Continuous Flow Cobalt‑mediated Radical Polymerization of Vinyl Acetate and Hydrolysis of Polyvinyl Acetate to get Polyvinyl Alcohol: Concurrent Control and Purification
摘要
Controlled radical polymerization (CRP) is a typical procedure for the synthesis of polymers with well-defined molecular parameters (Mn, Đ), composition, and architecture. However, control of the radical polymerization of vinyl acetate (VAc) and removal of residual metallic controlling agents from polyvinyl acetate (PVAc) remains a concern. Herein, tubular reactor connected to fixed bed of silica gel particles is designed for continuous flow cobalt-mediated radical polymerization (CMRP) of VAc and incessant separation of residual cobalt acetylacetonate (Co(acac)2) from product to get purified PVAc with well-defined molecular parameters. Linear polymerization time dependence of Ln[M]0/[M] and ascent of molecular weight (Mn) with the rise in conversion while keeping narrow polydispersity (Đ ≈ 1.5) revealed the CRP of VAc in the continuous flow process. The free Co(acac)2 from the polymer matrix was adsorbed by fixed bed of silica gel, resulting in pure PVAc with a decolorization efficiency (DE) of 65%. In addition, the obtained PVAc was hydrolysed to get polyvinyl alcohol (PVA) with isotactic triads (mm) of 26%, higher to compared with mm of 22% of PVA produced by saponification of PVAc obtained in the absence of Co(acac)2. This study therefore provides continuous flow process, an innovative strategy, to produce purified PVAc with well controlled molecular parameters without requiring additional purification steps and enabling technical assistance for potential large-scale practicability.