Liquid-phase polymerisation of acrylamide-acrylic acid to form polyelectrolytes used in wastewater cleaning was examined using accelerated electron beam and microwave irradiation methods. Polymerisation was carried out in aqueous solutions at temperatures ∼60 °C. Monomers total concentration was established at 40% (36% acrylamide and 4% acrylic acid). Only using the features of simultaneous radiation–induction and microwave heating can result in the formation of linear polymer chains with good water solubility and low residual monomer concentration. The flocculation capacity of the obtained polymers was tested using two wastewaters, one sampled from a slaughterhouse and the other from a vegetable oil plant. Quality indicators such as total suspended matters (TSM), chemical oxygen demand (COD), biological oxygen demand (BOD) and fat, oils and grease (FOG) were measured before and after the treatment with polymeric flocculants and compared with the results obtained in classical treatment with Al 2(SO 4) 3. It was found that the combined treatment with polymers and Al 2(SO 4) 3 increases the degree of purification of both wastewaters up to 99%.