Microporous, hyper-crosslinked poly-p-phenylenes have been prepared by combination of superacid-catalyzed polymerization and then crosslinking with external crosslinkers, e.g. tetrachloromethane (CCl4) and dimethoxymethane (DMM). The porosity property can be tuned by changing the molecular weight of the linear poly-p-phenylenes. With the increase of linear polymer molecular weight, the surface areas increase fleetly and then decrease. The highest surface area is 1019 m(2)/g, for HCP-9-DMM. The effect of solvent amount on HCPs' surface area was also studied. Moreover, the CO2 storage capacity of these materials was tested, where HCP-9-DMM shows the highest CO2 adsorption capacity of 93 mg/g. (C) 2015 Published by Elsevier Ltd.