P. Van Der Voort et al., Synthesis of stable, hydrophobic MCM-48/VOx catalysts using alkylchlorosilanes as coupling agents for the molecular designed dispersion of VO(acac)(2), J PHYS CH B, 103(46), 1999, pp. 10102-10108
The use of dimethyldichlorosilane as a coupling agent for the grafting of V
Ox structures on the MCM-48 surface produces a material that is simultaneou
sly hydrophobic (immiscible with water) and very active (all V centers are
accessible, even for water molecules). The VOx surface species are grafted
by the molecular designed dispersion of VO(acac)(2) on the silylated surfac
e, followed by a calcination in air at 450 degrees C. These hydrophobic MCM
-48 supported VOx catalysts are thermally stable up to 500 degrees C. The g
rafted VOx surface species are very resistant toward leaching-out in aqueou
s media. Also, the structural and hydrothermal stability has improved enorm
ously. The crystallinity of the materials does not decrease when the sample
s are subjected to a hydrothermal treatment at 150 degrees C and 4.7 atm pr
essure. A reaction mechanism is proposed and consolidated by FT-IR, Raman s
pectroscopy, and UV-vis diffuse reflectance. Pore size distributions, water
adsorption isotherms, and X-ray diffractograms confirm the structural stab
ility of these materials.