Yatomi, Masashi, et al. European Journal of Inorganic Chemistry 2021.19 (2021): 1836-1845.
Tetrabutylammonium fluoride (TBAF) serves as an effective catalyst for the interlayer silylation of cetyltrimethylammonium (C16TMA)-exchanged layered octosilicate with organotriethoxysilanes.
Experimental Protocol: C16TMA-octosilicate is reacted with various organotriethoxysilanes, including octyltriethoxysilane (C8TES), octadecyltriethoxysilane (C18TES), and 3-mercaptopropyltriethoxysilane (MPTES). TBAF is added at a molar ratio of 0.27 relative to the reaction sites. The silylation reaction is carried out under controlled conditions, and the degree of silylation is determined by thermogravimetric analysis and solid-state NMR spectroscopy.
Performance Evaluation: The addition of TBAF significantly enhances the silylation extent across all silane reagents. For C8TES, the silylation degree increases from 33% (without TBAF) to 60% (with TBAF). For C18TES, the silylation degree improves from 23% to 68%. MPTES achieves the highest silylation degree of 89% in the presence of TBAF. TBAF catalyzes the hydrolysis and condensation of silane molecules within the confined interlayer space of the layered silicate.