Contactless Raman Spectroscopy-Based Monitoring of Physical States of Silyl-Modified Polymers during Cross-Linking

Abstract

Cross-linking of silyl-modified polymers occurs at the alkoxysilane groups attached to the ends of polymer chains by hydrolysis and polycondensation mechanisms in the presence of moisture. During these reactions, three different physical states can be identified (viscous, skin effect and cross-linked state). Knowledge of the evolution of these states at each reaction time is essential to determine the open time for the adhesive industry and is generally obtained by a manual method. Automation of this monitoring could avoid operator error and could be used for very long cross linking reactions or to screen a large number of catalysts. Thus, a contactless micro process technology was developed to correlate these physical states with an optical technology, Raman spectroscopy, by monitoring the decrease in intensity of the Si-OCH3 groups during chemical reactions. This online characterization method can also be used to compare the efficiencies of several catalysts for the cross-linking of silyl-modified polymers, using a minimum amount of chemical materials.