A new and simple method was developed for fabricating palladium nanoparticles (PdNPs) captured in a mesoporous monolith based on thermally induced phase separation (TIPS) method. XRD result confirmed the formation of PdNPs inside the monolith. TEM image showed that most of the captured PdNPs were in the diameter range from 5 nm to 10 nm. The monolith had relatively high specific surface area and uniform mesopore structure. To measure its catalytic efficiency, the crosslinked monolith was applied to a heterogeneous Suzuki-Miyaura reaction of aryl halide and aryl boronic acid in a water/ethanol mixture. The monolith exhibited both high catalytic performance and excellent stability for repeated use. (C) 2015 Elsevier Inc. All rights reserved.