Synthesis and characterization of bentonites rich in beidellite with incorporated Al or Al-Fe oxide pillars

Abstract

Pillared clays (PILCs) based on bentonite clay from "Bogovina" (Serbia) were obtained using Al3+ and Fe3+ pillaring cations in different ratios. Thorough characterization of the starting material and PILCs was performed for better understanding of the catalytic activity that they had exibited in the catalytic wet peroxide oxidation (CWPO) of organic pollutants in water. The characterization consisted of the following techniques: XRD, XRD of oriented samples (swelling test), Greene-Kelley test (smectite type determination), TGA/DTA followed by XRD analysis of samples heated at characteristic temperatures, elemental analysis using ICP-OES and microwave digestion. FTIR, DR UV-Vis, Mossbauer spectroscopy, nitrogen physisorption at -196 degrees C and SEM imaging. Smectite in admixture with quartz was identified, together with impurities like feldspar, illite, chlorite and X-ray amorphous matter. Smectite mineral was dominantly of the beidellite type. Pillaring led to changes in the d(001) smectite basal spacing and stabilization of the smectite structure. Increasing Fe3+ content of the pillaring solutions resulted in the increased incorporation of iron into the PILCs as isolated octahedrally coordinated Fe3+ cations, smaller and bigger oligonuclear octahedrally coordinated Fe3+ species and octahedrally coordinated Fe3+ particles. The structure of incorporated pillars was similar to that of naturally occurring minerals akageneite and lepidocrocite. Micro- and mesoporosity were improved due to pillaring and the layered smectite structure was retained.