Effects of thermal history in the ring opening polymerization of CBT and its mixtures with montmorillonite on the crystallization of the resulting poly(butylene terephthalate)

Differential scanning calorimetrywas used to study the thermal characteristics and morphological structure of species produced during the ring opening polymerization of cyclic butylene terephthalate (CBT). Thermal programs consisting of a first ramp heating scan and an isothermal step, followed by cooling and a second ramp heating step,were used to study the effects of thermal history, catalyst (butyl chlorotin dihydroxide) at concentrations between 0.1 and 1.3% (w/w), and the presence of a layered silicate nanofiller (montmorillonite at 4.0%, w/w) on the structure of the resulting polymer (poly(butylene terephthalate), pCBT). Wide angle X-ray diffractionwas used to monitor the degree of exfoliation of the nanocomposites. It was found that pCBT is formed in the amorphous state, and crystallizes during the heating step or during the isothermal step at temperatures lower than the equilibrium melting temperature of the polymer(T0m ).Whenpremixed with the nanofiller, irrespective ofwhether thiswas previously intercalated with a tallowsurfactant or used in its pristine form, polymerization took place at higher temperatures and most of the crystallizationwas found to occur during the cooling stage. In those cases where crystallization took place during either the first heating scan, or during a prolonged isothermal step below the T0m of the polymer, the resulting crystals were found to have a higher lamellar thickness, as compared with the same polymer crystallized from the melt during the cooling step from temperatures above the polymer T0m