Fast synthesis of TS-1 on porous glass beads in a microreactor for cyclohexanone ammoximation

Supported small TS-1 particles are important catalysts in the ammoximation of ketones, but still facing challenges such as agglomeration in the reaction system and long synthesis time. In this work, we report the fast synthesis of small TS-1 particles supported on porous glass beads in a microreactor. Short crystallization time of only 1.5 h is needed for the synthesis of TS-1 particles with the mean size of ∼200 nm. Effects of aging time, size of the microchannel, sol/support mass ratio, crystallization temperature, and surface areas of the porous glass beads on the morphology and catalytic performance for ammoximation of cyclohexanone have been studied systematically. The as-synthesized supported TS-1 catalyst achieved 82.4% cyclohexanone conversion and > 99% selectivity to cyclohexanone oxime after reaction at 353 K for only 20 min, and the conversion rises to 97.6% if the duration prolongs to 40 min, outperforming the commercial TS-1 catalyst and supported TS-1 catalyst synthesized in an autoclave (crystallized for 48 h).