Monitoring of chemical reactions during polymer synthesis by real‐time attenuated total reflection (ATR)–FTIR spectroscopy

Abstract

ABSTRACT:The present study demonstrates in situ realtime attenuated total reflection (ATR)-FTIR spectroscopy as a powerful tool for monitoring and analyzing different polymerization and polymer modification reactions. Thus, a metallocene catalyzed copolymerization of propene and 10-undecene-1-ol, a polycondensation reaction towards polysulfone, and a modification reaction of OH end groups of hyperbranched poly(urea-urethane) were investigated successfully. The interpretation of the development of FTIR spectra was carried out on the basis of typical vibration bands of chemical groups of the corresponding monomers and polymers in each case, e.g. of the CAC double bond of 10-undecene-1-ol during the copolymerization, the new COOOC group of polysulfone, and the new urethane end group of poly(urea-urethane). Kinetics prediction is also under consideration.

Synthesis and characterization of polysulfone based on poly(ethylene terephthalate) waste

“…The characteristic band of CACl stretching vibration of DCDPS at 1089 cm 21 decreased during the chemical reaction. This decrease is due to the depletion of the labile chlorine atom [20,21]. The band at 3423 cm 21 was characteristic for the stretching frequency of AOH group, which is broad and intense especially in the product B due to the existence of hydrogen bonding.…”

Online Monitoring of Polymerizations: Current Status

“…[17] In situ attenuated total refection Fourier transform infrared (ATR-FTIR) spectroscopy was also employed to study the kinetics of carbocation-and ring-opening-polymerization processes as well as metallocene-catalyzed copolymerizations, polycondensations, and post-polymerization modifications ( Figure 1). [18][19][20] Figure 1. Decrease in absorbance at 1635 cm -1 and FTIR waterfall profiles showing the disappearance of the 1640-1620 cm -1 vibrations upon monomer conversion, corresponding to the vinyl bond of the acrylate monomer, upon the photoinduced SUMI reaction.…”

Kinetic Studies of Metallocene‐Catalyzed Copolymerization of Propene with 10‐Undecene‐1‐ol Using In‐Line FTIR Spectroscopy

“…The qualitative tracing of this copolymerization with respect to changes in chemical structures was published in former times. [8] In the polymerization of propene the metallocene catalyst systems offer control over regio-and stereoregularities, molecular weights, polydispersities, and they allow polar comonomer incorporation and that in a higher extent compared to the classical Ziegler-Natta catalysts. Poly(propylene) (PP) is well-known as non-polar polymer with excellent mechanical properties, but with only weak interactions to other compounds.…”

“…The in-line monitoring system is able to detect changes in chemical structures and to determine reaction rates by the monitoring of relevant signals in the spectroscopic fingerprint mid infrared range (4 000-650 cm À1 ). [1][2][3][4][5][6][7][8][9] The continuous real-time generation of analytical data allows observing the chemical process at the best resolution per time unit. The changes in reaction parameters are directly identifiable and consequently it will be possible to take corresponding actions in real time.…”