Hydrothermal synthesis and characterization of copper containing crystalline silicate mesoporous materials from gel mixture

• Published in: Applied clay science 2004-06, Vol.25 (3), p.195-205
• Main Authors: Chatterjee, M, Iwasaki, T, Onodera, Y, Hayashi, H, Ikushima, Y, Nagase, T, Ebina, T
• Format: Article
• Language: English
• Subjects: Characterization; Cu-SCMM; Earth sciences; Earth, ocean, space; ESR; Exact sciences and technology; Mineralogy; Selective hydrogenation; Silicates; Supercritical carbon dioxide
• ISSN: 0169-1317; 1872-9053
• DOI: 10.1016/j.clay.2003.11.003

Novel copper-containing crystalline silicate mesoporous materials (SCMM) have been synthesized by the hydrothermal treatment of slurries of silicon–magnesium–copper hydroxide precipitates along with quaternary ammonium salt. X-ray diffraction (XRD) and transmission electron microscopy (TEM) confirmed a house-of-cards type structure consists of very thin platy silicates. Nitrogen adsorption–desorption isotherms of calcined material show that it has a high surface area (∼550 m 2 g −1) and porosity properties. Pore characteristics are similar to that of MCM-41 and FSM-16, and fine-tuning of the pore size was achieved easily by modulating the synthesis temperature. Identification and the location of copper species in Cu-SCMM were done by X-ray photoelectron spectroscopy (XPS) and electron spin resonance (ESR), respectively. ESR data of air-dried Cu-SCMM consist of clearly defined g ||=2.34, A ||=140×10 −4 cm −1 and g ⊥=2.08 at room temperature and g ||=2.34, A ||=160×10 −4 cm −1 and g ⊥=2.10 at 77 K. The resulting material exhibited superior catalytic activity towards the hydrogenation of α–β unsaturated aldehyde in supercritical carbon dioxide.