BAMO-AMMO三嵌段共聚物的间接法合成及表征

Indirect Synthesis and Characterization of BAMO-AMMO Tri-Block Copolymer

以3,3′-双溴甲基环氧丁烷(BBMO)和3-溴甲基-3’-甲基环氧丁烷(BrMMO)为单体,通过活性顺序聚合法合成了BBMO-BrMMO三嵌段共聚物,并采用相转移催化法实现了3,3′-双叠氮甲基环氧丁烷-3-叠氮甲基-3′-甲基环氧丁烷(BAMO-AMMO)三嵌段共聚物的间接法合成。探讨了溶剂的选择及叠氮化反应时间的影响:选用极性和溶度参数接近的异亚丙基丙酮为溶剂,24 h后叠氮化率为99.97%。通过核磁共振(13C-NMR)和凝胶渗透色谱(GPC)对所得产物进行了表征,结果表明,共聚物组成接近于1∶1,分子量7053,分子量分布1.47。

BBMO-BrMMO tri-block copolymer was synthesized using 3,3′-bisbromomethyloxetane（BBMO） and 3-bromomethyl-3′-methyloxetane（BrMMO） by living sequence polymerization at first,indirect synthesis of 3,3′-bisazidomethyloxetane-3-azidomethyl-3′-methyloxetane（BAMO-AMMO） tri-block copolymer was then achieved through a phase transfer catalytic method.Choose of suitable solvent and the effect of reaction time on azidation was discussed emphatically.The results show that the optimal solvent is methyl isobutenyl ketone for the similar polarity and solubility parameter.Azidation degree is 99.97% after 24 h.At the same time,the product is characterized by 13C NMR and GPC.The results show that composition of BAMO-AMMO tri-block copolymer is nearly 1∶1,the molecular weight is 7053,and the molecular weight distribution is 1.47.