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Fractionation and DOSY NMR as analytical tools : from model polymers to a technical lignin

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acsomega.7b01287.pdf (1.467Mb)
Date
30/11/2017
Author
Montgomery, James
Lancefield, Christopher Stuart
Miles-Barrett, Daniel
Ackermann, Katrin
Bode, Bela Ernest
Westwood, Nicholas James
Lebl, Tomas
Keywords
QD Chemistry
DAS
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Abstract
One key challenge hindering the valorization of lignin is its structural complexity. Artificial lignin-like materials provide a stepping stone between the simplicity of model compounds and the complexity of lignin. Here, we report an optimized synthesis of an all-G β-O-4 polymer 1 designed to model softwood lignin. After acetylation, the polymer Ac-1(V) was fractionated using a protocol that involved only volatile organic solvents, which left no insoluble residue. Using diffusion ordered spectroscopy NMR in combination with gel permeation chromatography, it was revealed that this fractionated material behaved like a flexible linear polymer in solution (average α > 0.5). Acetylated kraft lignin was subsequently processed using the same fractionation protocol. By comparison with the model polymer, we propose that the acetylated kraft lignin is composed of two classes of materials that exhibit contrasting physical properties. One is comparable to the acetylated all-G β-O-4 polymer Ac-1, and the second has a significantly different macromolecular structure.
Citation
Montgomery , J , Lancefield , C S , Miles-Barrett , D , Ackermann , K , Bode , B E , Westwood , N J & Lebl , T 2017 , ' Fractionation and DOSY NMR as analytical tools : from model polymers to a technical lignin ' , ACS Omega , vol. 2 , no. 11 , pp. 8466-8474 . https://doi.org/10.1021/acsomega.7b01287
Publication
ACS Omega
Status
Peer reviewed
DOI
https://doi.org/10.1021/acsomega.7b01287
ISSN
2470-1343
Type
Journal article
Rights
© 2017 American Chemical Society. This is an open access article published under a Creative Commons Attribution (CC-BY) License, which permits unrestricted use, distribution and reproduction in any medium, provided the author and source are cited.
Description
This work was supported by EPSRC Ph.D. studentships (EP/ 1518175 (DMB) and EP/1654168 (JRDM)), the Industrial Biotechnology Innovation Centre (Ph.D. studentship to DMB), and an EPSRC Doctoral Prize Fellowship (CSL).
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  • University of St Andrews Research
URL
http://pubs.acs.org/doi/suppl/10.1021/acsomega.7b01287
URI
http://hdl.handle.net/10023/12221

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