Acrylamide precipitation polymerization in a continuous flow reactor: an in situ FTIR study reveals kinetics

Abstract

In this work, we present a combination of a continuous flow reactor with in situ monitoring of the monomer conversion in a precipitation polymerization. The flow reactor is equipped with a preheating area for the synthesis of thermoresponsive microgels, based on N-isopropylacrylamide (NIPAM). The reaction progress is monitored with in situ FTIR spectroscopy. The monomer conversion at defined residence times is determined from absorbance spectra of the reaction solutions by linear combination with reference spectra of the stock solution and the purified microgel. The reconstruction of the spectra appears to be in good agreement with experimental data in the range of 1710 to 1530 cm− 1, in which prominent absorption bands are used as probes for the monomer and the polymer. With increasing residence time, we observed a decrease in intensity of the ν(C=C) vibration, originating from the monomer, while the ν(C=O) vibration is shifted to higher frequencies by polymerization. Differences between the determined inline conversion kinetics and offline growth kinetics, determined by photon correlation spectroscopy (PCS), are discussed in terms of diffusion and point to a crucial role of mixing in precipitation polymerizations.Graphical Continuous flow syntheses of acrylamide-based microgels in combination with in situ FTIR spectroscopy and offline particle characterization reveal information about the reaction progress.