基于碘介导可控自由基聚合精准制备聚甲基丙烯酸酯的综合实验设计  

Comprehensive experimental design of precise preparation of polymethacrylate based on iodine mediated controlled radical polymerization

作　　者：肖龙强 邓称怀 侯琳熙 XIAO Longqiang;DENG Chenhuai;HOU Linxi(College of Chemical Engineering,Fuzhou University,Fuzhou 350116,China;Qingyuan Innovation Laboratory,Quanzhou 362801,China)

机构地区：[1]福州大学石油化工学院,福建福州350116 [2]清源创新实验室,福建泉州362801

出　　处：《实验技术与管理》2022年第9期197-201,共5页Experimental Technology and Management

基　　金：国家自然科学基金项目(U21A20313);福建省自然科学基金项目(2019J05040);清源创新实验室重点项目(00221003)。

摘　　要：针对现有聚甲基丙烯酸酯精准合成技术存在金属催化剂残留及产品颜色化问题,设计了有机小分子催化的碘介导可控自由基聚合反应综合实验,合成了分子量精确可控、具有极窄分子量分布的聚合物。通过核磁共振氢谱、凝胶渗透色谱考察了聚合反应动力学行为和所得聚合物的分子量及分量分散系数。并将所合成的聚合物作为大分子引发剂继续引发单体聚合,核磁共振氢谱和凝胶渗透色谱结果证明了所得聚合物具有优异的端基活性。该实验涉及有机合成、高分子合成及反应动力学行为研究,对促进可控自由基聚合的学习及实验教学起到了很好的作用。Aiming at the problems of metal catalyst residue and product colorization in the existing precise synthesis technology of polymethacrylate, a comprehensive experiment of iodine mediated controlled radical polymerization catalyzed by organic small molecules was designed, and a polymer with accurately controllable molecular weight and extremely narrow molecular weight distribution was synthesized. The kinetic behavior of the polymerization reaction and the molecular weight and component dispersion coefficient of the obtained polymer were investigated by NMR and gel permeation chromatography. The synthesized polymer was used as a macromolecular initiator to further initiate monomer polymerization. The results of NMR and gel permeation chromatography showed that the obtained polymer had excellent end group activity. The experiment involves the study of organic synthesis, polymer synthesis and reaction kinetic behavior, which plays a good role in promoting the learning and experimental teaching of controllable free radical polymerization.

关 键 词：综合性实验 可控自由基聚合 动力学 嵌段共聚物 碘介导 

分 类 号：O631.5[理学—高分子化学]