화학공학소재연구정보센터
Macromolecular Research, Vol.17, No.10, 725-728, October, 2009
Synthesis of New Sulfonated Polyimide and Its Photo-Crosslinking for Polymer Electrolyte Membrane Fuel Cells
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  20. Synthesis of SPI: Copolyimide of NTDA/SODA and NTDA/3DAC with 0.5:0.5 mol ratio was synthesized and used throughout the experiments. SODA (0.28 mol), TEA (0.67 mol) and 3DAC (0.28 mol) were added successively to 4,500 mL of mcresol in a 3-neck flask with stirring. After SODA and 3DAC were completely dissolved, NTDA (0.56 mol) and benzoic acid (1.12 mol) were added. The mixture was stirred at 80 °C for 20 h and 180 °C for 24 h under nitrogen atmosphere and then the reaction mixture was precipitated into ethyl acetate. The fibrous precipitate was filtered and dried at 80 °C in vacuo. Preparation of SPI membranes: Firstly, uncrosslinked membranes were prepared by pouring the m-cresol solution of 10% SPI onto a glass plate (4 cm × 10 cm) and dried at room temperature for 3 d in air, 60 ° for 24 h and 140 °C for 24 h in vacuo, respectively. The crosslinked membranes were obtained from SPI solution in m-cresol containing 10 wt% (to SPI) of 1,6-hexanedithiol (HDT) and 5 wt% (to SPI) of IRGACURE 907® as a crosslinking agent and photo-initiator, respectively, following the above process with subsequent UV light irradiation (198 mW/cm2) for 30 min. The uncrosslinked and crosslinked membranes were acidified by immersing the membranes of TEA salt form into 1.0 M HCl solution at room temperature for 48 h, and then soaked in methanol and deionized water successively to remove excess acid and any impurity.
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