β-环糊精基刺激响应星形聚合物的制备及其响应行为
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1.东北石油大学;2.东北石油大学提高油气采收率教育部重点实验室

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国家自然科学基金重点项目(51834005);黑龙江省应用技术研究与开发计划项目(GA20A201);吉林大学无机合成与制备化学国家重点实验室开放项目;东北石油大学提高采收率教育部重点实验室开放项目;东北石油大学化学工程与技术优势特色学科青年学术骨干支持计划


Synthesis of β-CD-Based Stimuli-Responsive Star-Shaped Polymers and Its Response Behavior
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National Nature Science Foundation of China (project no. 51834005), Applied Technology Research and Development Program Project in Heilongjiang Province (GA20A201), Open Project Fund of State Key Laboratory of Inorganic Synthesis & Preparative Chemistry Jilin University, Open Project Fund of Key Laboratory of Enhanced Oil and Gas Recovery of Ministry of Education of Northeast Petroleum University, Support Program for Research Talents in Chemical Engineering and Technology of Northeast Petroleum University

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    摘要:

    本文采用单电子转移活性自由基聚合法(SET-LRP)合成星形嵌段聚合物,以改性环糊精(Br-β-CD)为引发剂,溴化亚铜/三-(2-二甲氨基乙基)胺(CuBr/Me6TREN)原位歧化得到的初生零价铜(Cu0)及二价铜与配体的络合物(CuIIBr2/Me6TREN)为催化体系,在室温下成功实现了N-异丙基丙烯酰胺(NIPAM)、甲基丙烯酸二甲氨基乙酯(DMAEMA)的水相活性自由基聚合。通过扩链反应(DP=50-100)研究了这一聚合反应的活性特征。结果表明,单体转化率在30 min内可达100%且聚合产物分子量分布(PDI)小于1.55。为了证明这一方法可制备多嵌段刺激响应性的凝胶材料,通过连续加料链延伸的方法,分别加入温敏单体NIPAM,温度及pH双重刺激响应单体DMAEMA,合成了嵌段聚合物PNIPAM100-b-PDMAEMA100。产物只需要在最后一步提纯,链延伸后的PDI均小于1.55。用1H NMR和FT-IR对聚合物结构进行了表征。所得的刺激响应聚合物在选择性溶剂中自组装,用浊度法、透射电镜研究了星形共聚物的响应行为,可组装成立体楔形结构及球形结构,且星形聚合物具有良好的抗疲劳性。

    Abstract:

    We report herein the synthesis of a novel star-block copolymer by single-electron-transfer living radical polymerization (SET-LRP). The polymerization of NIPAM and DMAEMA were carried out at room temperature in aqueous solution, using Br-β-CD as iniator, full in situ disproportionation of CuBr/Me6TREN to Cu(0) powder and CuIIBr2/Me6TREN as catalyst system. Conditions for iterative block formation have been optimized for an N-isopropylacrylamide star-shaped polymer, which was prepared with DP=50–100 with full conversion in 30 min with polydispersity index (PDI) <1.55. To demonstrate this approach for true block stimuli-responsive copolymer materials, a well-defined block polymer PNIPAM100-b-PDMAEMA100 has been prepared in high purity, with purification only required in the final step. The PDI after each chain extension was below 1.55. The polymer has been characterized by FTIR spectroscopy and 1H NMR spectrometry. The responsive behaviors of the block-star copolymer have been studied by turbidity measurements and transmission electron microscopy. the star-block copolymer showed a strong thermal response and formed three-dimensional wedge assemblies and spherical micelles . And the star-shaped polymer has good fatigue resistance.

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  • 收稿日期:2021-12-27
  • 最后修改日期:2022-04-27
  • 录用日期:2022-06-18
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