ゼオライト膜の調製とその性質Synthesis zeolite film and its properties
物質工学工業技術研究所National Institute of Materials and Chemical Research, Japan
物質工学工業技術研究所National Institute of Materials and Chemical Research, Japan
ゼオライトの結晶化過程に関する知見を得るという観点から,ゼオライト結晶単独からなるゼオライト多結晶膜の調製について検討した。得られたZSM-5,シリカライト及びZSM-11ゼオライト膜の両面と断面の結晶形態及びAl濃度の解析から,(1)ゼオライト膜は結晶の積み重ねによって形成されること,及び(2)結晶化の初期にはシリケート種が優先的にゼオライト骨格に組み込まれ,Siリッチな結晶が形成されることが明らかとなった。SAPO-5,-11,-17多結晶膜についても同様な結果が得られた。
また,ステンレス及びアルミナ多孔質基板上にシリカライト膜を調製し,その分離膜素材としての可能性について検討した。多結晶膜であるため結晶粒界に基づく細孔や膜の前処理操作の際に生成する欠陥やクラックが問題になるものの,シリカライト膜は本質的にはアルコール選択透過型分離膜として利用できることが明らかとなった。
Zeolite and molecular sieves are widely used in many chemical processes such as heterogeneous catalysis and gas or liquid separation. Recently, great interest has been focused on zeolite films due to their uniform pore sizes and resistance to high temperatures. More recently, we succeeded in preparing polycrystalline zeolite films of ZSM-5, silicalite, ZSM-11 and SAPO by using a Teflon slab, a filter paper and a porous substrate. As the Al distribution and the change in the morphology along the width of film reflected the time course of the crystal growth, we could get much information regarding the crystal growth process by analyzing the film obtained. It was found that the polycrystalline zeolite films are formed through a successive accumulation of zeolite crystals. It was also found that during the initial crystallization of zeolite, the zeolite crystals with high SiO2/Al2O3 ratios are generated.
Next, we investigated the liquid separation potential of the zeolite film. Separation of ethanol/water mixture was carried out by pervaporation through the silicalite film on a porous stainless steel support. It was found that the film has the high ethanol permselectivity with a separation factor α(EtOH/H2O) of approximately 60 compared to various membranes reported up to now, indicating that the silicalite film is effective for alcohol concentration process.
Key words: Zeolite film; Silicalite; ZSM-5; Separation; Pervaporation
© 1993 ゼオライト研究会© 1993 Japan Association of Zeolite
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