A range of conjugated microporous polymer networks has been prepared using Sonogashira−Hagihara cross-coupling of 1,3,5-triethynylbenzene with a number of functionalized dibromobenzenes. Porous poly(arylene ethynylene) networks with surface areas up to 900 m2/g were produced. The surface chemistry of the networks was varied by monomer selection, thus allowing control over physical properties such as hydrophobicity. Additionally, it was shown that the dye sorption behavior of the networks can be controlled by varying the hydrophobicity. This expands significantly on the utility of this approach, allowing high surface area networks to be prepared with properties that can be tailored for applications such as catalysis and separations.