SynopsisPoly-1,2,4-triazoles containing arylene sulfone ether linkages have been synthesized by the reaction of polyhydrazide precursors and aniline in polyphosphoric acid at 260°C. The polyhydrazide intermediates were prepared from arylene sulfone ether containing dihydrazides and aromatic diacidchlorides via solution and interfacial polycondensation. These polymers and their intermediates were characterized by infrared, solubility, solution viscosity, elemental analysis, thermogravimetric analysis, differential scanning calorimetry, and X-ray diffraction.