β沸石膜的制备及其分离催化性能的研究
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摘要
沸石膜因其具有独特的物理化学性质以及与分子尺寸相近的孔道体系，故能耐高温、化学及生物侵蚀，可在分子级别上进行物质分离，实现催化分离一体化优点，兼具沸石分子筛与无机膜的特性，一直是无机膜领域研究的热点之一。β沸石是迄今为止唯一具有三维交叉孔道、十二元环且硅铝比在较大范围内可调的大孔沸石，它具有较强的热稳定性，较好的吸附性以及适度的酸性，因此，如果将β沸石制成膜，则会在膜分离与膜催化反应器上有着巨大的潜在应用。所以，开展β沸石膜的制备和应用研究，合成出性能优良的β沸石膜具有重要的意义。
沸石膜研究的关键是对于具有高性能、低成本的沸石分子筛膜的制备。为此，本文首先采用传统路线的模板剂法详细考察了制备β沸石膜的条件，得出了β沸石膜的合成规律，然后在此基础上把导向剂法引入沸石膜的制备中，即在制备沸石膜的过程中，并不像传统的模板剂法那样直接在晶化液中加入大量的有机模板剂，而是首先利用少量的有机模板剂合成出含有β沸石微晶核的沸石结构导向剂，然后用此导向剂代替有机模板剂加入到晶化液中，晶化液在导向剂的导向作用下在载体上晶化生长形成β沸石膜，从而在大量降低模板剂用量的条件下，合成出高质量的β沸石模。然后分别将两种方法合成的膜应用在渗透蒸发分离MeOH／MTBE混合体系上，得到了较好的分离效果；最后为了拓展β沸石膜的应用，在陶瓷管载体上制备了beta-NaA催化分离双功能沸石膜，并且将该双功能膜应用在了乙酸和乙醇的酯化反应中，为β沸石膜在膜反应器上的应用奠定了基础。实验得到的主要结论如下：
(1)在研究β沸石膜制备前，首先研究了适合作晶种用的小晶粒β沸石的合成条件，考察了晶化液中不同硅源、不同种类模板剂及其含量、碱度和水含量以及晶化温度、晶化时间等对小晶粒β沸石合成的影响。研究结果表明，以活化硅胶为硅源，TEAOH-TEABr为模板剂，按照SiO_2∶0.02Al_2O_3∶0.45(TEA)_2O∶0.061Na_2O∶0.8(NH_4)_2O∶20H_2O的摩尔比配制合成液，在150℃下晶化72 h可得到粒径为200～300 nm的高结晶度小晶粒β沸石。
(2)研究了在大孔载体管表面预涂晶种的方法，结果表明，对于大孔载体，浸渍提拉预涂晶种法简单易操作且效果好。分别从晶化液组成和模板剂的焙烧脱除等方面对传统的模板剂法在α-Al_2O_3陶瓷管载体表面合成β沸石膜的制备条件进行了考察，结果表明：配制成膜前驱液的最佳摩尔投料比为SiO_2∶Al_2O_3∶Na_2O∶(TEA)_2O∶H_2O=1∶0.02∶0.06∶0.35∶35；在晶化温度为150℃，晶化时间为72 h的条件下，经过6次晶化生长后，能够得到10μm左右厚度的β沸石膜；采用先于氮气气氛下缓慢升温，再于空气气氛下继续焙烧的分两步脱除模板剂的脱模方式较为适宜。用已经得到的最优制备条件再于多孔炭管和多孔不锈钢管载体表面合成β沸石膜，经过比较可知，选用α-Al_2O_3陶瓷管作为载体较为合适。
(3)考察了β沸石导向剂的制备条件，结果表明：用相对廉价且易于操作的活化硅胶做硅源，能够合成出β沸石导向剂；加料顺序和水含量对导向剂合成的影响较大。详细研究了水量、晶化时间以及晶化温度对导向剂法合成β沸石的结构和结晶度的影响，得到了导向剂法合成B沸石的最优合成条件，为进一步用该法合成β沸石膜奠定了基础。考察了水量，导向剂含量，有机物脱除等对导向剂法合成β沸石膜的影响，得出了导向剂法合成β沸石膜的最优合成条件为：按照1SiO_2∶0.033Al_2O_3∶0.317Na_2O∶28H_2O的摩尔配比配制成硅铝溶胶，然后再加入占该硅铝溶胶体积1／8的沸石结构导向剂，搅拌配制成晶化前驱液，在150℃下，晶化60 h；焙烧方式为先于氮气气氛下焙烧，在于空气下焙烧的分两步焙烧的脱模方式。在最优条件下，经过6次晶化生长的β沸石膜表面连续完整，沸石膜层大约9μm厚。对导向剂法合成的膜和传统的模板剂法合成的膜进行了比较，结果表明：在导向剂法合成膜过程中，价格高昂的有机物TEAOH的消耗量比传统方法少90％，这一方面降低了制膜成本，另一方面由于膜中需要脱除的有机物少，使得在焙烧过程中可能产生的晶间缺陷也少，从而提高了膜的质量。导向剂法不单可以应用在β沸石膜的制备上，还可以应用到其他种类需要有机物来做模板剂的沸石膜的制备中。
(4)将两种方法合成的β沸石膜分别应用在渗透蒸发分离MeOH／MTBE混合体系中，详细考察了渗透侧压力、进料组成、进料流速和进料温度对该分离的影响；结果表明，导向剂法合成的膜在分离性能上要明显优于传统方法合成的，其最高分离系数达到了9600。
(5)研究了NaA沸石膜在陶瓷管载体上的合成条件，然后采用导向剂法和模板剂法分别在生长于陶瓷管载体表面的NaA沸石膜表面制备了β沸石膜，最终晶化形成了beta-NaA催化分离双功能沸石膜；将该双功能沸石膜和单一催化功能的β沸石膜应用在了乙酸和乙醇的酯化反应上，通过比较可知，双功能沸石膜由于及时的将反应生成的水移走了，因而打破反应平衡提高了反应的转化率。
Owing to their unique physical and chemical characteristic and similar molecular-sized channel systems, zeolite membranes can not only work at high-temperature, chemical and biological corrosive environments but also have potential applications for separation of different substances at molecular levels and for integration of catalysis and separation processes. In the last decades, zeolite membrane materials drew the growing interests as the cutting age research field in the membrane community. Beta zeolite is a high-silica zeolite possessing a three-dimensional interconnected channel system of 12-O ring large pore and has good heat stability, adsorption capability and proper acidity, so if the beta zeolite membranes can be prepared they will have potential application in separations, even in separation and catalytic membrane reactors due to its unique pore structure and catalytic properties. The research on beta zeolite membrane is very scare, thus it is significant for the beta zeolite membrane to make many efforts on reseach of its preparation and then model application.
The key for the research is how to prepare the beta zeolite membranes with better performance under the conditions of lower cost. The membrane preparation was firstly investigated using conventional template method and the membrane preparation condition was optimized. This includes the synthesis condition optimization of small crystal-size beta zeolite as the seeds, the work on how to improve the quality of seeded layer on support tubes with 3～5μm pore diameter and the optimization of preparation conditions of beta zeolite membranes. On the other hand, a novel method of beta zeolite structure-directing agent (ZSDA) was developed for the preparation of beta zeolite membrane. First, the synthesis of beta ZSDA was investigated. Then, the optimal preparation conditions of beta zeolite prepared by ZSDA method were investigated from the following aspects respectively: content of water, crystallization time and crystallization temperature. By this ZSDA method, organic templates were substituted with beta ZSDA, as a result, a lot of expensive organic templates were saved compared with the conventional method. Then the membranes prepared by both template method and ZSDA method were applied for the pervaporation separation of MeOH/MTBE mixture. The effects of permeation side pressure, feed composition, feed flow rate and feed temperature on the flux and separation factor were investigated, At last to exploit the application of beta zeolite membranes the beta-NaA bi-founctional zeolite membranes were prepared on theα-Al_2O_3 support tubes and applied as membrane reactor for the esterification of acetic acid with ethanol. The main results achieved are as follows:
(1) For the synthesis of small crystal beta zeolite, the results indicated that when crystallization temperature and crystallization time were 150℃and 72h beta zeoltes with small crystal-size in the 200～300 nm range could be prepared according to the molar composition of SiO_2: 0.02Al_2O_3: 0.45 (TEA)_2O: 0.061Na_aO: 0.8 (NH_4)20: 20H_2O. Silicate gel was used as silicon source and TEAOH-TEABr was used as template.
(2) As for the optimal preparation conditions of beta zeolite membranes prepared by conventional template method, it is found that the optimal molar composition of precursor solution is of SiO_2: Al_2O_3: Na_2O: (TEA)_2O: H_2O=1: 0.02: 0.06: 0.35: 35. When the crystallization temperature was 150~C and crystallization time was 72h a continuous and dense membrane with 10μm in thickness, was obtained after 6 synthesis times.Templates were removed by the mode of calcinations in N2 and air orderly. At last beta zeolite membranes were grown on the porous carbon support tubes and porous steel support tubes respectively according to the optimal membranes preparation conditions above obtained. By comparing among the three supports used, it can be known thatα-Al_2O_3 support tubes were the most proper.
(3) It is found that beta ZSDA can be synthesized by using the silica gel as the silicon source that is cheap and easy operational. Moreover, the feed order and content of water had important effects on the synthesis of ZSDA. And the optimal preparation conditions were confirmed as follows: Silicon-aluminum sol was prepared by the molar composition of 1SiO_2:0.033Al_2O_3:0.317Na_2O:28H_2O; Precursor solution was confected by adding the ZSDA into the sol and the content of ZSDA added was 1/8 of the sol in .volume; Crystallization temperature was 150℃and crystallization time was 60h; The organic agent was removed by the mode of calcinations in N_2 and air orderly; A continuous and dense membrane with 9μm in thickness was obtained after 6 synthesis times. Compared with the conventional template method it can be concluded that by ZSDA method not only 90% of costly organic agent was saved but also the quality of membrane was improved due to the less defect was formed when the less organic agent needed to be removed. This ZSDA method can be extended to zeolite membrane preparation of other types in which organic templates are necessary.
(4) The membranes prepared by ZSDA method had better performance in pervaporation separation of MeOH/MTBE mixture. The maximum separation factor reached 9600.
(5) To compare with bi-founctional membranes, single catalytic beta zeolite membranes grown on theα-Al_2O_3 support tubes were also applied in the esterification of acetic acid with. ethanol under the same reaction conditions with that of bi-founcitonal membranes. It can be known from the comparison that conversion rate corresponding to bi-founctional membranes was much higher than that of the single catalytic beta zeolite membranes. This is because the bi-founctionalmembranes had the high performace of removing water, one of the reaction product, so the reaction equribrium was broken and conversion rate was increased.
沸石膜研究的关键是对于具有高性能、低成本的沸石分子筛膜的制备。为此，本文首先采用传统路线的模板剂法详细考察了制备β沸石膜的条件，得出了β沸石膜的合成规律，然后在此基础上把导向剂法引入沸石膜的制备中，即在制备沸石膜的过程中，并不像传统的模板剂法那样直接在晶化液中加入大量的有机模板剂，而是首先利用少量的有机模板剂合成出含有β沸石微晶核的沸石结构导向剂，然后用此导向剂代替有机模板剂加入到晶化液中，晶化液在导向剂的导向作用下在载体上晶化生长形成β沸石膜，从而在大量降低模板剂用量的条件下，合成出高质量的β沸石模。然后分别将两种方法合成的膜应用在渗透蒸发分离MeOH／MTBE混合体系上，得到了较好的分离效果；最后为了拓展β沸石膜的应用，在陶瓷管载体上制备了beta-NaA催化分离双功能沸石膜，并且将该双功能膜应用在了乙酸和乙醇的酯化反应中，为β沸石膜在膜反应器上的应用奠定了基础。实验得到的主要结论如下：
(1)在研究β沸石膜制备前，首先研究了适合作晶种用的小晶粒β沸石的合成条件，考察了晶化液中不同硅源、不同种类模板剂及其含量、碱度和水含量以及晶化温度、晶化时间等对小晶粒β沸石合成的影响。研究结果表明，以活化硅胶为硅源，TEAOH-TEABr为模板剂，按照SiO_2∶0.02Al_2O_3∶0.45(TEA)_2O∶0.061Na_2O∶0.8(NH_4)_2O∶20H_2O的摩尔比配制合成液，在150℃下晶化72 h可得到粒径为200～300 nm的高结晶度小晶粒β沸石。
(2)研究了在大孔载体管表面预涂晶种的方法，结果表明，对于大孔载体，浸渍提拉预涂晶种法简单易操作且效果好。分别从晶化液组成和模板剂的焙烧脱除等方面对传统的模板剂法在α-Al_2O_3陶瓷管载体表面合成β沸石膜的制备条件进行了考察，结果表明：配制成膜前驱液的最佳摩尔投料比为SiO_2∶Al_2O_3∶Na_2O∶(TEA)_2O∶H_2O=1∶0.02∶0.06∶0.35∶35；在晶化温度为150℃，晶化时间为72 h的条件下，经过6次晶化生长后，能够得到10μm左右厚度的β沸石膜；采用先于氮气气氛下缓慢升温，再于空气气氛下继续焙烧的分两步脱除模板剂的脱模方式较为适宜。用已经得到的最优制备条件再于多孔炭管和多孔不锈钢管载体表面合成β沸石膜，经过比较可知，选用α-Al_2O_3陶瓷管作为载体较为合适。
(3)考察了β沸石导向剂的制备条件，结果表明：用相对廉价且易于操作的活化硅胶做硅源，能够合成出β沸石导向剂；加料顺序和水含量对导向剂合成的影响较大。详细研究了水量、晶化时间以及晶化温度对导向剂法合成β沸石的结构和结晶度的影响，得到了导向剂法合成B沸石的最优合成条件，为进一步用该法合成β沸石膜奠定了基础。考察了水量，导向剂含量，有机物脱除等对导向剂法合成β沸石膜的影响，得出了导向剂法合成β沸石膜的最优合成条件为：按照1SiO_2∶0.033Al_2O_3∶0.317Na_2O∶28H_2O的摩尔配比配制成硅铝溶胶，然后再加入占该硅铝溶胶体积1／8的沸石结构导向剂，搅拌配制成晶化前驱液，在150℃下，晶化60 h；焙烧方式为先于氮气气氛下焙烧，在于空气下焙烧的分两步焙烧的脱模方式。在最优条件下，经过6次晶化生长的β沸石膜表面连续完整，沸石膜层大约9μm厚。对导向剂法合成的膜和传统的模板剂法合成的膜进行了比较，结果表明：在导向剂法合成膜过程中，价格高昂的有机物TEAOH的消耗量比传统方法少90％，这一方面降低了制膜成本，另一方面由于膜中需要脱除的有机物少，使得在焙烧过程中可能产生的晶间缺陷也少，从而提高了膜的质量。导向剂法不单可以应用在β沸石膜的制备上，还可以应用到其他种类需要有机物来做模板剂的沸石膜的制备中。
(4)将两种方法合成的β沸石膜分别应用在渗透蒸发分离MeOH／MTBE混合体系中，详细考察了渗透侧压力、进料组成、进料流速和进料温度对该分离的影响；结果表明，导向剂法合成的膜在分离性能上要明显优于传统方法合成的，其最高分离系数达到了9600。
(5)研究了NaA沸石膜在陶瓷管载体上的合成条件，然后采用导向剂法和模板剂法分别在生长于陶瓷管载体表面的NaA沸石膜表面制备了β沸石膜，最终晶化形成了beta-NaA催化分离双功能沸石膜；将该双功能沸石膜和单一催化功能的β沸石膜应用在了乙酸和乙醇的酯化反应上，通过比较可知，双功能沸石膜由于及时的将反应生成的水移走了，因而打破反应平衡提高了反应的转化率。
Owing to their unique physical and chemical characteristic and similar molecular-sized channel systems, zeolite membranes can not only work at high-temperature, chemical and biological corrosive environments but also have potential applications for separation of different substances at molecular levels and for integration of catalysis and separation processes. In the last decades, zeolite membrane materials drew the growing interests as the cutting age research field in the membrane community. Beta zeolite is a high-silica zeolite possessing a three-dimensional interconnected channel system of 12-O ring large pore and has good heat stability, adsorption capability and proper acidity, so if the beta zeolite membranes can be prepared they will have potential application in separations, even in separation and catalytic membrane reactors due to its unique pore structure and catalytic properties. The research on beta zeolite membrane is very scare, thus it is significant for the beta zeolite membrane to make many efforts on reseach of its preparation and then model application.
The key for the research is how to prepare the beta zeolite membranes with better performance under the conditions of lower cost. The membrane preparation was firstly investigated using conventional template method and the membrane preparation condition was optimized. This includes the synthesis condition optimization of small crystal-size beta zeolite as the seeds, the work on how to improve the quality of seeded layer on support tubes with 3～5μm pore diameter and the optimization of preparation conditions of beta zeolite membranes. On the other hand, a novel method of beta zeolite structure-directing agent (ZSDA) was developed for the preparation of beta zeolite membrane. First, the synthesis of beta ZSDA was investigated. Then, the optimal preparation conditions of beta zeolite prepared by ZSDA method were investigated from the following aspects respectively: content of water, crystallization time and crystallization temperature. By this ZSDA method, organic templates were substituted with beta ZSDA, as a result, a lot of expensive organic templates were saved compared with the conventional method. Then the membranes prepared by both template method and ZSDA method were applied for the pervaporation separation of MeOH/MTBE mixture. The effects of permeation side pressure, feed composition, feed flow rate and feed temperature on the flux and separation factor were investigated, At last to exploit the application of beta zeolite membranes the beta-NaA bi-founctional zeolite membranes were prepared on theα-Al_2O_3 support tubes and applied as membrane reactor for the esterification of acetic acid with ethanol. The main results achieved are as follows:
(1) For the synthesis of small crystal beta zeolite, the results indicated that when crystallization temperature and crystallization time were 150℃and 72h beta zeoltes with small crystal-size in the 200～300 nm range could be prepared according to the molar composition of SiO_2: 0.02Al_2O_3: 0.45 (TEA)_2O: 0.061Na_aO: 0.8 (NH_4)20: 20H_2O. Silicate gel was used as silicon source and TEAOH-TEABr was used as template.
(2) As for the optimal preparation conditions of beta zeolite membranes prepared by conventional template method, it is found that the optimal molar composition of precursor solution is of SiO_2: Al_2O_3: Na_2O: (TEA)_2O: H_2O=1: 0.02: 0.06: 0.35: 35. When the crystallization temperature was 150~C and crystallization time was 72h a continuous and dense membrane with 10μm in thickness, was obtained after 6 synthesis times.Templates were removed by the mode of calcinations in N2 and air orderly. At last beta zeolite membranes were grown on the porous carbon support tubes and porous steel support tubes respectively according to the optimal membranes preparation conditions above obtained. By comparing among the three supports used, it can be known thatα-Al_2O_3 support tubes were the most proper.
(3) It is found that beta ZSDA can be synthesized by using the silica gel as the silicon source that is cheap and easy operational. Moreover, the feed order and content of water had important effects on the synthesis of ZSDA. And the optimal preparation conditions were confirmed as follows: Silicon-aluminum sol was prepared by the molar composition of 1SiO_2:0.033Al_2O_3:0.317Na_2O:28H_2O; Precursor solution was confected by adding the ZSDA into the sol and the content of ZSDA added was 1/8 of the sol in .volume; Crystallization temperature was 150℃and crystallization time was 60h; The organic agent was removed by the mode of calcinations in N_2 and air orderly; A continuous and dense membrane with 9μm in thickness was obtained after 6 synthesis times. Compared with the conventional template method it can be concluded that by ZSDA method not only 90% of costly organic agent was saved but also the quality of membrane was improved due to the less defect was formed when the less organic agent needed to be removed. This ZSDA method can be extended to zeolite membrane preparation of other types in which organic templates are necessary.
(4) The membranes prepared by ZSDA method had better performance in pervaporation separation of MeOH/MTBE mixture. The maximum separation factor reached 9600.
(5) To compare with bi-founctional membranes, single catalytic beta zeolite membranes grown on theα-Al_2O_3 support tubes were also applied in the esterification of acetic acid with. ethanol under the same reaction conditions with that of bi-founcitonal membranes. It can be known from the comparison that conversion rate corresponding to bi-founctional membranes was much higher than that of the single catalytic beta zeolite membranes. This is because the bi-founctionalmembranes had the high performace of removing water, one of the reaction product, so the reaction equribrium was broken and conversion rate was increased.
引文
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[3] Hsieh H P. Inorganic Membranes. AIChE Symp.Ser.. New York. 1988,84(261):1
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