Regioselective Approach to Characterizing Increased Edge Availability in Layered Crystal Materials following Layer Expansion: Reaction of Kaolinite with Octadecyltrimethylammonium Salts

Abstract

In this paper, the regioselective reactions of kaolinite and methoxy-modified kaolinite (MeO-Kaol), methanol-expanded kaolinite, with octadecyltrimethylammonium salts are compared. This study mainly concerns the reactions of kaolinite or MeO-Kaol with octadecyltrimethylammonium chloride (C18TAC) in methanol and the subsequent exhaustive washing of the resultant products with ethanol. X-ray diffraction patterns of the products reveal no intercalation of C18TAC between pristine kaolinite layers. Additionally, intercalation and subsequent deintercalation of C18TAC proceed in the product using MeO-Kaol. In the Fourier-transform infrared spectra, the intensities of CH2 stretching bands of the product prepared using MeO-Kaol drastically increase compared to those using kaolinite. In addition, CH2 stretching bands of the product using kaolinite are hardly observed without enlarging the spectrum. The product using MeO-Kaol also displays mass loss in the range of 200–300 °C in the thermogravimetric curve and a nitrogen content with 0.15 mass% estimated using the CHN analysis. These results therefore demonstrate an increase in the available reactive edges in the layered crystal material following an expansion of the stacked layers.

Keywords

• kaolinite
• edge modification
• alkylammonium ion
• organically-modified kaolinite
• intercalation