珪藻土表面へのNaAゼオライトの生成Preparation of NaA zeolite on surface of diatomite
秋田大学鉱山学部資源・素材工学科Division of Materials Process Engineerlng, Department of Geosiences, Miming Engineering and Materials Processing, Mining Colleg, Akita University
秋田大学鉱山学部資源・素材工学科Division of Materials Process Engineerlng, Department of Geosiences, Miming Engineering and Materials Processing, Mining Colleg, Akita University
筆者らは秋田県産珪藻土資源の有効利用および高付加価値化を目的として,森吉珪藻土原鉱含有鉄分の有機酸による除去プロセスを開発し,さらに酸処理して得られた珪藻殻表面にゼオライトを生成させることによる表面改質を行い,吸着性を有するろ過助剤としての特性評価を行っている。ここでは温シュウ酸処理の後,650°C,2時間仮焼して得た非晶質シリカ表面でAlイオン,Naイオン,及びH2Oを反応させてNaAゼオライトを生成させた実験結果を紹介する。
原料シリカに対しAl,Na各原子比をそれぞれ(0.25~0.42),(0.5~0.7),水のモル比を(10~42)の範囲に調整した懸濁物を回分式撹拝槽中(50~80)°C,(4–48)時間反応させ,時間経過に伴うシリカ表面へのNaAゼオライトの析出,成長を観察した。そして,結晶化度の経時変化をもとに結晶化速度を求めたところ,その速度は反応温度が高いほど,またケイ酸ナトリウム試薬を出発原料とした場合に比してとくに反応初期で速いことがわかった。生成固体の内部表面積,および炭酸ガス吸着量は結晶化の進行に伴って特異な変化をする。
For efficient utilization and addition of value for doatomite resources in Akita Prefecture, we have developed a decreasing process of inherent iron contained in the Moriyoshi diatomite ore with help of organic acids. Modifying the surface of acid-treated diatomite shell by preparation of zeolite, we are evaluating possible characteristics for a diatomite filter-aid which has adsorption capacity.
Some experimental results are introduced of preparation of NaA zeolite by reacting Al and Na ions and H2O on the surface of amorphous silica obtained through calcination of original ore at 650°C for 2hrs after treating with warm oxalic acid.
By adjusting the atomic ratios of Al and Na, (0.25~0.42), (0.5~0.7) and the mole ratio of H2O, (10~42) to reactant silica, a slurry was served in a batch stirred vessel for observation of crystallization and growth of NaA zeolite on the silica surface at (50~80)°C for (4~48)hrs. Crystallization rate, evaluated by change in crystallinity with time, increased with reaction temperature and especially in the initial reaction-time region with comparison to the case of sodium silicate reagent as a starting material. Internal surface area of produced solid and its adsorption capacity of carbon dioxide changed uniquely as crystallization progressed.
Key words: Diatomite; NaA Zeolite; Oxalic Acid; Filter Aid
© 1994 ゼオライト研究会© 1994 Japan Association of Zeolite
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