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以丙酮为溶剂,将9,9-双(4-羟基苯基)芴(BHF)于室温下进行硝化反应得到二硝基化合物9,9-双(3-硝基-4-羟基苯基)芴,再经Pd/C-水合肼还原得到9,9-双(3-氨基-4-羟基苯基)芴(BAHF).采用上述二胺单体BAHF、与9,9-双(4-氨基苯基)芴(BAF)和六氟二酐(6FDA)通过低温溶液缩聚反应制备出一种含酚羟基的共聚聚酰胺酸溶液,经热酰亚胺化和热致重排反应得到共聚聚酰亚胺(CPI)和聚(酰亚胺-苯并恶唑)(PIPBO)热致刚性膜材料.采用核磁(NMR)、红外光谱(FTIR)、X-射线衍射仪(XRD)、热重分析仪(TGA)、差示扫描量热仪(DSC)和气体渗透性能测试等手段对所制得膜材料的结构、热性能和气体分离性能进行表征.研究结果表明,所制得的热致刚性膜主要表现出非晶结构,为无规共聚物,其Tg为340℃.随热处理温度升高,热致刚性膜的气体渗透性逐渐增加,450℃制得的热致刚性膜对O_2、N_2、H_2、CH_4和CO_2的渗透通量分别达到229.03、53.26、1497.35、33.52和818.76 Barrer.
Nitration of 9,9-bis (4-hydroxyphenyl) fluorene (BHF) at room temperature with acetone as the solvent gave the dinitro compound 9,9-bis (3-nitro-4- hydroxyphenyl) (3-amino-4-hydroxyphenyl) fluorene (BAHF) was obtained by reduction with Pd / C-hydrazine hydrate using the above diamine monomer BAHF and 9,9-bis Amino-phenyl) fluorene (BAF) and hexafluoro-dianhydride (6FDA) to prepare a kind of copolymerized polyamic acid solution containing phenolic hydroxyl group by the polycondensation reaction of low temperature solution to obtain copolymerized polyamic acid solution through thermal imidization and thermal rearrangement (CPI) and poly (imide-benzoxazole) (PIPBO) thermosensitive rigid film materials were prepared by the methods of nuclear magnetic resonance (NMR), infrared spectroscopy (FTIR), X-ray diffraction (XRD) (TGA), differential scanning calorimetry (DSC) and gas permeation test were used to characterize the structure, thermal properties and gas separation performance of the obtained membrane materials.The results show that the thermal induced The rigid film mainly shows an amorphous structure, which is a random copolymer with a Tg of 340 ° C. With the increase of the heat treatment temperature, the gas permeability of the thermally rigid film gradually increases. N 2, H 2, CH 4 and CO 2 fluxes Do not reach 229.03,53.26,1497.35,33.52 and 818.76 Barrer.