Decarboxylation-induced thermal cross-linking occurs at elevated temperatures (∼15 °C above glass transition temperature) for 6FDA–DAM:DABA polyimides, which can stabilize membranes against swelling and plasticization in aggressive feed streams. Despite this advantage, such a high temperature might result in collapse of substructure and transition layers in the asymmetric structure of a hollow fibers based on such a material. In this work, the thermal cross-linking of the 6FDA–DAM:DABA at temperatures much below the glass transition temperature (∼387 °C by DSC) was demonstrated. This sub-T
g cross-linking capability enables extension to asymmetric structures useful for large scale membranes. The resulting polymer membranes were characterized by swelling in known solvents for the un-cross-linked materials, TGA analysis, and permeation tests of aggressive gas feed stream at higher pressure. The annealing temperature and time clearly influence the degree of cross-linking of the membranes, and results in a slight difference in selectivity for membranes under various cross-linking conditions. Results indicate that the sub-T
g thermal cross-linking of 6FDA–DAM:DABA dense film membrane can be carried out completely even at a temperature as low as 330 °C. Permeabilities were tested for the polyimide membranes using both pure gases (He, O2, N2, CH4, CO2) and mixed gases (CO2/CH4). The selectivity of the cross-linked membrane can be maintained even under very aggressive CO2 operating conditions that are not possible without cross-linking. Moreover, the plasticization resistance was demonstrated up to 700 psia for pure CO2 gas or 1000 psia for 50% CO2 mixed gas feeds.
The effects of addition of an organoclay on the morphology and the mechanical properties of blends of an amorphous polyamide (a-PA) and an elastomer (with and without grafted maleic anhydride) prepared via melt processing are reported. Transmission electron microscopy (TEM) and wide-angle X-ray scattering (WAXS) were employed to obtain a detailed quantitative analyses of the morphology of the elastomer particles for these nanocomposites containing 80 wt % a-PA and 20 wt % elastomer. Stress-strain diagrams and impact strength were measured as a function of organoclay content for blends containing maleated and unmaleated elastomer. It is clear that the addition of organoclay to blends can be an effective way for reducing elastomer particle size and enhancing stiffness when the elastomer is not maleated; however, for this system, toughness is not improved in spite of these morphological changes. Blends based on the maleated elastomer give a more beneficial balance of toughness versus stiffness.
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