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Combination of nuclear magnetic resonance spectroscopy and nonlinear methods to analyze the copolymerization of phosphonic acid derivatives
Author(s) -
Heinze Marcus,
Starke Sandra,
Händler Marcel,
Komber Hartmut,
Drache Marco,
Moszner Norbert,
Voit Brigitte,
Pospiech Doris
Publication year - 2019
Publication title -
journal of applied polymer science
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.575
H-Index - 166
eISSN - 1097-4628
pISSN - 0021-8995
DOI - 10.1002/app.48256
Subject(s) - copolymer , reactivity (psychology) , monomer , polymer chemistry , materials science , methacrylate , nuclear magnetic resonance spectroscopy , monte carlo method , polymer , chemistry , organic chemistry , mathematics , composite material , medicine , alternative medicine , statistics , pathology
We demonstrate in this study that the combination of modern inline monitoring methods [here: inline nuclear magnetic resonance (NMR)] with simulations gains more exact and profound kinetic results than previously used methods like linearization without that combination. The 1 H‐NMR spectroscopic data (more than 100 data points) are used to construct the copolymerization diagram. The reactivity ratios are obtained applying the van Herks nonlinear least square method. The examination of the radical copolymerization of 2‐hydroxyethyl methacrylate (HEMA) with (2‐{[2‐(ethoxycarbonyl)prop‐2‐en‐1‐yl]oxy}ethyl) phosphonic acid (ECPPA) as important adhesive monomer used in dentistry yields reactivity ratios of r HEMA = 1.83; r ECPPA = 0.42. The copolymerization diagram reflects nonideal, non‐azeotropic copolymerization. The sequence distribution of the obtained by Monte Carlo simulation indicates the generation of statistical copolymers. As an important finding, it is demonstrated that the repeating units responsible for etching and adhesion are arranged over the whole polymer chain, which is necessary to achieve proper functionality. © 2019 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2019 , 136 , 48256.