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Acetone‐induced polymerisation of 3‐aminopropyltrimethoxysilane (APTMS) as revealed by NMR spectroscopy
Author(s) -
Mazzei Pierluigi,
Fusco Luigi,
Piccolo Alessandro
Publication year - 2014
Publication title -
magnetic resonance in chemistry
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.483
H-Index - 72
eISSN - 1097-458X
pISSN - 0749-1581
DOI - 10.1002/mrc.4076
Subject(s) - chemistry , reactivity (psychology) , acetone , nuclear magnetic resonance spectroscopy , siloxane , imine , proton nmr , spectroscopy , fluorine 19 nmr , two dimensional nuclear magnetic resonance spectroscopy , hydrolysis , carbon 13 nmr satellite , polymer chemistry , organic chemistry , catalysis , stereochemistry , medicine , physics , alternative medicine , pathology , quantum mechanics , polymer
We followed the reactivity of acetone with 3‐aminopropyltrimethoxysilane, a potential organosilane coupling agent, by 1 H, 13 C and 29 Si NMR spectroscopy. Selective 1D and 2D‐edited NMR experiments significantly contributed to simplify the spectral complexity of reaction solution and elucidated molecular structures within progressive reaction phases. The course of the 3‐aminopropyltrimethoxysilane reaction with acetone was shown by a progressive decrease of both reactants, and a concomitant appearance of water and methanol, due to formation of imine and hydrolysis of alkoxysilane groups, respectively. The occurrence of multiple siloxane linkages in a progressively larger cross‐linked macromolecular structure was revealed by DOSY‐NMR experiments and new signals in 29 Si‐NMR spectra at different reaction times. The NMR approach described here may be applied to investigate the reactivity of other γ‐aminopropylalkoxysilanes and contribute to define procedures for the preparation of silica‐based materials. Copyright © 2014 John Wiley & Sons, Ltd.