Three Schiff bases of 3-amino-5-mercapto-1,2,4-trizaole have been synthesized:5-benzylideneamino-4H-1,2,4-trizaole-3-thiol(Ia),5-(3-phenylallylideneamino)-4H-1,2,4-triazole-3-thiol(Ib),5-((5-mercapto-4H-1,2,4-triazol-3-ylimino)methyl)quinolin-8-ol(Ic).These compounds are characterized by UV-Vis,FT-IR,HPLC,1H-NMR and elementary analysis.The fluorescence spectra of compounds is investigated.We obtained different fluorescence spectra and compared the fluorescence of raw materials to products.Results show that the fluorescence is changed correspondingly when introduce the conjugated group.