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Cage-like Mesoporous Organosilicas With Isocyanurate Bridging Groups Synthesized by Soft Templating With Poly(ethylene Oxide)-Poly(butylene Oxide)-Poly(ethylene Oxide) Block Copolymer

Cage-like Mesoporous Organosilicas With Isocyanurate Bridging Groups Synthesized by Soft Templating With Poly(ethylene Oxide)-Poly(butylene Oxide)-Poly(ethylene Oxide) Block Copolymer

Rafal M Grudzien, Jonathan P Blitz, Stanislaw Pikus, Mietek Jaroniec

J Colloid Interface Sci. 2009 May 1;333(1):354-62.

PMID: 19200552

Abstract:

Ordered large-pore organosilicas with isocyanurate bridging groups were synthesized via co-condensation of tetraethyl orthosilicate (TEOS) and tris[3-(trimethoxysilyl)propyl]isocyanurate (ICS) in the presence of poly(ethylene oxide)-poly(butylene oxide)-poly(ethylene oxide) (EO(39)BO(47)EO(39)) B50-6600 template under acidic conditions. It was shown that the extraction of the B60-5500 triblock copolymer with acidified ethanol solution was insufficient to remove completely the template; however, calcination of as-synthesized and extracted samples under air atmosphere at 200 degrees C, 250 degrees C and 300 degrees C caused not only the removal of the polymer but also a substantial decomposition of the ICS groups. In contrast, the heat treatment of extracted organosilicas at 360 degrees C in flowing nitrogen was able to fully remove the residual template without degradation of the ICS bridging groups. Characterization of the resulting materials by small angle X-ray scattering (SAXS) and X-ray powder diffraction (XRD) revealed that isocyanurate-containing organosilicas have a body-centered cubic symmetry (Im3m). Argon adsorption-desorption isotherms of these organosilicas revealed cage-like mesopores, high surface areas and large pore volumes. The diameters of spherical cages were found to be very uniform in the range of 12-14 nm. A complete removal of triblock copolymer was confirmed by high-resolution thermogravimetry (TG), Fourier transform infrared spectroscopy (FT-IR) and CHNS elemental analysis (EA). The latter showed that the isocyanurate rings are intact in the framework and their loading is up to 1 mmol g(-1). Moreover, these organosilicas were also synthesized using low acid concentration, double amount of polymer and sodium chloride; in this case the template was completely extracted and there was no need for additional heat treatment.

Chemicals Related in the Paper:

Catalog Number	Product Name	Structure	CAS Number	Price
AP26115708	Tris[3-(trimethoxysilyl)propyl] isocyanurate		26115-70-8	Price

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