Synthesis and Characterization of a Novel Amphiphilic Azo Block Copolymer

Can-qiang YANG; Yu ZHU; Xiao-gong WANG

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Synthesis and Characterization of a Novel Amphiphilic Azo Block Copolymer

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- Synthesis and Characterization of a Novel Amphiphilic Azo Block Copolymer
- Polymer Bulletin Vol. 25, Issue 5, Pages: 70-75(2012)
- 作者机构：
  
  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　100084
- 作者简介：
- 基金信息：
- DOI：
  CLC：
- Published：2012-05，
  
  Received：15 November 2011，
  
  Revised：13 December 2011，
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Can-qiang YANG, Yu ZHU, Xiao-gong WANG. Synthesis and Characterization of a Novel Amphiphilic Azo Block Copolymer. [J]. Polymer Bulletin 25(5):70-75(2012)
DOI：

Can-qiang YANG, Yu ZHU, Xiao-gong WANG. Synthesis and Characterization of a Novel Amphiphilic Azo Block Copolymer. [J]. Polymer Bulletin 25(5):70-75(2012) DOI：

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-

-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-（

-甲基苯胺基）己酯进行ATRP反应，得到前体聚合物 P（HEMA-TMS-

-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-

-6CNAzo）。利用GPC、UV-Vis、

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-

-6MA）均具有较窄的分子量分布。

H-NMR分析结果表明，P（HEMA-TMS-

-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-

-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。

Abstract

A novel amphiphilic block copolymer functionalized with strong push-pull azobenzene moieties

P(HEMA-

-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-

-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-

-6CNAzo)

was obtained by azo-coupling reaction between P(HEMA-TMS-

-6MA) and diazonium 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

H-NMR and UV-vis. GPC results showed that both P(HEMA-TMS) and P(HEMA-TMS-

-6MA) had narrow molecular weight distributions.

H-NMR analysis indicated that the ratio of polymerization degree for HEMA andP6MA blocks is 0.95∶1. 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-

-6CNAzo) with the concentration of 0.2g/L

the amphiphilic 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

Keywords

Azo polymerBlock copolymerAmphiphilicSynthesisCharacterization

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