Intercalation of n-Alkylamines in Proton-Type Layered Titanium(IV) Oxide

• Published in: Bulletin of the Chemical Society of Japan Vol. 79; no. 5; pp. 711 - 716
• Main Authors: Suzuki, Noriko, Hayashi, Naomi, Honda, Chikako, Endo, Kazutoyo, Kanzaki, Yasushi
• Format: Journal Article
• Language: English
• Published: Tokyo The Chemical Society of Japan 2006; Chemical Society of Japan
• ISSN: 0009-2673; 1348-0634
• DOI: 10.1246/bcsj.79.711

Intercalation of proton-type layered titanium(IV) oxides, H2Ti5O11·xH2O (H-TiO2(A)) and H0.7Ti1.825O4·xH2O (H-TiO2(B)), with n-alkylamines were examined for carbon numbers nc = 3–18 in a benzene solution. The amount of intercalated n-alkylamines was about 1 mol per 1 mol of H-TiO2(A) and well-defined X-ray diffraction patterns were observed for nc = 4–14, reflecting the formation of a n-alkylamine bilayer between the layered lamellae. The alkyl chain in the bilayer was found to incline 66° against the basal plane. For nc = 3, a fluffy suspended colloid appeared in the reactant solution and the amount of intercalated amines was about 2 mol per 1 mol of H-TiO2(A), and weak X-ray diffraction peaks suggested the exfoliation and formation of the monolayer or several multilayer sheet of H-TiO2(A). The size of the exfoliated colloid particles was examined using dynamic light scattering photometry. The scatter angle dependence suggested the shape of the colloid particles was a thin lamella and the average radius was estimated to be about 80 and 210 nm for propylamine and tetrabutylammonium hydroxide intercalation compounds prepared in aqueous solution, respectively. The shape of the colloid particles was rather isotropic and the radius was about 1.0 μm for a propylamine intercalation compound prepared in a benzene solution. The result of dynamic light scattering seems consistent with the exfoliation and following coagulation of layered lamellae of H-TiO2(A).