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Living anionic polymerization of alkyl methacrylates initiated by 1,1-diphenylhexyllithium was conducted in a flow microreactor system. A high level of molecular-weight distribution control was achieved under easily accessible conditions, such as at −28 °C (MMA: Mw/Mn = 1.16), 0 °C (BuMA: Mw/Mn = 1.24) and 24 °C (Bu t MA: Mw/Mn = 1.12). The molecular weight (Mn) increased with an increase in the monomer/initiator ratio. The subsequent reaction of a reactive polymer chain end with a second alkyl methacrylate in integrated flow micoreactor systems led to the formation of a block copolymer having narrow molecular-weight distribution.

The polystyrene living polymer end, which was produced by butyllithium initiated anionic polymerization of styrene in a flow microreactor system was found to be effectively trapped with 1,1-diphenylethylene. The resulting organolithium species could be used as a macro initiator for anionic polymerization of alkyl methacrylates to obtain styrene−alkyl methacrylate diblock copolymers using an integrated flow microreactor system. A high level of control of molecular weight was achieved at easily accessible temperatures such as +24 to −28 °C by virtue of the fast mixing, fast heat transfer, and residence time control. Triblock copolymers were also synthesized by sequential introduction of styrene and two different alkyl methacrylates in a similar manner.