以硅氧烷基取代亚胺为封端剂原位负离子法合成官能化聚苯乙烯

Anionic Synthesis of Functionalized Polystyrenes Using Alkoxysilyl-Containing Aromatic Imine as Terminator

首先合成了含硅氧烷基的芳香亚胺封端剂N-苯亚甲基-3-三乙氧基硅烷基-1-丙胺(TEOS),然后用负离子原位聚合法合成了端基官能化聚苯乙烯PS-TEOS。采用红外光谱、核磁共振和凝胶渗透色谱对TEOS和PS-TEOS的结构进行了表征。研究了TEOS与聚苯乙烯基锂的定量反应关系,以及TEOS加入量、反应温度、反应时间及PS相对分子质量对封端效率的影响。结果表明,封端反应在10 min^5 min内快速完成,封端反应温度在55℃~80℃、PS的珚Mn在5000~50000范围内变化对封端效率影响不大,制备的PS-TEOS的官能度在80%以上,实现了TEOS与聚苯乙烯基锂等摩尔封端反应。

The novel kind of alkoxysilyl-containing aromatic imine terminator,N-benzylidene-3-( triethoxysilyl)-1-propanea mine( TEOS) was synthesized firstly,and then end functionalized polystyrene( PS-TEOS) was prepared via anionic in-situ polymerization by the reaction of poly( styryl) lithium with TEOS. The terminator and functionalized PS were characterized by FT-IR,1H-NMR and GPC. The quantitative reaction relationship between TEOS and poly( styryl) lithium,and the influence of the TEOS content,reaction temperature,reaction time,number-average relative molecular mass of poly( styryl) lithium on the functionality were investigated. The results show that TEOS can react with poly( styryl) lithium stoichiometrically and the terminating reaction was completed in 10 min ~ 15 min,terminating temperature at55 ℃ ~ 80 ℃ and 珚Mnof poly( styryl) lithium at 5000 ~ 50000 have no significant effect on the functionality of PS. The functionalized PS with high functionality( > 80%) was prepared with TEOS as terminator.