A facile
aerosol-assisted technique was employed for the design
of a new class of composite zeolite catalyst material with spherical
morphology. This technique enables the one-step encapsulation of zeolite
microcrystals into the matrix of spherical mesoporous silica particle
supports such as MCM-41. By introducing presynthesized zeolite microcrystals
into precursor solutions containing the templating surfactant and
the silica precursor followed by aerosolization through nozzles larger
than the microcrystals, it is possible to entrain the microcrystals
in the aerosol droplet. Transport of the droplet through the heated
zone of the furnace leads to hydrolysis and condensation of the silica
precursor (tetraethyl orthosilicate, TEOS) in each droplet and the
formation of spherical particles of MCM-41 containing embedded zeolite
microcrystals. This bottle-around-a-ship procedure to make zeolite-MCM-41
composites is extremely effective and can be easily scaled up. Detailed
characterization of these composite particles reveals that up to 75
wt % of ZSM-5 zeolite can be embedded in MCM-41 microspheres with
no loss of fidelity in particle morphology. To verify access of the
reactants to the zeolite, we impregnated the ZSM-5 with nickel (Ni@ZSM-5)
prior to encapsulation in MCM-41, and have shown the feasibility of
the system to the model reaction of the liquid phase catalytic reduction
of 4-nitrophenol to 4-aminophenol. While the reaction proceeds efficiently,
there are diffusional restrictions to the transport of 4-nitrophenol
resulting in a composite catalyst effectiveness factor of 0.4. The
encapsulation of zeolite crystals within a micrometer-sized mesoporous
MCM-41 shell provides structural stability to the zeolites and could
reduce the pressure drop across a fixed bed tubular reactor due to
the increased particle size of the composite. Potential applications
of such composite particles include the ability of the MCM-41 to act
as sacrificial adsorbents for coke and catalyst poisons, thus extending
the life of the active material.