Synthesis of organic–inorganic hybrid MSU-1 for separation and catalytic applications

A series of spherical hybrid MSU-1 composed of homogeneously distributed ethane groups in a silica framework was prepared via the twostep sol–gel process using 1,2-bis(triethoxysilyl)ethane (BTEE) in a nonionic alkyl polyethylene oxide (Tergitol 15-S-12) surfactant solution. Hydrolysis of BTEE was conducted in acidic condition at room temperature and condensation of silicate species was promoted by F− catalyst at 65 °C. The hybrid MSU-1 products synthesized were characterized by XRD, N2 adsorption/desorption isotherm, TGA, SEM, and TEM after solvent extraction. The materials were made of wormhole-like mesopore structures, and surface area, pore volume, and pore diameter increased with the concentration of NaF (NaF/BTEE = 0.03–0.15) and temperature (35–65 °C). Incorporation of the organic fraction was confirmed by 29Si and 13C CP MAS NMR. The hybrid MSU-1, after C8 grafting and end-capping, demonstrated a good performance as a stationary phase in chromatography. The hybrid MSU-1-supported palladium material also showed excellent catalytic performances in Sonogashira cross-coupling reactions of aryl iodide with phenylacetylene.