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以α-蒎烯为原料合成冰片烯。以冰片烯(BE)、二氧化硫(SO2)为单体,采用自由基聚合方法合成了冰片烯-二氧化硫聚砜树脂(BE-SO2),用同样的方法分别以冰片烯(BE)、二氧化硫(SO2)、马来酸酐为单体和以冰片烯(BE)、二氧化硫(SO2)、苯乙烯(St)为单体,合成冰片烯-二氧化硫-马来酸酐(BE-SO2-M a)以及冰片烯-二氧化硫-苯乙烯(BE-SO2-St)两种三元共聚物。讨论了单体配比、聚合反应的温度和时间对共聚物得率的影响,结果表明:n(BE)1 mmol,n(BE)∶n(M a)1∶1,n(BE)∶n(St)1∶1,加入4 mL CYC作溶剂,在-20℃条件下反应4 h,BE-SO2,BE-SO2-M a,BE-SO2-St得率最高,分别为70%、64%和71%。此外,分别用FT-IR、GPC、DSC、EA和SEM等方法对共聚物结构进行了表征,BE-SO2为粉末状黑色固体,重均相对分子质量(Mw)为1 069,数均相对分子质量(Mn)为376,Tg为134.5℃;BE-SO2-M a共聚物为粉末状黑褐色固体,Mw为1 576,Mn为402,Tg为152.0℃;BE-SO2-St共聚物为粉末状黄褐色固体,Mw为33 054,Mn为952,Tg为174.8℃。
Synthesis of norbornene from α-pinene. The isoprene-sulfur dioxide polysulfone resin (BE-SO2) was synthesized by the free-radical polymerization method using borneol (BE) and sulfur dioxide (SO2) ), Maleic anhydride as monomer and norbornene-sulfur dioxide-maleic anhydride (BE-SO2-M a) and norbornene as monomers with norbornene (BE), sulfur dioxide (SO2) and styrene (St) - Sulfur dioxide - styrene (BE-SO2-St) two terpolymers. The effects of monomer ratio, polymerization temperature and time on the yield of copolymer were discussed. The results showed that the molar ratio of n (BE): n (BE): n (M a) 1: n The yields of BE-SO2, BE-SO2-M a and BE-SO2-St were the highest with 70%, respectively, when 4 mL of CYC was added as the solvent. 64% and 71%. In addition, the copolymer structures were characterized by FT-IR, GPC, DSC, EA and SEM, respectively. BE-SO2 was a powdery black solid with a weight average molecular weight (Mw) of 1 069, The copolymer was BE-SO2-M a powdery dark brown solid with a Mw of 1 576, a Mn of 402 and a Tg of 152.0 ° C; the BE-SO2-St copolymer was a powder A tan solid, Mw 33 054, Mn 952, Tg 174.8 ° C.