Supported Rh catalysts on FSM-16 were prepared by treating FSM-16, impregnated with [Rh(OAc)(2)](2) in supercritical carbon dioxide at 398 K and 30.3 MPa, followed by calcination and hydrogen reduction. The resulting Rh/FSM-16 catalysts were characterized by CO chemisorption, XRD, TEM, FTIR and EXAFS, and catalytic performances of the Rh/FSM-16 were tested in butane hydrogenolysis reaction. It is demonstrated that highly dispersed Rh particles are obtained by the supercritical CO2 treatment. In the hydrogenolysis reactions, the supercritical CO2-treated catalyst showed higher conversions and ethane formation.