A kaolinite-NMF-methanol intercalation compound as a versatile intermediate for further intercalation reaction of kaolin
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A kaolinite-NMF-methanol intercalation compound as a versatile intermediate for further intercalation reaction of kaolinite Yoshihiko Komori and Yoshiyuki Sugahara Department of Applied Chemistry, School of Science and Engineering, Waseda University, Ohkubo-3, Shinjuku-ku, Tokyo 169, Japan
Kazuyuki Kurodaa) Department of Applied Chemistry, School of Science and Engineering, Waseda University, Ohkubo-3, Shinjuku-ku, Tokyo 169, Japan, and Kagami Memorial Laboratory for Materials Science and Technology, Waseda University, Nishiwaseda-2, Shinjuku-ku, Tokyo 169, Japan (Received 17 September 1997; accepted 6 January 1998)
A kaolinite-organic intercalation compound containing methanol was proved to be a versatile host for further displacement reaction with alkylamines. Kaolinite-organic intercalation compounds with polar molecules, such as N-methylformamide (NMF) and formamide, were used as the starting materials. After stirring the kaolinite-NMF intercalation compound with methanol, the basal spacing increased to 1.11 nm. The 13 C MAS NMR result of the product indicated that methanol was intercalated into kaolinite by partial displacement with NMF. By use of the methanol-treated kaolinite intercalation compound as the intermediate, alkylamines were intercalated into the interlayer space of kaolinite by displacing with methanol.
I. INTRODUCTION
Intercalation reaction of inorganic layered materials means the insertion of inorganic and/or organic guest species between the layers while maintaining the structural features of the host materials. The reaction has been well known as a method for organic modification of the interlayer surfaces of inorganic layered materials by “soft-solution processing.” Kaolinite is a clay mineral with the 1 : 1-type layered structure1 and has been investigated extensively from both industrial and academic viewpoints.2 Since the bonding between the layers of kaolinite is due to hydrogen-bonding between hydroxyl groups on the AlO6 octahedral sheets and the SiO4 tetrahedral sheets, only a limited number of polar guest species such as N-methylformamide (NMF), formamide (FA), and dimethylsulfoxide (DMSO) can be intercalated directly. Intercalation with a variety of the guest species can be extended by the so-called “displacement method,”3 in which preintercalated organic species (NMF or DMSO, for example) in kaolinite can be displaced with various types of organic molecules such as acrylamide,4 acrylic acid,5 lactam,6 and ammonium acetate.7 By utilizing a kaolinite-ammonium acetate intercalation compound as the second intermediate, further intercalation reactions of alkylamines,8,9 acrylonitrile,7 and vinyl-2-pyrrolidone10 have also been reported. By utilizing hydrated kaolinite as another intermediate, intercalation of alcohol11,12 and
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J. Mater. Res., Vol. 13, No. 4, Apr 1998
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pyridine13 was successful. These intermediates have been effective
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