Organic–inorganic hybrids were successfully synthesized by a simple ion self-assembly (ISA) method of H2[P2W18Ce3(H2O)2O71]10− (PWCe), and [Na(H2O)P5W30O110]14− (P5W30) polyoxometalates with p-Phenylenediamine (PPD). The nanohybrids and their products obtained by calcination (400 °C, 2 h) were characterized by FTIR, XRD, SEM/ EDS, DTGA and BET analysis. The catalytic efficiency of organic–inorganic nanohybrids were examined in degradation of some synthetic pollutants. The results showed that the PWCe based nanohybrids have very much efficiency toward degradation of synthetic pollutants compared of P5W30 based nanohybrids. Of these, the results confirmed that snowball PWCe nanocompposite obtained by calcination show even more efficiency. It was unveiled that snowball PWCe nanocomposite exhibited an outstanding catalytic activity higher than 90.0% MB, RhB, CR, EBT and 75.0% TC degradation efficiency within 12−40 min. Further investigations revealed that, the structure of the polyoxometalates, PWCe and P5W30 have changed due to calcination and tissue quality of nanohybrids has improved.
