In the presence of 5 wt% of p-toluenesulfonic acid (TsOH), the mixture (TPA/PR = 1.5/1.0) of pyrene (PR) and terephthalaldehyde (TPA) was heated at 160 A degrees C for 1.5 h under nitrogen to give the condensed polynuclear aromatic (COPNA) resin. It was transformed to an infusible and insoluble solid by further heating at 300 A degrees C for 1 h. The obtained material was treated with sulfuric acid at 80 A degrees C for 15 h under nitrogen to give the sulfonated COPNA(PR,TPA) resin. The sulfonated COPNA(PR,BA/TPA) resin was prepared by heating the mixture of PR, benzaldehyde (BA), and a small amount of TPA in the presence of TsOH followed by the treatment with sulfuric acid. The sulfonated COPNA(PR,TPA) resin was reused without significant loss of activities, and exhibited the higher performance than conventional solid acids.