在常压、惰性气体保护下,用正丁基锂(n-BuLi)引发苯乙烯阴离子聚合,在添加荆无水三氯化铝的存在下,用环氧氯丙烷(ECH)对聚苯乙烯阴离子进行封端反应,制得分子量约为5×10^3的末端带环氧基团的聚苯乙烯低聚物。用GPC、FT—IR、^1H—NMR及盐酸-二氧六环银量法对低聚物进行了表征,并考察了添加剂、封端反应的温度和时间对环氧端基含量的影响。结果表明:加入添加剂和降低封端温度有利于环氧端基含量的提高,在0℃左右封端效率较高,封端反应时间以1.0h为宜。
The living poly(styryl)lithium was formed by anionic polymerization with the protection of argon under nomal pressure, where styrene, cyclohexane, THF and n-butyllithium were used as monomer, solvent, polar reagent and initiator respectively. Then epoxy-terminated polystyrene oligomer with a molecular weight about 5 000, was systhesized by termination reaction of the poly (styryl) lithium with epichlorohydrin(ECH) over anhydrous aluminum chlorate as additive. The oligomer was characterized by GPC, FT-IR, ^1H-NMR and hydrochloric acid-dioxane argentimetric method. Effects of aluminum chlorate, termination temperature and time on the content of epoxy end group were studied. Results show that the termination efficiency increases with the addition of aluminum chlorate together with the decrease of termination temperature. The optimized termination temperature is 0 ℃ and the best termination time is 1 h.