Polymerization Initiated by Graphite Intercalation Compounds Revisited: One-Pot Synthesis of Amphiphilic Pentablock Copolymers †

This study reports the first attempt to employ a potassium–graphite intercalation compound (KC₂₄) as an initiator for the one-pot synthesis of a multi-block copolymer. The results obtained show that KC₂₄ successfully initiated the copolymerization, leading to a copolymer consisting of poly(styrene), poly(methyl methacrylate) and poly(ethylene oxide) blocks. When all three comonomers were introduced simultaneously or in a specific sequence, the resulting copolymers had molecular masses in the range between 170,000 Da and 280,000 Da. Their composition was investigated by size-exclusion chromatography with triple detection (dRI/UV/IR) and ¹H-NMR. The analyses indicated that all copolymers were enriched in methyl methacrylate (50–66 mol%) despite the fact that the comonomers were added in equimolar amounts. Due to the layered structure of the initiator, the polymerization took place in the graphite interlayer spaces and lead to extensive delamination, indicating at the potential to produce in situ graphite/copolymer composite materials.