POLYMERS AND POLYMER MATRIX COMPOSITES |
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Preparation and Gas Separation Properties of Polymers of Intrinsic Microporosity PIM-1 Based Thermally Induced Rigid Membranes |
LU Yunhua1, HAO Jican1, LI Lin2, SONG Jing2, XIAO Guoyong1, HU Zhizhi1, WANG Tonghua2
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1 School of Chemical Engineering, University of Science and Technology Liaoning, Anshan 114051; 2 School of Chemical Engineering, Dalian University of Technology, Dalian 116024 |
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Abstract Firstly,5,5',6,6'-tetrahydroxy-3,3,3',3'-tetramethylspirobisindane was synthesized from catechol and acetone as the raw materials. Then, the intrinsically microporous polymer PIM-1 was prepared from a dioxane-forming reaction between the home-made 5,5',6,6'-tetrahydroxy-3,3,3',3'-tetramethylspirobisindane and 2,3,5,6-tetrafluoroterephthalonitrile. The PIM-1 polymer membranes were thermally treated at 300 ℃,350 ℃ and 400 ℃ for 1 h under the N2 atmosphere, respectively. The structures and properties of the tetrahydroxyl compound, PIM-1 polymer and the PIM-1 based thermally induced rigid membranes were characterized by nuclear magnetic resource (NMR), gel permeation chromatography (GPC), differential scanning calorimeter (DSC), thermogravimetric analysis (TGA), Fourier transform infrared (FTIR), X-ray diffraction (XRD) and scanning electron microscope (SEM), and the gas separation properties of these membranes were also measured with five kinds of pure gases, including H2, O2, N2, CO2 and CH4. These experimental results showed that the obtained PIM-1 exhibited good thermal properties with the glass transition temperature (Tg) of 340 ℃ and the thermal decomposition temperature (Td) of 503 ℃. The gas permeabilities of the resultant PIM-1 based thermally induced rigid membranes were further improved by controlling the processing temperature. After the thermal treatment at 300 ℃, the permeabilities of H2, O2, N2, CO2 and CH4 of the thermally induced rigid membranes were 2 865 Barrer,1 071 Barrer,298 Barrer,7 070 Barrer and 495 Barrer, separately. Furthermore, with the temperature increasing, the permeabilities of these gas separation membranes were decreased, but the selectivity was improved. For the PIM-1-400 membrane, the selectivity of CO2/CH4 was 18.51.
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Published: 18 September 2018
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