NaA、FAU和ZSM-5沸石膜的制备及其应用
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摘要
微孔沸石是指有效孔径在2nm以下的一种分子筛,到目前为此已经发现或人工合成出100多种,而目前最常用的有LTA、FAU、MFI等类型分子筛。微孔沸石膜具有与分子尺寸相近的孔道体系,耐高温、耐腐蚀以及优异的分离性能,可在分子级别上进行物质分离,实现催化分离一体化优点,因而在膜分离、渗透蒸发及膜反应器等方面具有巨大的应用前景,近十多年来,沸石膜的研究取得了较大的发展。因此,进行微孔沸石膜的制备和应用研究具有重要的意义。
     本文主要进行了以下几方面的研究:利用动态法在载体内表面合成NaA沸石膜及其应用在乙醇脱水应用中;NaY沸石膜的制备及其在苯/环己烷和二氯乙烷/氮气混合系统的分离规律;NaX沸石膜的制备及其在苯/氮气混合系统的分离规律;ZSM-5沸石膜的制备及膜反应器在乙苯脱氢制苯乙烯过程的应用。
     采用动态水热合成在α-Al_2O_3陶瓷管载体内表面形成一层致密的NaA膜,膜管的H_2渗透率为7.66×10~(-7)mol/(m~2·s·Pa),H_2/C_3H_8的理想分离因数为4.85。并将动态合成的NaA膜应用在水/乙醇混合物体系中,取得了良好的分离效果。当进料乙醇含量为90wt.%,渗透温度为70℃时,乙醇/水的分离因数为9500,表明用动态法在陶瓷管内表面制备高性能的NaA沸石膜是可行的。
     采用热浸渍法引入晶种,通过二次生长在α-Al_2O_3陶瓷管的外表面上合成了NaY型沸石膜。将制备出的NaY沸石膜应用于渗透汽化分离苯和环己烷的实验中,并考察了操作温度、进料流速、膜后真空度、进料液浓度等因素对分离效果的影响。实验结果表明,NaY型沸石膜对苯具有良好的选择性,对于苯的质量含量为50%的苯/环己烷混合体系,操作温度为70℃时,分离因子可达13.6,渗透通量为0.173kg·m~(-2)·h~(-1)。
     基于NaY沸石膜对二氯乙烷较强的吸附能力,在膜孔内易产生毛细凝聚,将其用于二氯乙烷和氮气混合气体的分离,取得了较好的分离效果。结果表明分离因数随膜两侧的压差变化是先增加,达到一定值后,随压差的增加而下降;分离因数随温度的提高而下降,当膜两侧压差为50kPa时,分离因数达到最高值17.7;不同阳离子交换后,沸石膜对混合系统的分离也呈现了不同的结果,其中吸附能力较强的CaY沸石膜对混合系统的分离效果最好,二氯乙烷/氮气分离因数最高时接近30。5种沸石膜对二氯乙烷和氮气的分离因素大小顺序为:CaY>NaY≈BaY>KY≈LiY。
     按一定配方在α-Al_2O_3陶瓷管载体外表面合成的NaX沸石膜,其H_2渗透通量为2.15×10~(-6)mol/(m~2·s·Pa),H_2/C_3H_8的理想选择因数为6.19;通过实验发现,由于苯的分子结构中存在π键,与Ag~+产生络合吸附,增加了苯吸附扩散透过膜的能力,使Ag~+改性后的X型沸石膜可以更好的用于苯和氮气混合气的分离。NaX沸石膜经过离子改性后,膜的性质发生了很大的变化,渗透数据表明比未改性前分离因数增大。NaX沸石膜对苯和氮气混合系统的分离因数随膜两侧的压差、原料气浓度和原料气流速的变化而变化,当离子交换度达到最大值时,分离因数也达到最大值。在压差为40kPa,进气流速为180ml/min,浓度为12%时,改性完全的X型沸石膜达到最好分离效果,分离因数为30.1,实现了苯和氮气混合气的高效分离。
     最后以一定的合成液配方合成连续的ZSM-5沸石膜,室温下,制备的ZSM-5沸石膜的H_2/C_3H_8的理想选择因数为10.86;合成的沸石膜组装成膜反应器应用于乙苯脱氢反应体系,并考察了抽真空、液体空速、反应温度和吹扫气速对反应体系的影响。随着膜管两侧压差的增加,副产物苯几乎不变,甲苯略有上升,二段乙苯的转化率有明显提高,苯乙烯选择性略有下降。发现液体空速大时,副产物苯和甲苯略有降低,苯乙烯选择性提高,但乙苯的转化率有所下降。通过使用N_2气吹扫时,二段反应器乙苯的转化率和苯乙烯的选择性提高更明显,二段反应器乙苯的转化率比常压下提高了7.52%。
The micropore zeolite means molecular sieve with the the pore size under 2 nm.Up to now,more than one hundred kinds of micropore molecular sieve have been found or synthesized.The most popular molecular sieves are LTA,FAU,MFI.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 environment but also have potential applications for separation processes.In the last decades, much progresses have been made on the research of zeolite membranem.It is very important to research the preparation and application of zeolite membrane.
     The main research of this paper was as follows:The NaA membrane was synthesized on the inner surface ofα-Al_2O_3 support with the dynamic hydrothermal synthesis,and this kind of membrane was applied in the separation of ethanol/water;The effect of parameters on synthesis of the NaY membrane was studied,and it was used in the separation of benzene/cyclohexane and dichloroethane/nitrogen.The effect of parameters on synthesis of the NaX membrane was researched,and it was used in the separation of benzene/nitrogen. The ZSM-5 membranes were synthesized and was applied in the dehydrogenation of ethylbenzene to styrene.The main results achieved were as follows:
     The NaA membrane was synthesized on the inner surface ofα-Al_2O_3 support with the dynamic hydrothermal synthesis,the H_2 permeance of as-synthesized NaA membrane was 7.66×10~(-7)mol/(m~2·s·Pa),the idea separation factor of H_2/C_3H_8 was 4.85,respectively.This kind of membrane was applied in the separation of ethanol/water and the permeance flux was 1.5kg/(m~2·h) and the separation factor was 9500.These results indicated that the NaA membrane prepared with the dynamic hydrothermal synthesis was feasible.
     NaY zeolite membranes in out surface ofα-Al_2O_3 ceramic tube were synthesized by forming a seeding layer via hot dip-coated method,followed by secondary crystallization method.NaY zeolite membranes were used to separate the mixture of benzene and cyclohexane by pervaporation.The influence of operation temperature,operation pressure difference,feed flow rate and content of benzene in feed was studied thoroughly.The NaY zeolite membranes showed benzene permselective in pervaporation experiments (benzene-cyclohexane).With mass fraction of benzene 50%in benzene-cyclohexane mixture, separation factor of the membrane was 13.6,permeation flux was 0.173kg·m~(-2)·h~(-1) at 70℃.
     Y-type membranes were also used to separate the mixture of dichloroethane and nitrogen. The result showed that the separation factor was increased with the increasing of pressure difference.When it reached certain value,the separation factor was decreased with the increasing of pressure difference.When the pressure difference was 50 kPa,the separation factor was 17.7,which was the highest value.Membranes showed different separation ability when they were exchanged with different cations.The CaY membrane showed the separation effect and highest separation factor was almost 30.The order of separation factor of five Y-type membranes was CaY>NaY≈BaY>KY≈LiY.
     The NaX membrane was synthesized on outer surface of theα-Al_2O_3 support,the permeance rate of H_2 was 2.15×10~(-6)mol/(m~2·s·Pa),the idea separation factor of H_2/C_3H_8 was 6.19;NaX zeolite membranes were used to separate the mixture of benzene and nitrogen as a new method.The influence of pressure difference,the speed and concentration of the mixture and ion-exchanged degree are studied thoroughly.The result shows that the separation factor is changed with the pressure difference,speed and concentration change.Membranes show better separation ability when they are exchanged with Ag~+.When the pressure is 40kPa,the speed is 180ml/min and the concentration is 12%,Ag~+-exchanged completely membranes gain the best separation factor:30.1.
     The ZSM-5 zeolite membrane was synthesized and the idea separation factor of H_2/C_3H_8 was 10.86.The ZSM-5 zeolite membrane was applied in dehydrogenation of ethylbenzene to styrene.With the increasing of pressure difference,the by-product of benzene hardly changed and toluene slightly increased,the conversion of ethylbenzene improved evidently and the selectivity of styrene decreased slightly.With the increasing of space speed,the by-product of benzene and toluene slightly decreased,the conversion of ethylbenzene decreased and the selectivity of styrene increased.With N_2 as the sweep gas,the conversion of ethylbenzene and the selectivity of styrene advanced more remarkably,the convesion rate improved 7.52% compared to the condition of the atmospheric pressure.
引文
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