preparation and characterization of layered silicate polyethylene terephthalate nanocomposite by in situ polymerization

A series of experiments on the synthesis of poly (ethylene terephthalate) (pet)/organo‐montmorillonite(mmt) nanocomposites were carried out in a pressurized reactor using alkyl ammonium exchangedsmectite clays, (closite 30b). given the degradation of organoclay at high temperatures, the in situpolymerization process was carried out at mild temperatures ranging from 210 to 230°c for 40minutes followed by solid state polymerization (ssp) at 245°c for 30 minutes at a pressure of 5mbar. the nanocomposites were prepared using different weight percentages (1‐5) of organoclay.the reaction completed when the mixing torque ceased to change as recorded by the auto dataacquisition system of the pressure reactor. the dsc analysis provided information on the course ofthe thermal characterization of the pet nanocomposites versus regular pet. as shown by theresults of dsc cooling scan, all the pet nanocomposite samples have higher crystallizationtemperatures (tc) and faster crystallization rates (δhc/t) compared to regular pet. furthermore, theopposite behavior is observed for t1/2. this is due to the fact that the nucleation of organoclaynanoparticles reduces the crystallite size in the pet nanocomposites. the xrd results indicated thatthe peaks in the 2θ angle from 1° to 7° were disappeared, which is an indication of an exfoliatedmmt. in addition, the atomic force microscope (afm) results showed broken mirror like lamellae,confirming the exfoliated results of the xrd analysis. the peaks are indexed according to the 2θangle from 10 to 30° known assignments of the triclinic unit cell dimensions for pet. thecomparative crystallite size of the pet nanocomposites samples (1‐5%wt organoclay) can bededuced from the peak ratio change of 2θ angle from 10° to 30°. heat distortion (or deflection)temperature (hdt) was enhanced by increasing the amount of organoclay in pet nanocompositescompared to regular pet. the tensile test results of 2%wt organoclay show an increase of 58% inthe tensile strength of this sample. as a result of mmt agglomeration, due to the high temperatureinstability of closite 30b, the relative oxygen pressure drop data shows fluctuations. however, as anoverall trend, pet nanocomposite gives about 50% greater reduction in o2 pressure drop or relativeoxygen permeability compared with a homo structure.