Abstract
A new disordered microporous silica and its titanium silicate analog have been synthesized using a bola-amphiphile surfactant 1,12-diamino dodecane (DADD) as a structure directing agent (SDA). Powder X-ray diffraction, N 2 sorption, 29Si MAS NMR, UV–visible diffuse reflectance, FT-IR spectroscopic tools, and TEM and SEM–EDS were used to characterize this material. Only low angle peak was observed in the XRD for all the samples. TEM images indicated a wormhole-like structure in this material similar to that observed for mesoporous silica HMS, MSU-1, MSU-X, etc. or microporous Si-TMS7. Pore diameter of the micropore estimated from N 2 adsorption isotherms was ≈11.2 Å. Spectroscopic data indicated the incorporation of titanium in the tetrahedral silica network in this material. Three microporous type, Ti-DMS1 titanium silicate samples were synthesized with Si/Ti mole ratios of 24.5, 46.5 and 68.0 in the final solid products. After the removal of the template through calcination this microporous titanium silicate showed an excellent catalytic activity in the ammoximation of bulky ketones using dilute aqueous hydrogen peroxide and aqueous ammonia.
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