RAFT发剂的制备及PCL-b-PEG嵌段共聚物的合成和自组装

Preparation of RAFT Initiator and Synthesis and Self-assembly of PCL-b-PEG Block Copolymers

首先制备含有双官能团的引发剂2-(苄基硫烷基硫羰基硫烷基)乙醇(BSTSE),而后以BSTSE为引发剂,分两步合成了聚己内酯-b-聚丙烯酸酯聚乙二醇羧基(PCL-b-PEG),并进行自组装。利用核磁共振波谱仪氢谱(~1H-NMR)、傅立叶变换红外光谱仪(FT-IR)、ZS-90激光粒度仪(DLS)、透射电子显微镜(TEM)和扫描电子显微镜(SEM)等仪器对产物进行结构和形貌分析。结果表明:本研究合成的BSTSE引发剂纯度为83.3%,形成胶束性能最好的PCL-b-PEG嵌段共聚物的嵌段比为25∶45。DLS、SEM和TEM测试表明其形成的胶束粒径分布均一,尺寸在100 nm左右。

Bifunctional initiator 2-(benzylsulfanylthiocarbonylsulfanyl)ethanol(BSTSE) was prepared,and then polycaprolactone-block-plyacrylate polyethylene glycol carboxyl group(PCL-b-PEG)was synthesized in two steps using BSTSE as an initiator,and self-assembly.The structure and morphology of the product were analyzed by Nuclear magnetic resonance spectroscopy(~1H-NMR),Fourier transform infrared spectroscopy(FT-IR),ZS-90 laser particle size analyzer(DLS),transmission electron microscopy(TEM),and scanning electron microscopy(SEM).The results showed that the purity of the BSTSE initiator synthesized in this study was 83.3%.The block ratio of the PCL-b-PEG block copolymer which formed micelle the most properties was 25:45.DLS,SEM and TEM tests showed that the micelles formed were uniform in particle size distribution and the size was around 100 nm.