Two diallylamine salts, diallylammonium acetate (DAA acetate) and diallylguanidinium acetate (DAGA) were cyclocopolymerized in water with acrylonitrile (AN) using power ultrasound in order to prepare acrylonitrile copolymers involving thermally stable heterocyclic rings in their polymeric matrix. The structural characterization of the copolymers was performed using FTIR, $$^{13}$$ 13 C NMR, UV/Vis spectroscopy and elemental analysis. The results revealed that the diallyl amine salts cyclopolymerized to form pyrrolidine and not piperidine rings throughout the polymeric chains. The thermal behavior of the copolymers prepared under nitrogen atmosphere was investigated using thermogravimetry, differential thermal analysis (TGA/DTA) and differential scanning calorimetry. The morphological property was also discussed using scanning electron microscopy (ESEM). The results revealed that the thermal stability of the copolymers was improved by the increase in the content of N,N-diallylammonium and N,N-diallylguanidinium acetate. The power of ultrasonic waves enhanced the homogeneity of the copolymers blend films irrespective of the copolymer compositions.