Synthesis of Partially Carbonized Polyimide Membranes with High Resistance to Moisture

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  • Momose Wataru
    Division of Chemical Engineering, Graduate School of Engineering Science, Osaka University
  • Zheng Tao
    Division of Chemical Engineering, Graduate School of Engineering Science, Osaka University
  • Nishiyama Norikazu
    Division of Chemical Engineering, Graduate School of Engineering Science, Osaka University
  • Egashira Yasuyuki
    Division of Chemical Engineering, Graduate School of Engineering Science, Osaka University
  • Ueyama Korekazu
    Division of Chemical Engineering, Graduate School of Engineering Science, Osaka University

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Partially carbonized polyimide (CPI) membranes were prepared on a porous alumina support from carbonization of polyimide membranes at 460–500°C. The permeance of O2 through the CPI membrane increased with the increasing carbonization temperature, although the separation factors (O2/N2) reduced from 11 to 4. The highly permeable CPI membranes carbonized at 500°C were silylated with 1,1,1,3,3,3-hexamethyl disilazane (HMDS) at 90°C, 150°C and 180°C before or after carbonization to solve an adverse humidity effect on gas permeation. The molar ratios of C/Si in the cross section of the silylated CPI membranes were analyzed by SEM-EDX measurements. The separation of dry air through the nonsilylated and silylated CPI membranes was performed before and after a steam treatment. Continuous air permeation tests under saturated steam were also performed with prolonged time. The CPI membranes silylated at 180°C had deposition of organosilicate on the outer surface of polyamide layer, resulting in the reduction of the O2 flux. On the other hand, the flux of O2 and the separation factor for the CPI membrane silylated at 150°C before carbonization did not reduce drastically under saturated steam. The results of chemical composition analysis for polyimide and carbonized polyimide suggests that water-resistant CPI membranes with high O2 permeation flux were synthesized by taking advantage of reactive carboxyl groups in the membrane before carbonization.

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