In this study, a series of 4-azo derivatives of 1,2,4-triazole were synthesized through the reaction of melt thiocarbohydrazide with various substituted benzoic acids. Subsequently, these derivatives were coupled with different aromatic amines to obtain 4-azo derivatives of 1,2,4-triazole. The synthesized derivatives were then converted into 4-azo-3,5-substituted-1,2,4-triazole polymers using dry acetonitrile, pyridine, and poly acryloyl chloride. The physical properties, FT-IR spectra, and 1H-NMR spectra (for selected compounds) were utilized to confirm the structures of the synthesized compounds and polymers. Furthermore, the antibacterial and anticorrosion activities of the compounds and polymers were investigated.