一种含假芪型偶氮生色团两亲性嵌段共聚物的合成与表征  

Synthesis and Characterization of a Novel Amphiphilic Azo Block Copolymer

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作  者:杨灿强[1] 朱煜[1] 王晓工[1] 

机构地区:[1]清华大学化工系高分子研究所教育部先进材料重点实验室,北京100O84,北京100084

出  处:《高分子通报》2012年第5期70-75,共6页Polymer Bulletin

基  金:国家自然科学基金项目(91027024)

摘  要:利用原子转移自由基聚合(ATRP)合成了一种新型的含假芪型偶氮生色团的两亲性嵌段共聚物P(HEMA-b-6CNAzo)。首先,采用ATRP引发剂引发三甲基硅保护的羟乙基甲基丙烯酸酯(HEMA-TMS)聚合,得到大分子引发剂P(HEMA-TMS);接着进一步引发单体甲基丙烯酸6-(N-甲基苯胺基)己酯进行ATRP反应,得到前体聚合物P(HEMA-TMS-b-6MA)。最后,将前体聚合物与4-氰基苯胺的重氮盐进行重氮偶合反应,同时在强酸作用下使三甲基硅保护基团水解,得到目标聚合物P(HEMA-b-6CNAzo)。利用GPC、UV-Vis、1 H-NMR等手段对制备的聚合物进行了详细的表征。GPC结果表明,P(HEMA-TMS)与P(HEMA-TMS-b-6MA)均具有较窄的分子量分布。1 H-NMR分析结果表明,P(HEMA-TMS-b-P6MA)两嵌段的聚合度比为0.95∶1,重氮偶合反应转化率及三甲基硅基团的水解程度均接近100%。往浓度为0.2g/L的聚合物P(HEMA-b-6CNAzo)的THF溶液中,以1μL/s的速率滴加去离子水,该两亲性嵌段共聚物可自组装形成粒径为60~80nm的聚集体。A novel amphiphilic block copolymer functionalized with strong push-pull azobenzene moieties, P(HEMA-b-6CNAzo), was synthesized by using ATRP. First, the macromolecular initiator P (HEMA-TMS) was prepared through ATRP reaction of monomer HEMA-TMS, which was hydroxylethyl-mathacrylate (HEMA) protected with trimethylsilane (TMS) groups. Then, the precursor diblock copolymer, P(HEMA-TMS-b-6MA), containing aniline groups was prepared by a P (HEMA-TMS)-initiated ATRP of 6-(N-methylanilino)hexyl methacrylate. The amphiphilic azo block copolymer, P(HEMA-b-6CNAzo), was obtained by azo-coupling reaction between P(HEMA-TMS-b- 6MA) and cliazonium salt of 4-aminobenzonitrile and the TMS groups were removed at the same time because of the acidic conditiond. The macro-initiator and block copolymers were characterized by GPC, 1H-NMR and UV-vis. GPC results showed that both P (HEMA-TMS) and P (HEMA-TMS-b-6MA) had narrow molecular weight distributions. 1H-NMR analysis indicated that the ratio of polymerization degree for HEMA andP6MA blocks is 0. 95. The conversion rate of azo-coupling reaction and hydrolysis Of TMS groups were close to 100%. By adding deionized water under a rate of 1μL/s to a THF solution of P (HEMA-b-6CNAzo) with the concentration of 0.2g/L, the amphiphilie block copolymers self-assembled to form colloidal spheres with sizes in range from 60 and to 80nm.

关 键 词:偶氮聚合物 嵌段共聚物 两亲性 合成 表征 

分 类 号:O631.3[理学—高分子化学]

 

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