Journal of Applied Polymer Science, Vol.100, No.3, 1720-1727, 2006
Synthesis and characterization of poly(urethane-ester)s based on calcium salt of mono (hydroxybutyl)phthalate
Calcium-containing poly(urethane-ester)s (PUEs) were prepared by reacting diisocyanate (HMDI or TDI) with a mixture of calcium salt of mono(hydroxybutyl)phthalate [Ca(HBP)(2)] and hydroxyl-terminated poly(1,4-butylene glutarate) [HTPBG(1000)], using di-n-butyltin-diaaurate as catalyst. About six calcium-containing PUEs having different composition were synthesized by taking the mole ratio of Ca(HBP)(2):HTPBG(1000):diisocyanate (HMDI or TDI) as 3:1:4, 2:2:4, and 1:3:4. Two blank PUEs were synthesized by the reaction of HTPBG(1000) with diisocyanate (HMDI or TDI). The polymers were characterized by TR, H-1 NMR, Solid state C-13-CP-MAS NMR, TGA, DSC, XRD, solubility, and Viscosity Studies. The T l value of PUEs increases with increase in the calcium content and decreases with increase in soft segment content. The viscosity of the calcium-containing PUEs increases with increase in the soft segment content and decreases with increase in the calcium content. X-ray diffraction patterns of the polymers show that the HMDI-based polymers are partially crystalline and TDI-based polymers are amorphous in nature. The dynamic mechanical analysis of the calcium-containing PUEs based on HMDI shows that with increase in the calcium content of polymer, modulus (g' and g") increases at any given temperature. (c) 2006 Wiley Periodicals, Inc.
Keywords:poly(urethane-ester)s;calcium-containing polymer;NMR spectra;thermal properties;dynamic mechanical analysis