Chlorinated Solvent-Free Living Cationic Ring-Opening Polymerization of Epichlorohydrin Using BF 3 •OEt 2 as Co-Initiator: Toward Perfectly Functionalized Poly(epichlorohydrin) Diols - Archive ouverte HAL Accéder directement au contenu
Article Dans Une Revue ACS Applied Polymer Materials Année : 2023

Chlorinated Solvent-Free Living Cationic Ring-Opening Polymerization of Epichlorohydrin Using BF 3 •OEt 2 as Co-Initiator: Toward Perfectly Functionalized Poly(epichlorohydrin) Diols

Résumé

The cationic ring-opening polymerization of epichlorohydrin co-initiated by BF 3 •Et 2 O has been investigated here. Fast synthesis of pure poly(epichlorohydrin) diols (F n (OH) ≈ 2.0) with controlled molar mass (M n 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 BF 3 •Et 2 O-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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hal-04257779 , version 1 (25-10-2023)

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Georgy V Timofeev, Maksim I Hulnik, Irina V Vasilenko, Francois Ganachaud, Guy Jacob, et al.. Chlorinated Solvent-Free Living Cationic Ring-Opening Polymerization of Epichlorohydrin Using BF 3 •OEt 2 as Co-Initiator: Toward Perfectly Functionalized Poly(epichlorohydrin) Diols. ACS Applied Polymer Materials, 2023, 5 (8), pp.6549-6561. ⟨10.1021/acsapm.3c01105⟩. ⟨hal-04257779⟩
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