制备具有热降解丁二酸酐和尿素单元的聚硅氧烷基二氧化碳分离膜

Katsuhiro Horata, Tsubasa Yoshio, Ryuto Miyazaki, Yohei Adachi, M. Kanezashi, T. Tsuru, J. Ohshita
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摘要

通过共聚[3-(三乙氧基硅基)丙基]琥珀酸酐(TESPS)或[3-(三乙氧基硅基)丙基]脲(TESPU)的 1:3-(三乙氧基硅基)丙基]丁二酸酐 (TESPS) 或[3-(三乙氧基硅基)丙基]脲 (TESPU) 与双(三乙氧基硅基)乙烷 (BTESE) 的 1:1 混合物共聚制备而成。琥珀酸酐和单烷基脲单元发生热降解,分别形成酯和二烷基脲单元,并在 N2 气氛下释放出小分子(如 CO2 和 NH3)。研究了热降解对所得膜性能的影响。基于 TESPS-BTESE 和 TESPU-BTESE 的膜分别在 250 °C 和 200 °C 煅烧,表现出良好的 CO2/N2 过选择性,分别为 20.2 和 14.4,CO2 渗透率分别为 7.7 × 10-8 和 7.9 × 10-8 mol m-2-s-1-Pa-1 。当膜分别在 350 °C 和 300 °C 的高温下进一步煅烧以促进有机单元的热降解时,二氧化碳渗透率分别增加到 1.3 × 10-7 和 1.2 × 10-6 mol m-2-s-1-Pa-1 (3.9 × 102 和 3.6 × 103 GPU),但 CO2/N2 过选择性分别下降到 19.5 和 8.4。这些数据表明,有机单元的受控热降解为调整 PSQ 膜的二氧化碳分离性能提供了一种新方法。
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Preparation of Polysilsesquioxane-Based CO2 Separation Membranes with Thermally Degradable Succinic Anhydride and Urea Units
New polysilsesquioxane (PSQ)-based CO2 separation membranes with succinic anhydride and monoalkylurea units as thermally degradable CO2-philic units were prepared by the copolymerization of a 1:1 mixture of [3-(triethoxysilyl)propyl]succinic anhydride (TESPS) or [3-(triethoxysilyl)propyl]urea (TESPU) and bis(triethoxysilyl)ethane (BTESE). The succinic anhydride and monoalkylurea units underwent thermal degradation to form ester and dialkylurea units, respectively, with the liberation of small molecules (e.g., CO2 and NH3) under N2 atmosphere. The effects of thermal degradation on the performance of the obtained membranes were investigated. The TESPS-BTESE- and TESPU-BTESE-based membranes calcined at 250 °C and 200 °C exhibited good CO2/N2 permselectivities of 20.2 and 14.4, respectively, with CO2 permeances of 7.7 × 10−8 and 7.9 × 10−8 mol m−2·s−1·Pa−1, respectively. When the membranes were further calcined at elevated temperatures of 350 °C and 300 °C, respectively, to promote the thermal degradation of the organic units, the CO2 permeances increased to 1.3 × 10−7 and 1.2 × 10−6 mol m−2·s−1·Pa−1 (3.9 × 102 and 3.6 × 103 GPU), although the CO2/N2 permselectivities decreased to 19.5 and 8.4, respectively. These data indicate that the controlled thermal degradation of the organic units provides a new methodology for possible tuning of the CO2 separation performance of PSQ membranes.
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