摘要: 以 2-(十二烷基三硫代碳酸酯) -2-甲基丙烯酸为链转移剂,利用 RAFT/ 细乳液联合技术合成了相对分子质量分布较窄(PDI = 1.53)的大分子链转移剂聚甲基丙烯酸缩水甘油酯。 再以该大分子为可逆加成-断裂链转移(RAFT)试剂,通过连续加料的方式加入苯乙烯后进一步引发聚合,得到 PGMA-b-PS 二嵌段共聚物。 采用 GPC、FT-IR、1H-NMR、DSC 等方法对聚合产物进行了表征。 结果表明:合成的聚合物为线型二嵌段共聚物,相对分子质量分布为 1.87,该聚合过程具有活性/可控特征。 DSC 测得二嵌段共聚物具有 2 个玻璃化转变温度(Tg),分别为 77.33 ℃和 98.30 ℃ 。 此外,还考察了单体加料顺序对聚合过程的影响。
关键词:
可逆加成-断裂链转移(RAFT)自由基聚合,
细乳液聚合,
嵌段共聚物,
聚苯乙烯,
聚甲基丙烯酸缩水甘油酯
Abstract: Poly(glycidyl methacrylate)( PGMA)with narrow polydispersity(PDI=1.53) was synthesized in microemulsion system by reversible addition-fragmentation chain transfer(RAFT)polymerization, in which 2-( dodecylthio)-2-methyl propionic acid was used as the chain transfer agent. Then poly(glycidyl methacrylate )-b-poly( styrene)(PGMA-b-PS)diblock copolymer was synthesized using styrene as the second monomer,where the styrene were added by continuous loading method. The effect of monomer-feeding sequence on polymerization was investigated. The diblock copolymers were characterized by gelpermeation chromatography (GPC), indicating that a linear diblock copolymers with molecular mass polydispersity (PDI) of 1. 87 was synthesized. The structure of the copolymer was confirmed by infrared spectrometry (FT-IR and nuclear magnetic resonance spectroscopy(H-NMR). The glass transition temperature(Tg)(77.33℃ and 98. 30 ℃)of the diblock copolymer was measured by differential scanning calorimetry (DSC).
Key words:
reversible addition-fragmentation chain transfer polymerization(RAFT);microemulsion polymerization,
diblock copolymer polystyrene;poly(glycidyl methacrylate
张 梁, 郭长昊, 李晓芳, 宫希杰, 叶妮雅, 李海英, 雷良才. PGMA-b - PS 二嵌段共聚物的RAFT/细乳液合成及表征[J]. 涂料工业, 2014, 44(7): 18-24.
Zhang Liang, Guo Changhao, Li Xiaofang, Gong Xijie, Ye Niya, Li Haiying, Lei Liangcai. Synthesis and Characterization of PGMA-b - PS Diblock Copolymer by RAFT/Microemulsion Polymerization[J]. Paint & Coatings Industry, 2014, 44(7): 18-24.