首先合成了单取代的β环糊精ATRP引发剂(β-CD-Br),利用核磁、质谱等对其进行了表征,并通过ATRP聚合制备了端基为β-环糊精的水溶性聚合物聚甲基丙烯酸N,N-二甲基氨基乙酯(β-CD-PDMAEMA).聚合物β-CD-PDMAEMA可以通过环糊精与金刚烷之间的主客体包结络合作用与端基为金刚烷的聚芴(PFADA)形成水溶性的聚芴纳米粒子.重点探讨了β-CD-PDMAEMA与PF-ADA的质量比和不同的组装方法对纳米粒子尺寸及分布的影响,研究表明质量比为4∶1时通过向2种聚合物的THF混合溶液中缓慢加水的方法可得到流体力学半径(Rh)为80 nm、PDI为0.11的纳米粒子.最后利用透射电子显微镜和原子力显微镜对纳米粒子的形貌进行了表征,进一步依照纳米粒子的R_h随温度升高的实验可以证实纳米粒子具有明显的核壳结构,其中刚性的聚芴为核半径约为50 nm,水溶性的PDMAEMA聚合物为壳.
First,the ATRP initiator monosubstituted β-CD-Br was successfully prepared,which was confirmed by~1H-NMR and MALDI-TOF. And then the water-soluble polymer( β-CD-PDMAEMA) modified with β-CD at the one end was synthesised by ATRP polymerization. The β-CD-PDMAEMA and PF-ADA can form watersoluble nanoparticle( PF-NP) via the host-guest inclusion complexation between β-CD and adamantane( ADA) as driving force. Dynamic light scattering( DLS) was employed to measure the effect of weight ratio ofβ-CD-PDMAEMA/PF-ADA on Rhand PDI of PF-NP. The DLS results show that the weight ratio of β-CDPDMAEMA/PF-ADA with 4∶ 1 could form smaller nanoparticle,the Rhis 119 nm. As well as four diffent selfassembly methods impact on character of nanoparticles were also focused,while fixing the weight ratio of β-CDPDMAEMA/PF-ADA at 4 ∶ 1. When 4 m L water was slowly injected into 1 m L THF solution of β-CDPDMAEMA and PF-ADA under ultrasonication,the Rhof nanoparticle is equal to 81 nm. Transmission electron microscopy( TEM) and atomic force microscopy( AFM) were used to exam the morphology of nanoparticles.The results from TEM and AFM show that the nanoparticles are spherical with diameter of 100 nm,which is smaller than the results observed from DLS measuements. It is well-known that PDMAEMA chains exhibit a coil-to-globule transition above their lower critical solution temperature( LCST) in water solution. At last,the Rhof nanoparticles decreases with temperature increase. All these results show that the nanoparticles have the PF polymer as the core,with diameter of 100 nm and the PDMAEMA polymer as the shell with thick ness of 30 nm.