4-(1-Naphthyl)-1,2,4-triazolidine-3,5-dione was prepared from 4-naphthyl isocyanate. This compound was reacted with excess acetyl chloride in N,N -dimethylacetamide (DMAc) solution and gave 1,2-bisacetyl-[4-(1-naphthyl)]-1,2,4-triazolidine-3,5-dione as a model compound. Solution polycondensation reactions of monomer with succinyl chloride, suberoyl chloride and sebacoyl chloride were performed under conventional solution polymerization techniques in the presence of different catalysts such as pyridine (Py) and triethylamine (TEA) in DMAc and N -methylpyrrolidone (NMP) and led to the formation of novel aliphatic polyamides. These novel polyamides have inherent viscosities in a range of 0.04-0.46 dL/g -1 in N,N -dimethylformamide (DMF) at 25 o C. The reaction of This compound with n -isopropylisocyanate was performed at room temperature in DMAc solution, and the resulting bis-urea derivative was obtained in high yield and was finally used as a model for polymerization reaction. The step-growth polymerization reactions of monomer with hexamethylene diisocyanate (HMDI), isophorone diisocyanate (IPDI) and toluene-2,4-diisocyanate (TDI) were performed in DMAc solution in the presence of pyridine or TEA or dibutyltin dilurate (DBTDL) as catalysts. Some physical properties and structural characterization of these novel polyureas are reported. Fluorimetric studies of the model compound as well as polymers were done. The resulted polymers were characterized by FTIR, 1 H-NMR, UV and TGA analyses. The flurescence excitation and emission spectra of the monomer and polymers were also studied.