) was synthesized from dicyclopentadiene (DCPD) and cyclopentadiene (CPD) by Diels-Alder dienes addition reaction,which was a valuable cyclic olefin monomer for optical materials.The effects of reaction temperature,pressure and time on the yield of TCPD have been investigated and the optimized conditions are as follows: the reaction temperature is 150 ℃,the reaction time is 6 h and the pressure is 0.2 MPa.Under the optimized conditions,the yield of TCPD can reach 82.5% and the purity is higher than 99.5%[ area normalization method (GC)],the impurity such as the oligomers were controlled effectively.The obtained TCPD has been identified by ^1 H NMR and MS.