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Controlled/Living Radical Polymerization in the Undergraduate Laboratories. 2. Using ATRP in Limited Amounts of Air to Prepare Block and Statistical Copolymers of n-Butyl Acrylate and Styrene
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Abstract
Developments in controlled radical polymerization have facilitated the use of living polymer chemistry in the undergraduate laboratories. In the first paper of this series, a procedure for the use of atom transfer radical polymerization (ATRP) to prepare block and statistical copolymers was described and the use of kinetic analysis to differentiate between living and conventional processes was demonstrated. In this paper, the experiment is extended to polymerizations run in limited amounts of air so that the use of inert gases is unnecessary. The Cu(I) catalyst can be lost owing to oxidation or termination reactions; however, a scavenger, Cu(0), is added to react with oxidized catalyst to regenerate the Cu(I) complex. A difunctional macroinitiator of poly(n-butyl acrylate) is prepared and chain-extended with polystyrene. A statistical copolymer using the same monomer pair is also prepared. These copolymers are isolated and characterized along with the homopolymeric macroinitiator using 1H NMR and SEC. Kinetic analysis is also carried out using GC and SEC. The significant difference in these two approaches, in addition to slight variations in the reaction conditions, is apparent in the chain extension to yield the ABA triblock copolymer.
Keywords (Audience):
Upper-Division UndergraduateKeywords (Domain):
Laboratory InstructionKeywords (Pedagogy):
Hands-On Learning / ManipulativesKeywords (Subject):
ChromatographyCiting Articles
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This article has been cited by 7 ACS Journal articles (5 most recent appear below).
Polymerization Kinetics: Monitoring Monomer Conversion Using an Internal Standard and the Key Role of Sample t0
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Monitoring the Nitroxide-Mediated Polymerization of Styrene Using Gel Permeation Chromatography and Proton NMR
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Eric S. Tillman , Nathan D. Contrella and Joshua G. LeasureJournal of Chemical Education2009 86 (12), 1424This laboratory exercise is designed to give students experience in controlled radical polymerization (CRP) techniques, with an emphasis on monitoring the conversion of monomer into polymer as the reaction proceeds. Specifically, nitroxide-mediated ...
Role of Cu0 in Controlled/“Living” Radical Polymerization
Krzysztof Matyjaszewski, Nicolay V. Tsarevsky, Wade A. Braunecker, Hongchen Dong, Jinyu Huang, Wojciech Jakubowski, Yungwan Kwak, Renaud Nicolay, Wei Tang, and Jeong Ae YoonMacromolecules2007 40 (22), 7795-7806Role of Cu0 in Controlled/“Living” Radical Polymerization
Krzysztof Matyjaszewski, Nicolay V. Tsarevsky, Wade A. Braunecker, Hongchen Dong, Jinyu Huang, Wojciech Jakubowski, Yungwan Kwak, Renaud Nicolay, Wei Tang, and Jeong Ae YoonMacromolecules2007 40 (22), 7795-7806Several propositions have been made about the mechanism in which Cu0 mediates controlled radical polymerization that include (1) exclusive activation of an alkyl halide initiator by exceptionally active Cu0 to generate a propagating radical and a CuI ...
Synthesis of Chromophore-Labeled Polymers and Their Molecular Weight Determination Using UV–Vis Spectroscopy
Eric S. Tillman , Amanda C. Roof , Steven M. Palmer , Beth Ann Zarko , Caton C. Goodman and Alissa M. RolandJournal of Chemical Education2006 83 (8), 1215Synthesis of Chromophore-Labeled Polymers and Their Molecular Weight Determination Using UV–Vis Spectroscopy
Eric S. Tillman , Amanda C. Roof , Steven M. Palmer , Beth Ann Zarko , Caton C. Goodman and Alissa M. RolandJournal of Chemical Education2006 83 (8), 1215This laboratory experiment is designed to allow undergraduate students to gain experience in polymer synthesis and characterization. Polystyrene quantitatively end-labeled with fluorene is produced via atom transfer radical polymerization run under a ...
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- Received: August 03, 2009
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