Influence of the synthesis parameter on the interlayer and framework structure of lamellar octadecyltrimethylammonium kanemite

• ODTMA was efficiently intercalated kanemite under all synthesis conditions.
• Lamellar structure was observed in ODTMA-kanemite with five-member ring formation.
• ODTMA/Si ratio, stirring, pH and washing affected the final products.

Inorganic–organic nanostructures, used as host materials for selective adsorption of functional molecules and as mesostructured material precursors, can be constructed by the interlayer modification of inorganic layered materials with surfactants. The formation mechanism is mainly determined by the surfactant assemblies in the 2D limited space. In this paper, a detailed structural analysis of the lamellar mesophases prepared from kanemite, a lamellar silicate, and octadecyltrimethylammonium (ODTMA) under various conditions was reported. The adsorbed amount of ODTMA and the long and short range structural orders were explored by TGA, XRD, IR/FT and MAS NMR spectroscopies. The results revealed that ODTMA molecules were efficiently intercalated in the interlayer space of kanemite and, in all synthesis conditions, an ordered lamellar structure was obtained. The ODTMA adsorption in kanemite caused changes not only in the interlayer space but also in the silicate framework, where five-member rings were formed. The characteristics of the final products were influenced by the synthesis conditions, although the separation mode, filtration or centrifugation, was not relevant. Therefore, the adsorption conditions of ODTMA in kanemite will contribute to the design of novel layered materials with potential environmental and technological use.

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