类沸石咪唑骨架膜的制备与性能研究
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摘要
金属有机骨架(MOFs)化合物作为一种新型的多孔晶态材料,基于其结构多样、孔径可调以及拥有可化学修饰的孔道,突破了沸石分子筛孔道尺寸和化学组成的局限性,成为具有潜在应用价值的新一代膜材料。目前,金属有机骨架材料的成膜化研究刚刚起步,主要以较高稳定性的一类MOFs材料：类沸石咪唑骨架(ZIFs)为研究对象,集中在片状小孔载体上成膜或有机膜中掺杂ZIFs晶体制备混合基质膜。相较于小孔片状载体,大孔管状载体更有利于工业化应用。但大孔载体表面缺陷多,缺乏MOFs生长的异相成核点,不利于膜的生长。本文以改变载体表而性质为出发点,降低载体表面粗糙度和增加异相成核点,克服了大孔载体难以制备MOFs膜的技术难点,成功地制备出高性能的ZIFs膜,并创新性地提出修补缺陷膜的方法。主要结果如下：
(1)以水取代有机溶剂作为反应介质,不添加模板剂的条件下得到大小为500nm、粒径分布均匀的[Co(Im)2]。。晶种,采用二次生长法在大孔管状载体表而制备连续致密、厚度约为9μmm的[Co(Im)2]。膜,并考察了成膜时间、合成液浓度对膜的形貌和性能的影响。室温下H2的渗透速率达1.1×10-8molm-2s-1Pa-1, H2/CO2, H2/N2和H2/CH4的理想分离系数分别为7.8,9.1和7.9,超过努森扩散选择性。
(2)采用高分子聚乙二醉(PEG)包裹的方法,将ZIF-8纳米晶种涂覆至大孔载体表面,解决了晶种尺寸与载体孔径不匹配以及晶种层与载体结合力差的问题,制备出高性能的ZIF-8膜。考察了晶种分散剂、PEG和ZIF-8晶种浓度对涂覆晶种与膜质量和性能的影响,得出体积比为1/1/1的混合溶剂水/乙醇/N,N-二甲基甲酰胺(H2O/EtOH/DMF)为分散剂、PEG浓度为5%、ZIF-8浓度为1.5%,成膜液配方为1.1ZnCl2-4H20:1.7mlm:4.5NaCHO2:985CH3OH时制备的ZIF-8膜质量最好,H2渗透速率达到5.6×10-7mol·m-2s-1Pa-1, H2/CO2、H2/N2、 H2/CH4、 H2/C3H6、和H2/SF6分别达5.96、4.09、6.12、10.74、8.8和16.52,均超过努森扩散选择性,具有潜在的应用价值。
(3)针对弱配位键、MOFs(?)与载体间膨胀系数相差大使MOFs膜易产生缺陷的问题,提出一种将ZIF-8缺陷膜进行打磨并提拉含有ZIF-8晶种的PEG溶液,经过晶化反应修补缺陷的方法。打磨使缺陷膜表面产生大量的ZIF-8小晶粒填补到缺陷处,提拉PEG-ZIF-8溶液能进一步提高载体表而的Z1F-8晶种含量,具有粘稠性的PEG固定载体表面的ZIF-8晶粒并使载体表面平整,晶化反应后,得到致密无缺陷的ZIF-8膜,厚度为19μm,单组分气体渗透速率随着分子尺寸地增加而降低,H2/N2, H2/CH4和CO2/CH4的混合气分离性能分别为6.5,6.7和3.5,H2的渗透速率达1.17×10-7mol·m-2s-1Pa-1。
(4)发展了一种新颖的二合一法,即将经过化学修饰的无机粒子涂覆到载体表面,不仅能够修补大孔载体表面的缺陷,同时增加异相成核点,解决了大孔结构导致膜缺陷化和异相成核点低下的问题。通过内外扩散法获得了厚度小于2gm、高渗透性能和高选择性的ZIF-8膜,在保持较高选择性的条件下,H2/CO2和H2/N2的理想分离系数达17.05和15.44,H2渗透速率高达5.73×10-5mol·m-2·S-1Pa-1,是迄今为止报道的ZIF-8膜的一至两个数量级,在报道的多孔透氢膜中,该膜的分离指数最高。涂覆无机粒子能够使载体有效外表面积从28.56cm2提高到215.38cm2,经元素分析表征,无机粒子表面APTES含量达到16nm-2。而原位法在涂覆无机粒子的载体表而制备的膜容易产生缺陷,主要原因是无机粒子与载体以及无机粒子间结合力比较差。
(5)结合文献中报道的双金属源法,将ZnO粒子涂覆到大孔载体表面形成连续的ZnO层,并经过高温固载。ZnO粒子不仅修补了载体表面,同时能够提供过饱和的Zn2+作为金属源诱导ZIF-8在载体表面成核生长。经过原位晶化反应制备出高性能的ZIF-8膜,厚度在15μm, H2渗透速率达3.4×10-7molm-2s-1Pa-1, H2/CO2, H2/N2, H2/CH4, H2/C3H8和H2/SF6的理想分离系数分别为7.4,8.8,8.2,37.8和20.7,都远大于相应的努森扩散选择性。如果将涂覆ZnO层的载体与配体溶液前处理后再晶化成膜,膜容易产生缺陷。
Metal-organic frameworks (MOFs) as hybrid organic-inorganic nanoporous materials exhibiting regular crystalline lattices with relatively well-defined pore structures have been widely used in catalysis, gas storage, drug delivery and photo/electron/magnetic areas. Chemical functionalization of the organic linkers in the structures of MOFs affords facile control over pore size and chemical/physical properties, making MOFs attractive as new separation membrane materials. Different from the discontinuous and limited range of available pore sizes of zeolites, MOFs could be designed or tailored in gas separation applications due to their ultramicropores in the scale of gas molecules.
The processing of MOFs as films is a domain that has only recently been initiated. The avenues of MOFs membrane researches focus on fabricating pure MOFs phases on the microporous or nonporous supports and the mixed matrix membranes which are generally polymer/inorganic composites consisting of a primary polymer phase and a secondary phase of dispersed MOFs particles. In contrast, the macroporous tubular supports are more conducive to industrial applications, due to the easier assembly, larger loading density and lower cost. A thin and dcfects/pinholes free membrane on the support with large pore size is desirable for high flux and high selectivity. However, the larger the pore size of the support, the larger the risk of forming defects which decrease the separation factor. On the other hand, the poor bonding between the inorganic substrates and the organic ligand and tubular geometry of the support increased the difficulties in the preparation of defect-free MOFs membranes. Despite of the much progress on preparation of MOFs membranes, there is still a long way ahead for the facile synthesis of MOFs membranes with high performance before robust synthetic strategies can be developed.
In views of the problems in preparation of MOFs membranes on macroporous support, we combined the seeded growth method with chemical modification method into one for the synthesis of MOFs membranes. High performance MOFs membranes were successfully obtained. We also proposed the innovative strategy for elimination the cracks in the MOFs layers and obtainment the defect-free membranes. The main research contents are listed below.
[Co(lm)2]∞seeds with size of500nm were obtained in aqueous solution at room temperature. The characterization of SEM, XRD showed that the [Co(lm)2]∞. crystals with uniform particle size distribution is suitable as seeds for the selected macroporous support. Through secondary growth method in aqueous solutions, continuous and crack-free [Co(lm)2]∞membrane was successfully obtained on the low-cost macroporous α-Al2O3support, exhibiting H2permeance of1.1x10-8mol m-2s-1Pa-1with ideal selectivity for H2/CO2, H2/N2and H2/CH4system of7.8,9.1and7.9at room temperature. Moreover, the effects of other parameters including the concentration of solution and synthesis time on the formation of [Co(Im)2]∞were also investigated. Through deposition of PEG solution containing ZIF-8particles on the macroporous support, continuous and defect-free ZIF-8membranes were successfully obtained, solving the issue of seed size unmatched with the aperture of the support. The effects of the solvents as dispersing agent, the concentration of PEG and ZIF-8seeds on the formation seed layer and ZIF-8membrane were investigated. While the mixed solvent (DMF/EtOH/H2O, v/v/v=1/1/1) as solvent, the concentration of PEG and ZIF-8seeds reaching5%and1.5%, the ZIF-8membrane obtained under recipe of1.1ZnCl2-4H2O:1.7mlm:4.5NaCHO2:985CH3OH showed the best separation performance, exhibiting H2permeance of5.6rme"7mol m-2s-1Pa-1with ideal selectivity exceeding Knudesen selectivity at room temperature.
The formation of cracks within the MOFs layers is a big challenge to their practical applications. Here, a new strategy, namely through polishing the cracked ZIF-8membrane and dip-coating PEG solution containing ZIF-8seeds was developed to eliminate cracks and form a continuous and crack-free ZIF-8membranes on coarse macroporous tubes. After polishing, rhombic crystals of the thick cracked ZIF-8membrane were crushed into small and irregularly shaped particles, leading to form a much thinner ZIF-8layer. The dip-coated PEG solution served to fix plenty of "seeds" in the cracks and give a flat surface through the glutinosity of PEG. When the cracked ZIF-8membrane was subject to both of polishing and dip-coating PEG solution and one more crystallization growth, continuous and defect-free ZIF-8membrane showing molecular sieving selectivity for H2/N2, H2/CH4and CO2/CH4of6.5,6.7and3.5was obtained. In contrast, only polishing without dip-coating the PEG solution, the secondly synthesized ZIF-8membrane showed a few cracks and a Knudesen selectivity for the light gas.
Through deposition of APTES-functionalized A12O3particles onto a coarse macroporous support, a new strategy to reduce the pore size and simultaneously promote high heterogeneous nucleation sites was developed, and a continuous and thin ZIF-8membrane exhibiting remarkably high H2permeance of5.73×10-5mol m-2s-1Pa-1，with ideal selectivity for H2/N2and H2/CO2system of17.05and15.44, respectively, was achieved. Moreover, the density of hetergeneous nucleation sites on the APTES-a-Al2O3particle deposited support is higher than that on the support directly modified with APTES, due to the resulting larger amount of APTES molecules considering the large surface area (215.38cm2·g-1) of the deposited α-Al2O3particles, which is about8times of that of the corresponding bare support(28.56cm2·g-1). Due to the lack of bonding force between the bare inorganic particles and the support, the ZIF-8membranes obtained by in situ growth method always form cracks.
The enormous flexibility in pore size, shape, structure and myriad opportunities for functionalization and grafting make metal organic frameworks (MOFs) as excellent candidate of membrane materials. In the article, we report a modified "two in one" strategy through deposition ZnO particles onto low-cost and large-pore tubular supports with average pore size of3-4μm for the synthesis of ZIF-8membranes. The ZnO particles were directly deposited on the support to act as filler to reduce the pore size and simultaneously as "metal source" to create a high supersaturation degree to promote high heterogeneous nucleation sites. Through such simultaneous surface and pore structure modification, continuous and crack-free ZIF-8membrane was successfully obtained, exhibiting H2permeance of3.4×10-7mol m-2-1Pa-1with ideal selectivities for H2/CO2, H2/N2, H2/CH4, H2/C3H8, and H2/SF6system of7.4,8.8,8.2,37.8and20.7, respectively at150℃. When.the supports deposited with ZnO particles were treated by pre-reacting with the ligand of2-methylimidazole, big cracks/gaps occurred at the interface between the ZIF-8membrane and the support. The work demonstrates the high flexibility and universality of the modified "two in one" strategy for synthesis of MOFs membranes on large-pore supports through the rational selection of metal oxides.
(1)以水取代有机溶剂作为反应介质,不添加模板剂的条件下得到大小为500nm、粒径分布均匀的[Co(Im)2]。。晶种,采用二次生长法在大孔管状载体表而制备连续致密、厚度约为9μmm的[Co(Im)2]。膜,并考察了成膜时间、合成液浓度对膜的形貌和性能的影响。室温下H2的渗透速率达1.1×10-8molm-2s-1Pa-1, H2/CO2, H2/N2和H2/CH4的理想分离系数分别为7.8,9.1和7.9,超过努森扩散选择性。
(2)采用高分子聚乙二醉(PEG)包裹的方法,将ZIF-8纳米晶种涂覆至大孔载体表面,解决了晶种尺寸与载体孔径不匹配以及晶种层与载体结合力差的问题,制备出高性能的ZIF-8膜。考察了晶种分散剂、PEG和ZIF-8晶种浓度对涂覆晶种与膜质量和性能的影响,得出体积比为1/1/1的混合溶剂水/乙醇/N,N-二甲基甲酰胺(H2O/EtOH/DMF)为分散剂、PEG浓度为5%、ZIF-8浓度为1.5%,成膜液配方为1.1ZnCl2-4H20:1.7mlm:4.5NaCHO2:985CH3OH时制备的ZIF-8膜质量最好,H2渗透速率达到5.6×10-7mol·m-2s-1Pa-1, H2/CO2、H2/N2、 H2/CH4、 H2/C3H6、和H2/SF6分别达5.96、4.09、6.12、10.74、8.8和16.52,均超过努森扩散选择性,具有潜在的应用价值。
(3)针对弱配位键、MOFs(?)与载体间膨胀系数相差大使MOFs膜易产生缺陷的问题,提出一种将ZIF-8缺陷膜进行打磨并提拉含有ZIF-8晶种的PEG溶液,经过晶化反应修补缺陷的方法。打磨使缺陷膜表面产生大量的ZIF-8小晶粒填补到缺陷处,提拉PEG-ZIF-8溶液能进一步提高载体表而的Z1F-8晶种含量,具有粘稠性的PEG固定载体表面的ZIF-8晶粒并使载体表面平整,晶化反应后,得到致密无缺陷的ZIF-8膜,厚度为19μm,单组分气体渗透速率随着分子尺寸地增加而降低,H2/N2, H2/CH4和CO2/CH4的混合气分离性能分别为6.5,6.7和3.5,H2的渗透速率达1.17×10-7mol·m-2s-1Pa-1。
(4)发展了一种新颖的二合一法,即将经过化学修饰的无机粒子涂覆到载体表面,不仅能够修补大孔载体表面的缺陷,同时增加异相成核点,解决了大孔结构导致膜缺陷化和异相成核点低下的问题。通过内外扩散法获得了厚度小于2gm、高渗透性能和高选择性的ZIF-8膜,在保持较高选择性的条件下,H2/CO2和H2/N2的理想分离系数达17.05和15.44,H2渗透速率高达5.73×10-5mol·m-2·S-1Pa-1,是迄今为止报道的ZIF-8膜的一至两个数量级,在报道的多孔透氢膜中,该膜的分离指数最高。涂覆无机粒子能够使载体有效外表面积从28.56cm2提高到215.38cm2,经元素分析表征,无机粒子表面APTES含量达到16nm-2。而原位法在涂覆无机粒子的载体表而制备的膜容易产生缺陷,主要原因是无机粒子与载体以及无机粒子间结合力比较差。
(5)结合文献中报道的双金属源法,将ZnO粒子涂覆到大孔载体表面形成连续的ZnO层,并经过高温固载。ZnO粒子不仅修补了载体表面,同时能够提供过饱和的Zn2+作为金属源诱导ZIF-8在载体表面成核生长。经过原位晶化反应制备出高性能的ZIF-8膜,厚度在15μm, H2渗透速率达3.4×10-7molm-2s-1Pa-1, H2/CO2, H2/N2, H2/CH4, H2/C3H8和H2/SF6的理想分离系数分别为7.4,8.8,8.2,37.8和20.7,都远大于相应的努森扩散选择性。如果将涂覆ZnO层的载体与配体溶液前处理后再晶化成膜,膜容易产生缺陷。
Metal-organic frameworks (MOFs) as hybrid organic-inorganic nanoporous materials exhibiting regular crystalline lattices with relatively well-defined pore structures have been widely used in catalysis, gas storage, drug delivery and photo/electron/magnetic areas. Chemical functionalization of the organic linkers in the structures of MOFs affords facile control over pore size and chemical/physical properties, making MOFs attractive as new separation membrane materials. Different from the discontinuous and limited range of available pore sizes of zeolites, MOFs could be designed or tailored in gas separation applications due to their ultramicropores in the scale of gas molecules.
The processing of MOFs as films is a domain that has only recently been initiated. The avenues of MOFs membrane researches focus on fabricating pure MOFs phases on the microporous or nonporous supports and the mixed matrix membranes which are generally polymer/inorganic composites consisting of a primary polymer phase and a secondary phase of dispersed MOFs particles. In contrast, the macroporous tubular supports are more conducive to industrial applications, due to the easier assembly, larger loading density and lower cost. A thin and dcfects/pinholes free membrane on the support with large pore size is desirable for high flux and high selectivity. However, the larger the pore size of the support, the larger the risk of forming defects which decrease the separation factor. On the other hand, the poor bonding between the inorganic substrates and the organic ligand and tubular geometry of the support increased the difficulties in the preparation of defect-free MOFs membranes. Despite of the much progress on preparation of MOFs membranes, there is still a long way ahead for the facile synthesis of MOFs membranes with high performance before robust synthetic strategies can be developed.
In views of the problems in preparation of MOFs membranes on macroporous support, we combined the seeded growth method with chemical modification method into one for the synthesis of MOFs membranes. High performance MOFs membranes were successfully obtained. We also proposed the innovative strategy for elimination the cracks in the MOFs layers and obtainment the defect-free membranes. The main research contents are listed below.
[Co(lm)2]∞seeds with size of500nm were obtained in aqueous solution at room temperature. The characterization of SEM, XRD showed that the [Co(lm)2]∞. crystals with uniform particle size distribution is suitable as seeds for the selected macroporous support. Through secondary growth method in aqueous solutions, continuous and crack-free [Co(lm)2]∞membrane was successfully obtained on the low-cost macroporous α-Al2O3support, exhibiting H2permeance of1.1x10-8mol m-2s-1Pa-1with ideal selectivity for H2/CO2, H2/N2and H2/CH4system of7.8,9.1and7.9at room temperature. Moreover, the effects of other parameters including the concentration of solution and synthesis time on the formation of [Co(Im)2]∞were also investigated. Through deposition of PEG solution containing ZIF-8particles on the macroporous support, continuous and defect-free ZIF-8membranes were successfully obtained, solving the issue of seed size unmatched with the aperture of the support. The effects of the solvents as dispersing agent, the concentration of PEG and ZIF-8seeds on the formation seed layer and ZIF-8membrane were investigated. While the mixed solvent (DMF/EtOH/H2O, v/v/v=1/1/1) as solvent, the concentration of PEG and ZIF-8seeds reaching5%and1.5%, the ZIF-8membrane obtained under recipe of1.1ZnCl2-4H2O:1.7mlm:4.5NaCHO2:985CH3OH showed the best separation performance, exhibiting H2permeance of5.6rme"7mol m-2s-1Pa-1with ideal selectivity exceeding Knudesen selectivity at room temperature.
The formation of cracks within the MOFs layers is a big challenge to their practical applications. Here, a new strategy, namely through polishing the cracked ZIF-8membrane and dip-coating PEG solution containing ZIF-8seeds was developed to eliminate cracks and form a continuous and crack-free ZIF-8membranes on coarse macroporous tubes. After polishing, rhombic crystals of the thick cracked ZIF-8membrane were crushed into small and irregularly shaped particles, leading to form a much thinner ZIF-8layer. The dip-coated PEG solution served to fix plenty of "seeds" in the cracks and give a flat surface through the glutinosity of PEG. When the cracked ZIF-8membrane was subject to both of polishing and dip-coating PEG solution and one more crystallization growth, continuous and defect-free ZIF-8membrane showing molecular sieving selectivity for H2/N2, H2/CH4and CO2/CH4of6.5,6.7and3.5was obtained. In contrast, only polishing without dip-coating the PEG solution, the secondly synthesized ZIF-8membrane showed a few cracks and a Knudesen selectivity for the light gas.
Through deposition of APTES-functionalized A12O3particles onto a coarse macroporous support, a new strategy to reduce the pore size and simultaneously promote high heterogeneous nucleation sites was developed, and a continuous and thin ZIF-8membrane exhibiting remarkably high H2permeance of5.73×10-5mol m-2s-1Pa-1，with ideal selectivity for H2/N2and H2/CO2system of17.05and15.44, respectively, was achieved. Moreover, the density of hetergeneous nucleation sites on the APTES-a-Al2O3particle deposited support is higher than that on the support directly modified with APTES, due to the resulting larger amount of APTES molecules considering the large surface area (215.38cm2·g-1) of the deposited α-Al2O3particles, which is about8times of that of the corresponding bare support(28.56cm2·g-1). Due to the lack of bonding force between the bare inorganic particles and the support, the ZIF-8membranes obtained by in situ growth method always form cracks.
The enormous flexibility in pore size, shape, structure and myriad opportunities for functionalization and grafting make metal organic frameworks (MOFs) as excellent candidate of membrane materials. In the article, we report a modified "two in one" strategy through deposition ZnO particles onto low-cost and large-pore tubular supports with average pore size of3-4μm for the synthesis of ZIF-8membranes. The ZnO particles were directly deposited on the support to act as filler to reduce the pore size and simultaneously as "metal source" to create a high supersaturation degree to promote high heterogeneous nucleation sites. Through such simultaneous surface and pore structure modification, continuous and crack-free ZIF-8membrane was successfully obtained, exhibiting H2permeance of3.4×10-7mol m-2-1Pa-1with ideal selectivities for H2/CO2, H2/N2, H2/CH4, H2/C3H8, and H2/SF6system of7.4,8.8,8.2,37.8and20.7, respectively at150℃. When.the supports deposited with ZnO particles were treated by pre-reacting with the ligand of2-methylimidazole, big cracks/gaps occurred at the interface between the ZIF-8membrane and the support. The work demonstrates the high flexibility and universality of the modified "two in one" strategy for synthesis of MOFs membranes on large-pore supports through the rational selection of metal oxides.
引文
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