环氧氯丙烷
阳离子聚合
聚合
单体
高分子化学
分散性
聚合物
摩尔质量
开环聚合
溶液聚合
本体聚合
化学
离子聚合
材料科学
自由基聚合
有机化学
作者
Georgy V. Timofeev,Maksim I. Hulnik,Irina V. Vasilenko,François Ganachaud,Guy Jacob,Sergei V. Kostjuk
出处
期刊:ACS applied polymer materials
[American Chemical Society]
日期:2023-07-12
卷期号:5 (8): 6549-6561
标识
DOI:10.1021/acsapm.3c01105
摘要
The cationic ring-opening polymerization of epichlorohydrin co-initiated by BF3•Et2O has been investigated here. Fast synthesis of pure poly(epichlorohydrin) diols (Fn(OH) ≈ 2.0) with controlled molar mass (Mn up to 4000 g mol–1) and low dispersity (Đ < 1.25) was performed both in toluene and in bulk. An original approach was developed here, consisting of first generating in situ the initiator through the BF3•Et2O-catalyzed reaction of ECH with water, leading to a mixture of oligomers with better solubility in the reaction medium than conventional initiators previously used. Then, through a second monomer starved-feed step, polymerization proceeds exclusively through the activated monomer mechanism, allowing perfect control of the polymer growth. The developed procedure was successfully upscaled to 100 g of polymer to validate a future industrial production of PECH, as well as its derivative glycidyl azide polymer (GAP), the most important energetic binder for solid propellants. Additionally, a separate study was performed to elucidate the reasons for coloration of the polymer observed in the course of polymerization and/or under storage.
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