Evidence of Liquid-Liquid Demixing During Bi-Soft  Segment Polyurethane Prepolymerization

Christian Wenning; Jens Noe; Stéphan Barbe; Marc C. Leimenstoll

Macromolecular Research, Vol.26, No.5, 395-398, May, 2018

DOI10.1007/s13233-018-6065-5 Export Citation

Evidence of Liquid-Liquid Demixing During Bi-Soft Segment Polyurethane Prepolymerization

Christian Wenning, Jens Noe, Stéphan Barbe, and Marc C. Leimenstoll^†

Macromolecular Chemistry and Polymertechnology, TH Köln, Kaiser-Wilhelm-Allee E39, 51368 Leverkusen, Germany

E-mail:

Bi-soft segment isocyanate-terminated polyurethanes (ITPUs) currently play a major role in the industrial production of high performance polyurethanes (adhesives, coating, foams, thermoplastics, nanoparticles, dispersion). The present contribution reports on the investigation of liquid-liquid demixing phenomena during the synthesis of bi-soft segment ITPUs. For this purpose, a dedicated experimental setup based on coupled in-line reaction monitoring via UV/Vis and FTIR technique was developed. It was used to monitor phase separation and reaction progress in the course of a prepolymerization using 1,6-hexamethylene diisocyanate and a polyether polyol mixture. Such phenomena may have a great impact on reaction kinetics and product quality. Furthermore, in-line FTIR analysis appeared to be sensitive to phase separation processes in the way that it predominantly detects the continuous phase rather than the dispersed droplets.

Keywords:bi-soft segment isocyanate-terminated polyurethanes;ITPUs;liquid-liquid demixing;UV/VIS;FTIR

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[2] Meier-Westhues U, Polyurethane: Lacke, Kleb- und Dichtstoffe, Technologie des Beschichtens, Vincentz Network, Hannover, 2007.

[3] Adhikari R, Gunatillake PA, McCarthy SJ, Meijs CF, J. Appl. Polym. Sci., 78(5), 1071 (2000)

[4] Hsu DY, Chou CM, Chuang CY, Hong PD, ACS Macro Lett., 4, 1341 (2015)

[5] Matuszak ML, Frisch KC, J. Polym. Sci. A: Polym. Chem., 11, 637 (1973)

[6] McNaught AD, Wilkinson A, IUPAC. Compendium of Chemical Terminology, 2nd ed. (the "Gold Book"), Blackwell Scientific Publications, Oxford, 1997.

[7] Schrader B, Bougeard D, Infrared and Raman Spectroscopy: Methods and Applications, VCH: Weinheim, New York, 1995.

[8] Li HH, J. Phys. Chem. Ref Data, 13, 103 (1984)

[9] Comelli F, Ottani S, J. Chem. Eng. Data, 49(4), 970 (2004)

[10] Kiefer J, Frank K, Zehentbauer MF, Schuchmann PH, Biosensors, 6 (2016)

[11] Kiefer J, Frank K, Schuchmann HP, Appl. Spectrosc., 65, 1024 (2011)

[12] Bohren CF, Huffman DR, Absorption and Scattering of Light by Small Particles, Wiley, New York, 1983.

[13] Boulet-Audet M, Buffeteau T, Boudreault S, Daugey N, Pezolet M, J. Phys. Chem. B, 114(24), 8255 (2010)

[14] Miljkovic M, Bird B, Diem M, Analyst, 137, 3954 (2012)

[15] Mohlenhoff B, Romeo M, Diem M, Wood BR, Biophys. J., 88, 3635 (2005)