2,5-降冰片二烯的制备

该文对以双环戊二烯(DCPD)和乙炔为原料,经Diels Alder反应制备2,5 降冰片二烯(NBD)的工艺进行了研究。在高压釜内考察了反应工艺条件和产品的提纯。较理想的反应条件为:反应温度180～190℃、n(乙炔)/n(DCPD)≥1 18、m(丙酮)/m(DCPD)≥1 8,此时,以DCPD计算的转化率≥80%,NBD选择性在40%左右。反应液的精馏在15块理论塔板的填料塔中进行,当绝对压力为39 51～51 36kPa、回流比为2∶1、塔釜温度在130℃以下时,得到的产品质量分数为99 5%。

Preparation of 2,5-Norbornadiene

2,5-Norbornadiene (2,5-NBD) was prepared by the Diels-Alder reaction of dicyclopentadiene (DCPD) and acetylene in an autoclave.The reaction conditions and the purification of the product were also investigated.The conversion of DCPD was about 80% and the selectivity for 2,5-NBD was no less than 40% at 180～190 ℃,with the molar ratio of acetylene to DCPD≥1.18 and the mass ratio of acetone to DCPD≥1.8.When rectificating the reaction mixture in a packed column with 15 theoretical plates under an absolute pressure of 39.51～51.36 kPa at reflux ratio of 2∶1 and the bottom temperature below 130 ℃,the purity of 2,5-NBD obtained was as high as 99.5%.