Monitoring of lignin-based polyurethane synthesis by FTIR-ATR

FTIR-ATR (Fourier Transform Infrared Spectroscopy working in the mode of Attenuated Total Reflectance) was applied to study the formation of lignin-based polyurethanes. Although some studies related to the use of lignin in polyurethane synthesis, are available in literature, still persist a gap for a systematic study of this kind of systems, involving the measurement of kinetic data, modelling and optimization of the polymerization process. The present methodology allows the test of different formulations at a scale of 3-5 g, considering several process variables: temperature, NCO/OH ratio, type and average molecular weight of the polyol, type of isocyanate, type and weight content of lignin. This work aims to describe the methodology used to perform the FTIR experiments by presenting a case study. The polyurethane samples have been prepared starting with 4,4'-methylene-diphenylene isocyanate (MDI), policaprolactonediol (PCL) of three different average molecular weights (1000, 750 and 400) and a commercial lignin (Indulin AT from Meadwestvaco) at different weight contents (10, 15, 20 and 25%). The results obtained in this work point out for the validation of the proposed experimental technique and confirm that lignin was incorporated in the final three-component polyurethane sample by chemical reaction with isocyanates, i.e., formation of urethane linkages. (c) 2007 Elsevier B.V All rights reserved.