High-Resolution 13C and 1H Solution NMR Study of Poly(lactide)

Khalid A. M. Thakur,* Robert T. Kean, Eric S. Hall, Jeffrey J. Kolstad, and Tim A. Lindgren
Cargill Incorporated, Central Research, P.O. Box 5699, Minneapolis, Minnesota 55440
Matthew A. Doscotch, J. Ilja Siepmann, and Eric J. Munson*
Department of Chemistry, University of Minnesota, 207 Pleasant Street SE, Minneapolis, Minnesota 55455
Macromolecules, 1997, 30 (8), pp 2422–2428
DOI: 10.1021/ma9615967
Publication Date (Web): April 21, 1997
Copyright © 1997 American Chemical Society
*

In papers with more than one author, the asterisk indicates the name of the author to whom inquiries about the paper should be addressed.

Abstract

High-resolution 500 MHz solution-state 1H and 13C NMR spectra of various poly(lactides) indicate at least hexad stereosequence sensitivity. The poly(lactides) were prepared in vials by melt polymerization of various combinations of l-lactide, d-lactide, and meso-lactide at 180 °C for 3 h using tin(II) bis(2-ethylhexanoate) (tin(II) octoate) as the catalyst in a 1:10 000 ratio. The intensity distribution of the various stereosequence resonances in the NMR spectra indicates a preference for syndiotactic addition during the polymerization process. Minimal evidence of transesterification was observed for these polymerization conditions.

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History

  • Published In Issue April 21, 1997
  • Received October 28, 1996
    Revised Manuscript Received January 15, 1997

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