成果報告書詳細
管理番号20110000001566
タイトル*平成22年度中間年報 グリーン・サステイナブルケミカルプロセス基盤技術開発 規則性ナノ多孔体精密分離膜部材基盤技術の開発(9)
公開日2011/12/13
報告書年度2010 - 2010
委託先名国立大学法人大阪大学
プロジェクト番号P09010
部署名電子・材料・ナノテクノロジー部
和文要約和文要約等以下本編抜粋:1. 研究開発の内容及び成果等
「新規な親水性ゼオライト分離膜の探索」
1.緒言
ゼオライトは、細孔径の異なる多種の(酸素6、8、10、12員環)構造を有し、多様な用途に対応できる。しかし、幅広い需要に貢献するためには、多種のゼオライト膜を実用化・工業化する必要がある。すでにモルデナイト(MOR型)、ZSM-5(MFI型),Y 型(FAU型)などの各種規則性ナノ多孔体膜合成および分離性能について論文・特許等で公表されているが、本研究ではそれ以外の新規な膜材料を探索し、合成手法および分離特性に関する基礎的データを集める。耐酸性・高透過流束・高選択性を有する膜材料の設計指針を打ち出す。本研究では、層状ゼオライトMCM-22とリン酸塩系ゼオライトSAPO-34の製膜に取り組んだ。H21年度では、平膜状アルミナ基板への製膜条件の探索を行ってきたが、H22年度は、管状アルミナ基板上での製膜を行い、製膜条件の探索および結晶化機構・膜形成機構の解明に取り組んだ。
英文要約Development novel hydrophilic zeolite membranes
Many zeolite membranes have been extensively studied so far, such as ZSM-5 (MFI), silicalite (MFI), mordenite (MOR), faujasite (FAU) and A-type (LTA). But, for applying zeolite membranes to versatile applications, it is required to develop new membrane materials and investigate on their separation/permeation properties. The objective of this study is to offer a direction of the optimum design of zeolite membranes with high permeation flux, high separation factor and high stability in solvents. This year, we have developed the following two types of zeolite membranes (SAPO-34 and MCM-22) on a tubular-type alumina support. A membrane formation mechanism of the SAPO-34 and MCM-22 membranes and their permeation/separation properties were studied.
(1) SAPO-34 membranes
The SAPO-34 membranes were grown on a porous α-alumina tube by using a secondary growth technique, which consists of a deposition of seed crystals on the substrate followed by a crystal growth under hydrothermal conditions. From gas permeation and vapor permeation results, we found that the SAPO-34 membranes were not compact when SAPO-34 crystals with crystal sizes of 8 μm and 0.8μm were used as seed. Instead, when SAPO-34 nanocrystals (80 nm) were used as a seed, the SAPO-34 membrane shows high separation factors (α >1000) for the water/isopropanol (15/85 w/w) vapor permeation at 110°C. From SEM observation, we found that SAPO-34 seed crystals were partly dissolved and then amorphous phase were deposited on the surface. The amorphous layer was changed to SAPO-34 crystals. The dissolved species in the early stage of synthesis seems to play an important role in the deposition of amorphous phase (precursor for SAPO-34 crystals) and further nucleation and crystallization.
(2) MCM-22 membranes
MCM-22 membranes were prepared on a porous α-alumina tube by using a secondary growth technique. Here, two types of seed crystals, MCM-22 and delaminated MCM-22 (MCM-22(D)), were used. The MCM-22 membrane prepared using MCM-22(D) seed crystals (MCM-22(D) membrane) was composed of a monolayer of MCM-22 crystals with a thickness of 5 μm, which is much thinner than that of the MCM-22 membrane prepared using MCM-22 seed crystals (15-20 μm). Vapor permeation of water/acetic acid mixtures through the MCM-22 membranes was studied. The MCM-22(D) membranes calcined at 400 ºC shows a separation factor as high as 78 with a water permeance of 4×10-8 mol m-2 s-1 Pa-1 at 120 °C. The elevated calcination temperature to 500 ºC resulted in a decrease of separation factor. The MCM-22(D) membrane calcined at 400 ºC has a hydrophilic internal surface because of a presence of silanol groups in the framework structure, which contributes to the high selectivity to water permeation.
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