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e-Polymers

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Volume 12, Issue 1

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Optimization of 4-vinylpyridine nitroxide mediated controlled radical polymerization: Effect of initiator protection and complexation with C60

Benoît H. Lessard
  • McGill University, Department of Chemical Engineering, McGill Institute of Adv. Mater. (MIAM), Centre for Self-Assembled Chemical Structures (CSACS), 3610 University Street, Montréal, Québec, Canada H3A 2B2
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/ Milan Marić
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  • McGill University, Department of Chemical Engineering, McGill Institute of Adv. Mater. (MIAM), Centre for Self-Assembled Chemical Structures (CSACS), 3610 University Street, Montréal, Québec, Canada H3A 2B2; tel: (514) 398-4272; fax: (515) 398-6678
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Published Online: 2013-08-31 | DOI: https://doi.org/10.1515/epoly.2012.12.1.741

Abstract

Nitroxide mediated polymerization (NMP) of 4-vinylpyridine (4VP) using 2-([tert-butyl[1-(diethoxyphosphoryl)-2,2-dimethylpropyl]amino]oxy)-2-methyl pro pionic acid (BlocBuilder)-derived initiators was studied. Controlled homo polymerization of 4VP using 10 mol% [tert-butyl[1-(diethoxyphosphoryl)-2,2- dimethylpropyl]amino] nitroxide (SG1) relative to BlocBuilder was limited to low conversions (X = 0.20-0.30) due to interaction between the pyridine group of 4VP and BlocBuilder’s carboxylic acid group. Converting BlocBuilder into a succinimidyl ester terminated form (NHS-BlocBuilder) resulted in 4VP polymerizations with a linear increase in number average molecular weight, M̅n, versus X to X = 0.80, while maintaining a narrow molecular weight distribution ( w/n<1.2). Final poly(4VP) samples were determined to be pseudo-“living” by subsequent chain extension with a fresh batch of 4VP, with very few dead chains. Attempts to homopolymerize 4VP in the presence of as little as 0.04 wt% C60 relative to 4VP resulted in inhibition, preventing the polymerization from exceeding beyond X = 0.40 and thus 4VP/C60 complexation has to be done post-polymerization.

About the article

Published Online: 2013-08-31

Published in Print: 2012-12-01


Citation Information: e-Polymers, Volume 12, Issue 1, 063, ISSN (Online) 1618-7229, ISSN (Print) 2197-4586, DOI: https://doi.org/10.1515/epoly.2012.12.1.741.

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