用不同结构三乙氧基硅烷为原料,通过水解缩合和环氧化的方法合成了环氧基苯基低聚笼型倍半硅氧烷,再利用胺基和环氧开环反应与聚醚胺反应合成 POSS 基嵌段共聚物(PEA-POSS),最后将苯基结构羧酸化合成两亲性嵌段共聚物(PEA-POSS-COOH).利用傅里叶变换红外光谱(FT-IR)和核磁共振氢谱(1H-NMR)表征了PEA-POSS-COOH的化学结构.采用溶剂挥发诱导法促使PEA-POSS-COOH自组装,形成以疏水POSS为核、亲水PEA链为壳的球形胶束.利用扫面电子显微镜(SEM)、能量分散型X射线光谱(EDS)、动态激光光散射(DLS)、小角 X 射线散射仪(XRD)和差示扫描量热仪(DSC)表征了组装体的形貌与结构性能.结果表明,POSS基两亲性嵌段聚合物可组装成粒径约1.14 μm的球形胶束,且POSS结构中的π-π堆叠作用使得球形胶束具有较为稳定结构,熔点提高.
Synthesis of POSS-based Amphiphilic Block Copolymers and Their Self-assembly Behavior
Epoxy-based phenyl polyhedral oligomeric silsesquioxanes(POSS)were synthesized by hydrolytic condensation using different structures of triethoxysilanes as raw materials,and then POSS-based block copolymers(PEA-POSS)were synthesized by reaction of the amine group and epoxy ring-opening reaction with the polyether amine(PEA),and finally amphiphilic block copolymers(PEA-POSS-COOH)were synthesized by carboxylating the phenyl structure.The structural compositions of PEA-POSS-COOH were characterized using Fourier-transform infrared(FT-IR)and nuclear magnetic resonance hydrogen spectroscopy(1H-NMR).The PEA-POSS-COOH were self-assembled to form spherical micelles with hydrophobic POSS as the cores and hydrophilic PEA chains as the shell by the solvent evaporation-induced method.The morphology and structure properties of the assemblies were investigated by scanning electron microscopy(SEM),energy dispersive X-ray spectroscopy(EDS),dynamic light scattering(DLS),small-angle X-ray scattering(XRD),and differential scanning calorimetry(DSC).These results show that the POSS-based amphiphilic block polymers can be assembled into spherical micellar structures with a particle size of about 1.14 μm,and the π-π stacking effect in the POSS structure makes the spherical micelles have a more stable structure with an increased melting point.
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