Polymerization-Induced Self-Assembly for the Synthesis of Polyisoprene-Polystyrene Block and Random Copolymers: Towards High Molecular Weight and Conversion.

IF 4.2 3区 化学 Q2 POLYMER SCIENCE Macromolecular Rapid Communications Pub Date : 2024-10-26 DOI:10.1002/marc.202400727
Maryam Moradi, Prokopios Georgopanos
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Abstract

In this study, reversible addition-fragmentation chain- transfer (RAFT) polymerization combined with the polymerization-induced self-assembly (PISA) technique is used to synthesize polyisoprene (PI)-based block and random copolymers with polystyrene (PS), aiming for high molecular weight and monomer conversion. The focus is to optimize the polymerization conditions to overcome the existing challenge of cross-linking and Diels-Alder reactions during the polymerization of isoprene, which typically constrain the reaction conversion and molecular weight of the final polymers. Using a poly(methacrylic acid) (PMAA) macroRAFT agent synthesized in ethanol at 80 °C, random and block copolymers of PS-PI with a target molecular weight of 50 000 g mole-1 and a high monomer conversion of ≈80% are achieved under optimized conditions in water-emulsion at 35 °C. 1H nuclear magnetic resonance (NMR) verified the successful synthesis as well as the high content of 1,4 microstructure in polyisoprene. The thermal analysis via differential scanning calorimetry indicated distinct glass transitions for the microphase-separated PI-PS block copolymer, while a single transition for PI-PS random copolymer, indicating no microphase separation. Furthermore, dynamic light scattering analysis together with transmission electron microscopy provided further insight into the self-assembled emulsion nanoparticles of the polymers indicating a particle size in the range 70 to 130 nm.

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聚合诱导自组装合成聚异戊二烯-聚苯乙烯嵌段和无规共聚物:实现高分子量和高转化率。
本研究采用可逆加成-碎片链转移(RAFT)聚合与聚合诱导自组装(PISA)技术相结合的方法,合成聚异戊二烯(PI)与聚苯乙烯(PS)的嵌段和无规共聚物,旨在获得高分子量和单体转化率。重点是优化聚合条件,以克服异戊二烯聚合过程中交联和 Diels-Alder 反应带来的挑战,这些反应通常会限制最终聚合物的反应转化率和分子量。利用在 80 °C乙醇中合成的聚(甲基丙烯酸)(PMAA)大 RFT 剂,在 35 °C水乳液中的优化条件下,实现了 PS-PI 的无规和嵌段共聚物,其目标分子量为 50 000 克摩尔-1,单体转化率高达≈80%。1H 核磁共振(NMR)证实了合成的成功以及聚异戊二烯中 1,4 微结构的高含量。通过差示扫描量热仪进行的热分析表明,微相分离的 PI-PS 嵌段聚合物有明显的玻璃化转变,而 PI-PS 无规共聚物只有一个转变,表明没有微相分离。此外,动态光散射分析和透射电子显微镜进一步揭示了聚合物自组装乳液纳米颗粒的情况,表明其粒径在 70 至 130 纳米之间。
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来源期刊
Macromolecular Rapid Communications
Macromolecular Rapid Communications 工程技术-高分子科学
CiteScore
7.70
自引率
6.50%
发文量
477
审稿时长
1.4 months
期刊介绍: Macromolecular Rapid Communications publishes original research in polymer science, ranging from chemistry and physics of polymers to polymers in materials science and life sciences.
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