Guang Lu Han,Pei Yu Xu,Ke Zhou,Qiu Gen Zhang,Ai Mei Zhu,Qing Lin Liu
A series of poly (arylene ether sulfone) block copolymers with hydrophilic segments containing fluorene groups were successfully synthesized as confirmed by 1 H NMR. The molecular weights were measured in the range 115–140 kDa by gel permeation chromatography (GPC). The hydrophilic segment showed a helical structure due to fluorene with butterfly-shaped framework in the main chain. With incorporating imidazolium groups, the microphase separation can also be achieved between the hydrophilic and the hydrophobic moieties. The membrane structure was characterized by positron annihilation lifetime spectroscopy (PALS) and small angle X-ray scattering (SAXS). The block copolymers were used to prepare membranes successfully for pervaporation separation of methanol (MeOH)/methyl tert-butyl ether (MTBE) mixture. The correlation between the membrane microstructure and the separation performance was discussed thoroughly. By increasing the hydrophilic segment proportion, the permeation flux increased while the separation factor declined. The membranes have the highest permeation flux (0.334 kg m −2 h −1 ) and the lowest separation factor (287) for a 15 wt% MeOH feed mixture at 40 °C, and the mass fraction of MeOH in the permeate is higher than 98 wt%.
A seeding-free synthesis strategy was developed for the preparation of dense and phase-pure MFI zeolite membranes based on “like grows like” principle. Through covalent modification of the porous ceramic supports by using 1H,1H,2H,2H-perfluoroalkyltriethoxysilanes (POTS), the support surface was changed from hydrophilic to hydrophobic, which promotes the nucleation and growth of hydrophobic MFI zeolite membranes. Thin, well-intergrown and phase-pure MFI zeolite membranes, with a thickness of about 2.0–3.0 μm, can be facilely prepared on POTS-modified supports like Al 2 O 3 and TiO 2 at 175 °C for 24 h. No cracks, pinholes or other visible macroscopic defects are observed in the membrane layer. The MFI zeolite membranes were evaluated in the hydrophobic separation of 5.0 wt% ethanol/water mixture at 75 °C by pervaporation . The MFI zeolite membrane prepared on the POTS-modified TiO 2 disk shows high pervaporation separation for ethanol recovery. At 75 °C, a separation factor of 103 and total flux of 2.56 kg/m 2 h can be obtained, which is promising to extract bio-alcohols from the fermentation broth.
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