AbstractPoly(2‐methyl‐ or 2‐phenyl‐s‐triazinylenehydrazones) were prepared both by dehyhydration of dihydrazino‐s‐triazines with terephthalaldehyde and by dehydrochlorination of dichloro‐s‐triazines with terephthalaldehyde dihydrazone. The structure of the polymers was confirmed by infrared spectrometry and elemental analyses in comparison with those of a model compound. Dehydration yielded soluble polymers, while the dehydrochlorination yielded insoluble polymers. Most of the polymers degraded at about 350°C, and the polymers of higher molecular weight showed better thermal stability. The thermal behavior of the polymers indicated that the phenyl‐substituted polymers obtained by dehydrochlorination and the methyl‐substituted polymers obtained by dehydration had a degree of polymerization similar to that of the phenyl‐substituted polymers obtained by dehydration. The soluble polymers could form chelate polymers, these took two accelerated decomposition phases. The lower phase suggested a decomposition accelerated by a metal. The higher phase, in which the chelate polymers decomposed more rapidly at a higher temperature (above 400°C) than their ligand polymer, was related to the atomic number and the electro‐negativity of the metals. The formation of decomposition products, guanamines and nitrile compounds, in all cases indicate the preferential scission
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