氧化铝中空纤维载体上NaA分子筛膜的制备与分离性能研究
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摘要
NaA分子筛膜,由于其具备极强的亲水性和0.42nm的孔径,适用于渗透汽化实现有机物的脱水。目前,NaA分子筛膜已由日本三井造船公司实现工业化,但膜的性能还有待于进一步提高,膜成本可进一步降低,成膜机理需进一步完善。陶瓷中空纤维耐高温耐腐蚀,且具备比表面积大、壁厚薄和表面平整的优势,适于用作分子筛膜的载体,近年吸引了广泛的研究兴趣。本文致力于在氧化铝中空纤维载体表面制备NaA分子筛膜的研究,阐述了二次生长过程中晶种的诱导成膜作用,提出了载体预置硅源的改良原位水热合成法,评价了载体层产生的透过阻力,并针对性地改善了中空纤维载体的结构和性能,制备了具备高渗透汽化分离性能的NaA分子筛膜。
(1)晶种诱导成膜过程的探究
采用浸涂法在氧化铝中空纤维外表面涂敷晶种,通过二次生长法制备NaA分子筛膜。通过比较纳米级与微米级晶种诱导成膜形貌和性能的差异性,阐述了水热合成阶段NaA分子筛晶体生长与成膜过程。对纳米级晶种而言,源自合成液的初晶核围绕在载体表面预置晶种周围,二者共同生长,迅速连接成层；而对微米级晶种而言,晶体团聚体是膜层的主要构成单元,且源自合成液的共生性较差的晶体嵌入膜层,导致瑕疵位的产生。使用1wt.%的晶种液浓度,90nm晶种对应的膜层醇水分离因子>10,000,而1500nm晶种合成的膜层分离因子<10。另外,研究了球磨所得无规则形状纳米级晶体碎片的诱导成膜作用,并呈现了晶种浓度对NaA分子筛膜分离性能的影响曲线。随晶种液浓度增加,膜层醇水分离因子先增加然后趋于稳定,对表面平整的中空纤维载体而言,合成连续致密NaA分子筛膜所需的最低晶种液浓度仅为0.1wt.%。
(2)改良原位水热合成方法的研究
从陈化和晶化两个阶段,从增加晶核数目和促进晶体生长两方面,研究合成条件对NaA分子筛膜形貌与性能的影响。提出了载体预置硅源的新型原位水热合成法,具体制备过程为,A.将中空纤维载体预置硅源中,B.滴加铝源制备合成液,C.载体与合成液一同陈化,D.将载体取出旋抹表面凝胶,E.将载体垂直放入合成液离心所得清液中,完成晶化。载体预先被硅源所浸润,随着铝源的滴加,Si和Al成分在载体表面相遇,初晶核从载体表面长出,消除了凝胶不易在载体表面成核的问题,增加了分子筛膜成核位点的分散密度。采用该改良的原位水热法,单次合成即实现具有高醇水分离性能的NaA分子筛膜(分离因子超过10,000,渗透通量范围为5.0～6.5kg m-2h-1)的制备。
(3)分子筛膜渗透通量影响因素的考察
从分子筛分离层和载体支撑层两方面考察影响整体渗透通量的因素。通过延长晶化时间和增加晶化次数的方式制备了不同膜厚的NaA分子筛膜,并研究了分子筛膜厚对其渗透汽化通量的影响。通过调整挤出压力、A12O3/PES(聚醚砜)比和焙烧温度等纺丝条件,制备了具有不同大孔结构和壁厚的非对称氧化铝中空纤维,并以之为载体合成NaA分子筛膜,研究了载体孔结构、孔隙率和壁厚对分子筛膜渗透汽化通量的影响。中空纤维载体孔隙率为69%时,NaA分子筛膜渗透汽化通量可达11.1kg m-2h-1；而使用孔隙率接近而壁厚减半的中空纤维作为分子筛膜载体时,合成的NaA膜渗透通量提高～35%。另外,模型化计算了渗透汽化过程透过组分在载体两侧的压降,计算结果表明,使用不同壁厚的载体合成NaA分子筛膜,醇水分离时载体层产生的传质阻力都超过载体与分子筛膜层整体阻力的50%。另外,采用具备内外贯通指状孔结构的新型氧化铝中空纤维作为成膜载体,可使分子筛膜通量进一步提高约15%。可见,载体层结构的改善是提高NaA分子筛膜分离性能和机械性能的关键。
(4)提高氧化铝中空纤维机械性能的研究。
将NaA分子筛晶体混入Al2O3/PES纺丝液中,采用浸入诱导相转化结合焙烧技术,通过调整NaA分子筛含量,纺丝液配比,挤出压力以及焙烧温度等条件,制备了机械性能显著提高的Al2O3中空纤维。通过分析NaA分子筛晶体在焙烧过程中的晶型与状态的改变,考察其焙烧残余物对氧化铝中空纤维形貌,结构及性能的影响。发现,高温焙烧过程中,NaA分子筛晶体经历骨架坍塌,晶型改变以及溶解固化过程,成为Al2O3粒子间强有力的粘合剂,可以降低氧化铝中空纤维的烧结温度。
Zeolite NaA with high Al content and small pore size (4.2A), has been found to be suitable for dehydrating water/organic mixtures by pervaporation. Despite the successful commercialization of supported zeolite NaA membranes (Mitsui Engineering&Shipbuilding Co. Ltd.), the fundamental understanding of membrane formation remains limited. Also, the separation performance of zeolite membranes needs to be further improved, and the manufacture cost could be further reduced. Ceramic hollow fibers, used as supports of zeolite membranes, have attracted wide attentions, not only because of their relatively high resistance to abrasion and, to chemical and thermal degradation, but also their higher surface/volume ratio and thinner walls compared with their counterparts of tubular supports. This research focuses on the preparation of zeolite NaA membranes on alumina hollow fiber supports. The induction nucleation of pre-coated zeolite seeds during the secondary growth process is investigated. The in situ hydrothermal synthesis is developed by placing the support in Si source before mixing. The contribution of the support layer to the overall mass-transfer resistance is determined. Accordingly, the permeation property and mechanical strength of alumina hollow fibers is improved. And finally, the dense zeolite NaA membranes with high pervaporation performance are obtained on the suitable alumina hollow fiber supports.
(1) Influences of seeds on the properties of zeolite NaA membranes
Zeolite NaA membranes were prepared by seeded growth on the external surface of alumina hollow fiber supports. Based on the morphology and performance of zeolite NaA membranes grown from nano-and micro-sized seeds, seed-assisted membrane formation process is briefly discussed. It is easier for nano-sized seeds to uniformly cover the surface of the support with a low concentration while micro-sized seeds need unreasonably large concentration to get the same coverage. Initial nuclei generated from hydrogel surround the precoated nano-sized seeds everywhere and grow up together with them, leading to a relatively continuous layer at the early crystallization stage. For the micro-sized seeds, the inadequate coverage of seed crystals leads to the embedding of less intergrown cubic crystals and defects. When the seed concentration is as low as1wt.%, the separation factor of as-synthesized membrane from90-nm-sized seeds was higher than10.000with high reproducibility, while for1500-nm-sized seeds, separation factors are even below10. Furthermore, the influence of crystal fragments (～50nm) obtained by ball-milling available crystals (e.g.,1500nm) on the formation of zeolite membranes is also studied. Initially, a rise in the seed concentration leads to an increase of the separation factor. When the concentration reaches a specific value, the separation factors maintain more than10,000. In order to ensure uniform and adequate coverage of seeds, the amount of seeds implanted in the support by dip-coating has to exceed a certain limit. The lowest seed concentration is～0.1wt.%.
(2) Improvement of in situ hydrothermal synthesis
The in situ hydrothermal synthesis is developed by placing support in Si source before mixing. The detailed preparation process is as follows. At first, the hollow fiber support is placed in Si solution before mixing with the Al solution; then, the synthesis mixture is aged together with the support; after that, the support is taken out and a bottom-up rotary wiping is applied; finally, a centrifugal clear solution from the synthesis mixture is used to accomplish the zeolite crystallization. As Si ingredient encounters the Al near support, the initial zeolite nuclei start to grow from the surface of the support. Due to the elimination of crowding effect, the dispersion density of nucleation sites for the zeolite membrane increases greatly. As a result, we demonstrate for the first time that, by one single in situ hydrothermal synthesis, zeolite membranes with high pervaporation performance (separation factor>10,000and flux is5.0～6.5kg m-2h-1) and high reproducibility on ceramic hollow fiber supports can be obtained using a placing-support-in-Si source method.
(3) Effects of support resistances on pervaporation performance of zeolite membranes
Porous Al2O3hollow fibers with different asymmetric macrostructures, i.e. single or double finger-like layer, have been prepared by a phase inversion/sintering technique. Such hollow fibers are used as supports to synthesize zeolite NaA membranes with high separation factors (>10,000) in the pervaporation of ethanol/water solution (90wt.%,75℃). By means of extending the crystallization time (4～6h) and increasing the number of synthesis cycles (single/double/triple syntheses), zeolite membranes with different thicknesses are synthesized. Extrusion pressure, Al2O3/PES ratio, and calcination temperataure are adjusted to control the asymmetric macrostructure of the ceramic hollow fibers. Influences of both the zeolite layer thickness and support layer macrostructures on pervaporation properties of zeolite NaA/Al2O3supported membranes are investigated. It is indicated that the variation of the support macrostructure rather than zeolite layer thickness results in a greater difference in the pervaporation flux of the supported membrane. There is an approximate linear dependence of the pervaporation flux of the supported membrane on the support porosity despite the fact that these hollow fibers are produced with different preparation conditions. Using a hollow fiber with the porosity of69%as a support, a flux of11.1kg m-2h-1could be achieved. When the wall thickness of the support is reduced by half, the flux could increase by～35%. Furthermore, a mathematical model is used to calculate the pressure drop in the support layer. Using hollow fibers with different wall thickness as supports, the contribution of the support layer to the overall mass-transfer resistance is over50%. In addition, when the alumina hollow fiber with through finger-like pores is used as the support, the flux could further increase by～15%. Therefore, in order to obtain the zeolite NaA/Al2O3supported membranes with the high pervaporation performance and mechanical strength, it is probably effective to focus on the improvement and development of the support properties.
(4) Improvement in the mechanical strength of ceramic hollow fibers
With the addition of zeolite NaA to Al2O3/PES spinning slurry, the alumina hollow fibers with high mechanical strength are prepared by a combined phase-inversion and sintering method. Effects of zeolite NaA content, dope composition, extrusion pressure and calcination temperature on the morphology and structure of the ceramic hollow fibers are investigated. Improvement in the mechanical strength of hollow fibers resulting from the addition of zeolite NaA crystals is analysed. During the calcination process, zeolite NaA crystals probably experience framework collapse, crystalline phase transition, dissolution and solidification. Finally the zeolite NaA remains play a role as rivets and lead to the strong adhesive of alumina particles.
(1)晶种诱导成膜过程的探究
采用浸涂法在氧化铝中空纤维外表面涂敷晶种,通过二次生长法制备NaA分子筛膜。通过比较纳米级与微米级晶种诱导成膜形貌和性能的差异性,阐述了水热合成阶段NaA分子筛晶体生长与成膜过程。对纳米级晶种而言,源自合成液的初晶核围绕在载体表面预置晶种周围,二者共同生长,迅速连接成层；而对微米级晶种而言,晶体团聚体是膜层的主要构成单元,且源自合成液的共生性较差的晶体嵌入膜层,导致瑕疵位的产生。使用1wt.%的晶种液浓度,90nm晶种对应的膜层醇水分离因子>10,000,而1500nm晶种合成的膜层分离因子<10。另外,研究了球磨所得无规则形状纳米级晶体碎片的诱导成膜作用,并呈现了晶种浓度对NaA分子筛膜分离性能的影响曲线。随晶种液浓度增加,膜层醇水分离因子先增加然后趋于稳定,对表面平整的中空纤维载体而言,合成连续致密NaA分子筛膜所需的最低晶种液浓度仅为0.1wt.%。
(2)改良原位水热合成方法的研究
从陈化和晶化两个阶段,从增加晶核数目和促进晶体生长两方面,研究合成条件对NaA分子筛膜形貌与性能的影响。提出了载体预置硅源的新型原位水热合成法,具体制备过程为,A.将中空纤维载体预置硅源中,B.滴加铝源制备合成液,C.载体与合成液一同陈化,D.将载体取出旋抹表面凝胶,E.将载体垂直放入合成液离心所得清液中,完成晶化。载体预先被硅源所浸润,随着铝源的滴加,Si和Al成分在载体表面相遇,初晶核从载体表面长出,消除了凝胶不易在载体表面成核的问题,增加了分子筛膜成核位点的分散密度。采用该改良的原位水热法,单次合成即实现具有高醇水分离性能的NaA分子筛膜(分离因子超过10,000,渗透通量范围为5.0～6.5kg m-2h-1)的制备。
(3)分子筛膜渗透通量影响因素的考察
从分子筛分离层和载体支撑层两方面考察影响整体渗透通量的因素。通过延长晶化时间和增加晶化次数的方式制备了不同膜厚的NaA分子筛膜,并研究了分子筛膜厚对其渗透汽化通量的影响。通过调整挤出压力、A12O3/PES(聚醚砜)比和焙烧温度等纺丝条件,制备了具有不同大孔结构和壁厚的非对称氧化铝中空纤维,并以之为载体合成NaA分子筛膜,研究了载体孔结构、孔隙率和壁厚对分子筛膜渗透汽化通量的影响。中空纤维载体孔隙率为69%时,NaA分子筛膜渗透汽化通量可达11.1kg m-2h-1；而使用孔隙率接近而壁厚减半的中空纤维作为分子筛膜载体时,合成的NaA膜渗透通量提高～35%。另外,模型化计算了渗透汽化过程透过组分在载体两侧的压降,计算结果表明,使用不同壁厚的载体合成NaA分子筛膜,醇水分离时载体层产生的传质阻力都超过载体与分子筛膜层整体阻力的50%。另外,采用具备内外贯通指状孔结构的新型氧化铝中空纤维作为成膜载体,可使分子筛膜通量进一步提高约15%。可见,载体层结构的改善是提高NaA分子筛膜分离性能和机械性能的关键。
(4)提高氧化铝中空纤维机械性能的研究。
将NaA分子筛晶体混入Al2O3/PES纺丝液中,采用浸入诱导相转化结合焙烧技术,通过调整NaA分子筛含量,纺丝液配比,挤出压力以及焙烧温度等条件,制备了机械性能显著提高的Al2O3中空纤维。通过分析NaA分子筛晶体在焙烧过程中的晶型与状态的改变,考察其焙烧残余物对氧化铝中空纤维形貌,结构及性能的影响。发现,高温焙烧过程中,NaA分子筛晶体经历骨架坍塌,晶型改变以及溶解固化过程,成为Al2O3粒子间强有力的粘合剂,可以降低氧化铝中空纤维的烧结温度。
Zeolite NaA with high Al content and small pore size (4.2A), has been found to be suitable for dehydrating water/organic mixtures by pervaporation. Despite the successful commercialization of supported zeolite NaA membranes (Mitsui Engineering&Shipbuilding Co. Ltd.), the fundamental understanding of membrane formation remains limited. Also, the separation performance of zeolite membranes needs to be further improved, and the manufacture cost could be further reduced. Ceramic hollow fibers, used as supports of zeolite membranes, have attracted wide attentions, not only because of their relatively high resistance to abrasion and, to chemical and thermal degradation, but also their higher surface/volume ratio and thinner walls compared with their counterparts of tubular supports. This research focuses on the preparation of zeolite NaA membranes on alumina hollow fiber supports. The induction nucleation of pre-coated zeolite seeds during the secondary growth process is investigated. The in situ hydrothermal synthesis is developed by placing the support in Si source before mixing. The contribution of the support layer to the overall mass-transfer resistance is determined. Accordingly, the permeation property and mechanical strength of alumina hollow fibers is improved. And finally, the dense zeolite NaA membranes with high pervaporation performance are obtained on the suitable alumina hollow fiber supports.
(1) Influences of seeds on the properties of zeolite NaA membranes
Zeolite NaA membranes were prepared by seeded growth on the external surface of alumina hollow fiber supports. Based on the morphology and performance of zeolite NaA membranes grown from nano-and micro-sized seeds, seed-assisted membrane formation process is briefly discussed. It is easier for nano-sized seeds to uniformly cover the surface of the support with a low concentration while micro-sized seeds need unreasonably large concentration to get the same coverage. Initial nuclei generated from hydrogel surround the precoated nano-sized seeds everywhere and grow up together with them, leading to a relatively continuous layer at the early crystallization stage. For the micro-sized seeds, the inadequate coverage of seed crystals leads to the embedding of less intergrown cubic crystals and defects. When the seed concentration is as low as1wt.%, the separation factor of as-synthesized membrane from90-nm-sized seeds was higher than10.000with high reproducibility, while for1500-nm-sized seeds, separation factors are even below10. Furthermore, the influence of crystal fragments (～50nm) obtained by ball-milling available crystals (e.g.,1500nm) on the formation of zeolite membranes is also studied. Initially, a rise in the seed concentration leads to an increase of the separation factor. When the concentration reaches a specific value, the separation factors maintain more than10,000. In order to ensure uniform and adequate coverage of seeds, the amount of seeds implanted in the support by dip-coating has to exceed a certain limit. The lowest seed concentration is～0.1wt.%.
(2) Improvement of in situ hydrothermal synthesis
The in situ hydrothermal synthesis is developed by placing support in Si source before mixing. The detailed preparation process is as follows. At first, the hollow fiber support is placed in Si solution before mixing with the Al solution; then, the synthesis mixture is aged together with the support; after that, the support is taken out and a bottom-up rotary wiping is applied; finally, a centrifugal clear solution from the synthesis mixture is used to accomplish the zeolite crystallization. As Si ingredient encounters the Al near support, the initial zeolite nuclei start to grow from the surface of the support. Due to the elimination of crowding effect, the dispersion density of nucleation sites for the zeolite membrane increases greatly. As a result, we demonstrate for the first time that, by one single in situ hydrothermal synthesis, zeolite membranes with high pervaporation performance (separation factor>10,000and flux is5.0～6.5kg m-2h-1) and high reproducibility on ceramic hollow fiber supports can be obtained using a placing-support-in-Si source method.
(3) Effects of support resistances on pervaporation performance of zeolite membranes
Porous Al2O3hollow fibers with different asymmetric macrostructures, i.e. single or double finger-like layer, have been prepared by a phase inversion/sintering technique. Such hollow fibers are used as supports to synthesize zeolite NaA membranes with high separation factors (>10,000) in the pervaporation of ethanol/water solution (90wt.%,75℃). By means of extending the crystallization time (4～6h) and increasing the number of synthesis cycles (single/double/triple syntheses), zeolite membranes with different thicknesses are synthesized. Extrusion pressure, Al2O3/PES ratio, and calcination temperataure are adjusted to control the asymmetric macrostructure of the ceramic hollow fibers. Influences of both the zeolite layer thickness and support layer macrostructures on pervaporation properties of zeolite NaA/Al2O3supported membranes are investigated. It is indicated that the variation of the support macrostructure rather than zeolite layer thickness results in a greater difference in the pervaporation flux of the supported membrane. There is an approximate linear dependence of the pervaporation flux of the supported membrane on the support porosity despite the fact that these hollow fibers are produced with different preparation conditions. Using a hollow fiber with the porosity of69%as a support, a flux of11.1kg m-2h-1could be achieved. When the wall thickness of the support is reduced by half, the flux could increase by～35%. Furthermore, a mathematical model is used to calculate the pressure drop in the support layer. Using hollow fibers with different wall thickness as supports, the contribution of the support layer to the overall mass-transfer resistance is over50%. In addition, when the alumina hollow fiber with through finger-like pores is used as the support, the flux could further increase by～15%. Therefore, in order to obtain the zeolite NaA/Al2O3supported membranes with the high pervaporation performance and mechanical strength, it is probably effective to focus on the improvement and development of the support properties.
(4) Improvement in the mechanical strength of ceramic hollow fibers
With the addition of zeolite NaA to Al2O3/PES spinning slurry, the alumina hollow fibers with high mechanical strength are prepared by a combined phase-inversion and sintering method. Effects of zeolite NaA content, dope composition, extrusion pressure and calcination temperature on the morphology and structure of the ceramic hollow fibers are investigated. Improvement in the mechanical strength of hollow fibers resulting from the addition of zeolite NaA crystals is analysed. During the calcination process, zeolite NaA crystals probably experience framework collapse, crystalline phase transition, dissolution and solidification. Finally the zeolite NaA remains play a role as rivets and lead to the strong adhesive of alumina particles.
引文
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