The following two procedures describe two ATRP polymerization reactions as performed by Prof. Dave Hadddleton′s research group at the University of Warwick.
Figure 1.Polymerization of methylmethacrylate (MMA) with N-propyl-2-pyridylmethanimine, where 1a = N-propyl-2-pyridylmethanimine
The polymerization is carried out under oxygen free conditions. First the transition metal salt is deoxygenated and then the solution, followed by adding initiator to start the polymerization:
Samples can be removed at 30-60 minute intervals using a degassed syringe and analyzed by GC or NMR to determine the extent of conversion and SEC for molecular weight and polydispersity (PDI). After 300 minutes, the poly(methylmethacrylate) (PMMA) is isolated with a final conversion of 89.3 %. Mn = 8,760 g mol-1 (theoretical Mn = 8,930 g mol-1), PDI = 1.20.
Figure 2.Polymerization of styrene with N-pentyl-2-pyridylmethanimine, where 1b = N-pentyl-2-pyridylmethanimine
The polymerization is carried out under oxygen free conditions. First the transition metal salt is deoxygenated, and then the monomer and initiator are added to the solution and deoxygenated, followed by adding ligand to start the polymerization:
Samples can be removed at 30-60 minute intervals using a degassed syringe and analysed by GC or NMR for conversion and SEC for molecular weight and polydispersity (PDI). The reaction was stopped after 360 minutes, with a final conversion of 77.9 %. Mn = 5,270 (theoretical Mn = 7,900 g mol-1), PDI = 1.29.
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