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复合炭膜的缺陷修饰

发布时间:2018-08-22 08:06
【摘要】:炭膜作为一种新颖的无机膜材料具有化学性能稳定,耐酸碱、耐腐蚀,孔径可调等优点,在膜分离领域具有广阔的应用前景。按结构炭膜可以分为均质炭膜和复合炭膜。复合炭膜增强了炭膜的机械性能,但在制备过程中易产生缺陷降低其分离性能。有序介孔炭是指具有大面积排列规整孔道结构的无机炭材料,介孔炭材料孔径均一,比表面积较高且孔容相对较大,可以用作复合炭膜缺陷的修饰材料。本文采用软模板法利用间苯二酚/甲醛反应制得的酚醛树脂(PFR)为前驱体与三嵌段共聚物(F127)通过溶剂挥发自组装方法制备有序介孔炭材料。结合实验室原有工艺对介观相酚醛树脂进行了放大工艺(公斤级)的考察,探讨了在放大过程中料液的反应时间、反应温度对介孔孔道结构的影响。得出了最佳工艺条件:在45℃下反应12h制得具有介观相的酚醛树脂,炭化后可以得到具有二维六角(P6mm)结构的介孔炭材料。以介观相酚醛树脂为前驱体,通过浸渍手段对复合炭膜缺陷进行修饰。考察了浸渍工艺对修饰效果的影响。结果表明PFR溶液浓度越大,修饰效果越好,同时膜层增厚,易产生二次缺陷;加入5%PEG能够增加溶液的浸润能力,增强修饰效果;共混物聚酰氨酸(PAA)的加入提高了浸渍溶液的残炭量,对尺度较大的缺陷具有良好的修饰能力。确定最佳工艺配方为15%PFR+5%PEG+1%PAA,在40℃下通过单次“浸渍-炭化”流程在复合炭膜表面能够形成具有介孔结构的修饰层,对复合炭膜的缺陷具有良好的修饰效果。对修饰后的炭膜作通量分析,测得氧气通量为1149.54GPU, O2/N2的分离系数为1.30。
[Abstract]:As a novel inorganic membrane material, carbon membrane has the advantages of stable chemical properties, acid and alkali resistance, corrosion resistance and adjustable pore size, and has a broad application prospect in membrane separation field. According to the structure of carbon film can be divided into homogeneous carbon film and composite carbon film. The composite carbon membrane enhances the mechanical properties of the carbon membrane, but it is easy to produce defects in the preparation process and reduce its separation performance. Ordered mesoporous carbon is a kind of inorganic carbon material with large area arrangement and regular pore structure. The mesoporous carbon material has uniform pore size, high specific surface area and relatively large pore volume, so it can be used as a modified material for composite carbon membrane defects. In this paper, an ordered mesoporous carbon material was prepared by solvent volatilization self-assembly method using phenolic resin (PFR) prepared by soft template reaction with resorcinol / formaldehyde as precursor and triblock copolymers (F127). The effect of reaction time and reaction temperature on the mesoporous structure of mesoporous phenolic resin (KG) was investigated in combination with the original process in laboratory, and the effects of reaction time and reaction temperature on the structure of mesoporous channel were discussed. The optimum technological conditions were obtained as follows: phenolic resin with mesoscopic phase was prepared at 45 鈩,

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