Controlled/Living Radical Polymerization in the Undergraduate Laboratories. 1. Using ATRP to Prepare Block and Statistical Copolymers of n-Butyl Acrylate and Styrene

Kathryn L. Beers and Krzysztof Matyjaszewski
Department of Chemistry, Carnegie Mellon University, Pittsburgh, PA 15213
Brian Woodworth
PPG Industries, Inc., Alison Park, PA 15101
J. Chem. Educ., 2001, 78 (4), p 544
DOI: 10.1021/ed078p544
Publication Date (Web): April 1, 2001

Abstract

A simple method of preparing well-defined (co)polymers has been developed for application in an advanced undergraduate laboratory. The method utilizes atom transfer radical polymerization (ATRP), a controlled/living radical polymerization, to prepare difunctional poly(n-butyl acrylate) with bromine end groups, which is chain-extended with styrene to yield an ABA triblock copolymer. Simultaneously, a statistical copolymer of the two monomers is prepared for comparison. The two copolymers are isolated and compositions and molecular weights are determined using 1H NMR and SEC, respectively. Optional additions to the experiment include performing a kinetic analysis of the homopolymerization using GC and SEC, and possibly comparing the results to those expected for conventional radical polymerization. Material differences in the copolymers can be observed qualitatively or measured using thermal or mechanical analysis. The lab is designed in such a way that several parts of the whole can be used to emphasize different areas of polymer science. A more synthetic course such as the organic synthesis lab can opt to investigate only the kinetic and composition analyses, whereas an engineering or materials science course may pursue more rigorous analysis of the materials' properties. Results included here are intended for application in an organic synthesis laboratory course.

Keywords (Audience):

Upper-Division Undergraduate

Keywords (Domain):

Laboratory Instruction

Keywords (Pedagogy):

Hands-On Learning / Manipulatives

Keywords (Subject):

Catalysis

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  • Received: August 03, 2009

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