Conjugated nanoporous polymer colloids (CNPCs) consisting of covalently cross-linked poly(p-phenyleneethynylene) networks were synthesized by using the Sonogashira coupling reaction in a toluene-in-water miniemulsion. The synthesized CNPCs having a uniform particle size distribution exhibit high porosity with a specific surface area of 421 m 2 /g and a dual distribution of pore size in the micropore and mesopore ranges. They are amenable to postfunctionalization and enhancement of their dispersibility in solvents, and retain their native photoluminescence. The modified CNPCs allow for in situ incorporation of palladium nanocrystals to form the Pd@CNPC composite materials. The Pd@CNPCs are validated to have excellent catalytic activity, outstanding reusability, and exceptionally high TOF (44100 h −1 ) for the Suzuki−Miyaura coupling reaction.
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