Crystallization process of zeolite rho prepared by hydrothermal synthesis using 18-crown-6 ether as organic template

Abstract

There are many viewpoints on the formation mechanisms for zeolites, but the details are not clear. An understanding of the elementary steps for their formation is important for the development of large-scale membranes and efficient manufacturing processes. In this study, the effects of silicon, aluminum, and the incorporation of 18-crown-6 (18C6) ether, on the formation of zeolite rho, using 18C6 as the structure directing agent (SDA) have been investigated by using field emission scanning electron microscopy (FE-SEM), energy dispersive X-ray fluorescence spectrometry (EDX), nuclear magnetic resonance spectroscopy (NMR), thermo gravimetric analysis (TGA), and the pH measurement. These results suggested that a zeolite rho has four synthesis steps; (1) 0–3h, the dehydration and condensation reaction between the silica and alumina to form amorphous aluminosilicates; (2) 3–20h, the particle growth and aggregation process for the amorphous aluminosilicates; (3) 20–48h, the crystallization and crystal growth of zeolite rho, with the incorporation of 18C6; and (4) 48–96h, gentle growth with an increase in Na/Si ratio and a change in rate for the bounding state between the silica- and the alumina-based species. We consider the above to reflect the four steps for the formation of zeolite rho.