Hexafluorosilicic Acid (FSA): from Hazardous Waste to Precious Resource in Obtaining High Value-Added Mesostructured Silica

Vacca, Mirko Antonio;Cara, Claudio;Mameli, Valentina;Sanna Angotzi, Marco;Scorciapino, Mariano Andrea;Cutrufello, Maria Giorgia;Musinu, Anna;Tyrpekl, Vaclav;Pala, Luca;Cannas, Carla

2020-01-01

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Abstract

In this work, industrial waste hexafluorosilicic acid (H2SiF6 or FSA) has been proven to be a low-cost alternative to silicate esters for the synthesis of high-quality MCM-41 (high surface area, high degree of order, narrow pore size distribution, high thermal stability) through a head-to-head comparison between the most common silica precursor, tetraethylorthosilicate (TEOS), and FSA. The effect of different parameters such as temperature, time, hydrothermal treatment, and the presence of ethyl acetate has been explored by studying the textural, structural, and morphological features. On the most promising samples, thermal and hydrothermal stability has been assessed, indicating a higher thermal stability for the FSA-derived sample, due to the thicker walls, and comparable hydrothermal stability. The mother solution treatment has allowed the obtainment of nanostructured fluorite as an additional valuable product and a CTAB-rich ammonia solution for successive synthesis with FSA. Recovery processes for the templating agent entrapped in the MCM-41 mesostructure have also been explored for both FSA- and TEOS-derived samples, showing an easier removal in the case of FSA-MCM-41. Moreover, mesostructured silica derived from FSA has also been proven to be an ideal support to design efficient and regenerable mesostructured iron oxide-based sorbents for H2S removal from syngas, showing similar performance to that of the corresponding nanocomposite prepared from TEOS.