Solution polymerization synthesized alt-resistant superabsorbent poly (acrylic acid-acrylamide/fly ash) composites. The mass ratio of acrylic acid (AA) to acrylamide (AM), the concentration of crosslinker, the neutralization degree (ND) of AA, and the polymerization temperature were investigated by single-factor method. Optimized conditions for the synthesis of poly (acrylic acid-acrylamide/fly ash) (PAA-AM/FA) are, as following: m (AA)/m (AM) is 1.5, the content of crosslinker N, N-methylenebisacrylamide. (MBA) is 0.7%, neutralization degree of AA is 70%, polymerization temperature is 70 °C, and fly ash (FA) content is 50%. The prepared PAA-AM/FA demonstrated superior water absorption performance. The absorption capacities of PAA-AM/FA for pure water and 0.9% NaCl solution were found to be 976 g·g−1 and 81 g·g−1, respectively. Furthermore, PAA-AM/FA was found to have excellent adsorption capacity (148 mg·g−1) for Rhodamine B in water. Fourier Transform-Infrared Spectroscopy (FT-IR), Thermogravimetric Analysis (TGA), and Scanning Electron Microscopy (SEM) characterized the prepared materials. Results showed that fly ash was incorporated into the macromolecular polymer matrix and played a key role in improving the performance of the polymer composites.