Crystals (Jan 2023)
Synthetic Conditions for Obtaining Different Types of Amine-Holding Silica Particles and Their Sorption Behavior
Abstract
The Stöber version of a sol-gel method of co-condensation of two alkoxysilanes (structuring tetraethoxysilane (TEOS) and functionalising N-containing silane) in an ammonia medium was used for the one-pot synthesis of spherical silica particles with ≡Si(CH2)3NH2, ≡Si(CH2)3NH(CH2)2NH2, and ≡[Si(CH2)3NH]2 functional groups with available groups content of 1.3–2.3 mmol/g. The materials were researched by a range of methods, including SEM, TEM, IR spectroscopy, 13C, and 29Si solid-state NMR spectroscopy, acid-base titration, and thermal analysis to identify the peculiarities of the morphology, functional groups content, composition, and thermal resistance of the surface layers in the synthesised samples. The type of N-containing silane was shown to affect the structure and properties of the synthesised spherical particles. The silane with the simplest, 3-aminopropyl, functional group caused the formation of nonporous material composed of large 600–800 nm spherical microparticles. Meanwhile, the complication of functional groups enhanced the emergence of small 15 nm primary particles and the origination of porosity, generated by the slits between particles and particle agglomerates. Thereafter, the sorption properties of the synthesised hybrid materials for nickel(II) and copper(II)ions, and bovine serum albumin (BSA) were also found to be dependent on the structure of the materials and the type of incorporated functional group. The maximal static sorption capacity values towards the targeted adsorbates were shown by the samples with 3-aminopropyl groups (1.27 mmol Ni/g), diamine groups (1.09 mmol Cu/g), and secondary amine groups (204.6 mg BSA/g). The conducted research opens up the prospects of directed one-pot synthesis of amino-functionalised hybrid organosilica materials for different applications.
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