Effect of the degree of template removal from mesoporous silicate materials on their adsorption of heavy oil from aqueous solution

The key aim of this study is to evaluate the adsorption of heavy oil from aqueous solutions with different oil contents over mesoporous silicate materials having different surfactant template contents. The mesoporous silicate materials have been synthesized from tetraethylorthosilicate as a silica precursor and cetyltrimethylammonium bromide as a template using the sol-gel technique. Four samples were prepared by (1) totally removing the template using the calcination process, (2) partially removing the template via ethanol extraction, (3) partially removing the template via water extraction, and (4) keeping the template as synthesized, respectively. These four samples have been characterized using X-ray diffraction, nitrogen adsorption, thermal gravimetric analysis and Fourier transformed infrared. The effect of the degree of template removal of these mesoporous materials for the oil removal has been investigated. The oil removal is inversely proportional to the surfactant content in the mesoporous material, being highest for the calcined sample but lowest for the as-synthesized sample. The kinetic of oil adsorption over the calcined material has been also studied and the data obtained fit well a second-order model

Modifying the Hierarchical Porosity of SBA-15 via Mild-Detemplation Followed by Secondary Treatments

Fenton-chemistry-based detemplation combined with secondary treatments offers options to tune the hierarchical porosity of SBA-15. This approach has been studied on a series of SBA-15 mesophases and has been compared to the conventional calcination. The as-synthesized and detemplated materials were studied with regard to their template content (TGA, CHN), structure (SAXS, TEM), surface hydroxylation (BlinCarterets approach), and texture (high-resolution argon physisorption). Fenton detemplation achieves 99% of template removal, leading to highly hydroxylated materials. The structure is better preserved when a secondary treatment is applied after the Fenton oxidation, due to the intense capillary forces during drying in water. Two successful approaches are presented: drying in a low-surface-tension solvent (such as n-BuOH) and a hydrothermal stabilization to further condense the structure and make it structurally more robust. Both approaches give rise to remarkably low structural shrinkage, lower than calcination and the direct water-dried Fenton. Interestingly, the derived textural features are remarkably different. The n-BuOH exchange route gives rise to highly hierarchical structures with enhanced interconnecting pores and the highest surface areas. The hydrothermal stabilization produces large-pore SBA-15 structures with high pore volume, intermediate interconnectivity, and minimal micropores. Therefore, the hierarchical texture can be fine-tuned in these two fashions while the template is removed under mild conditions