Automated parallel anionic polymerizations: Enhancing the possibilities of a widely used technique in polymer synthesis

Abstract

Anionic polymerization techniques have been implemented successfully in a commercial automated synthesizer. The main problems for a successful adaptation of the experimental technique in the automated synthesizer are addressed, as well as some simple potential applications, such as the anionic polymerization of styrene, isoprene, and methyl methacrylate. The obtained results were reproducible and in concordance with literature knowledge. The apparent rate constant of the anionic polymerization of styrene in cyclohexane initiated by sec‐butyllithium could be determined at two different concentrations of the monomer and initiator in a temperature range of 10–60 °C. All the synthesis and characterization experiments of the polymers were performed within a short time period. Moreover, the syntheses of poly(styrene‐b‐isoprene) and poly(styrene‐b‐methyl methacrylate) block copolymers were also successfully carried out within the automated synthesizer. © 2005 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 43: 4151–4160, 2005

Ability of nitrones of various structures to control the radical polymerization of styrene mediated by in situ formed nitroxides

“…In the high-throughput experimentation, pre-reactions and polymerizations were carried out with a Chemspeed ASW 2000 automated synthesizer and 15 ml reactors blocks (equipped with a heating/cooling jacket and coldfinger reflux condensers) [47]. Addition of compounds and sampling of the polymerization medium were performed with the fully automated liquid handling system of the synthesizer.…”

Combinatorial and High‐Throughput Methods in Macromolecular Materials Research and Development

“…[22][23][24][25] They have demonstrated the parallel synthesis of polyoxazolines, [26][27][28] anionic polymerization, [22,29,30] emulsion polymerization, [31] the synthesis of polymers using controlled-radical polymerization methods such as atom-transfer radical polymerization (ATRP) [32][33][34][35][36] and reversible addition-fragmentation chain transfer (RAFT). [22,32,37,38] In addition, they have explored the synthesis of block copolymers, [39] star polymers, [40,41] and supramolecular polymers.…”

Protocol for Automated Kinetic Investigation/Optimization of the RAFT Polymerization of Various Monomers

“…However, the type of monomer or catalyst can be varied and an analogous version of this protocol can equally be applied for other polymerization reactions, i.e., ATRP [25], NMP [24], anionic [26], and cationic ring opening polymerization [27], with some additional precautions depending on the oxygen and water sensitivity of the polymerization technique. This protocol is a step-by-step procedure that is applicable in the automated parallel synthesizer platform.…”