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合成了缩酮保护的一代甲基丙烯酸羟乙酯单体DHEMA(G1),通过顺序ATRP聚合方法,制备得到大分子引发剂PDHEMA(G1)-Br,再引发苯乙烯单体得到一代嵌段聚合物PDHEMA(G1)-b-PS.以PDHEMA(G1)-b-PS为反应前体,通过重复的缩酮保护和脱保护反应,进一步得到了二代和三代的树状化-线形两亲嵌段聚合物PDHEMA(Gn-OH)-b-PS(n=2～3).IR和1H-NMR表征结果证实了两亲嵌段聚合物的生成.在DMF/CH3 OH溶液组装体系中,当CH3 OH含量为50 wt%时,PDHEMA(G1-OH)-b-PS、PDHEMA(G2-OH)-b-PS和PDHEMA(G3-OH)-b-PS均形成核壳结构的球形胶束,且随树状化嵌段代数的增加,球形胶束尺寸也相应增大.对于PDHEMA(G3-OH)-b-PS,当CH3OH含量增加到66 wt%时,出现支化结构和环形结构的棒状胶束复合体与少量球形胶束共存,继续增加CH3OH含量到75 wt%,只能观察到支化和环形结构的棒状胶束复合体.研究认为,在棒状胶束生长过程中同时存在支化作用和成环作用是棒状胶束复合体中多环结构形成的主要原因.
Synthesis of a ketal-protected hydroxyethyl methacrylate monomer DHEMA (G1), by sequential ATRP polymerization method to prepare a macro-initiator PDHEMA (G1) -Br, re-initiator of styrene monomer to give a generation of block polymerization PDHEMA (G1) -b-PS. The second and third generations of dendron-linear amphiphiles were further obtained by repeated ketal protection and deprotection using PDHEMA (G1) -b-PS as the reaction precursor The block copolymer PDHEMA (Gn-OH) -b-PS (n = 2 ~ 3) was confirmed by IR and 1H-NMR characterization.Among the DMF / CH3OH solution assembly system, PDHEMA (G1-OH) -b-PS, PDHEMA (G2-OH) -b-PS and PDHEMA (G3-OH) -b-PS all formed spherical core-shell structure when CH3OH content was 50 wt% And the size of the spherical micelles increased with the increase of dendritic block algebra.For PDHEMA (G3-OH) -b-PS, when the CH3OH content increased to 66 wt%, the branching structure and the ring shape appeared The structure of the rod-shaped micelle complexes and a small amount of spherical micelles co-exist, continue to increase the CH3OH content to 75 wt%, only the branched and ring-shaped rod micelles complex observed .Studies, in the process of rod micelles growth Branching and ringing exist A rod-like micelles is the main composite body formed by a multi-ring structure.