Dimercapto-1,3,4-thiadiazole was prepared by using triethylamine as catalyst.Compared with the traditional synthesis techniques,using triethlamine as catalyst,the reaction yield can be raised from 82.50% to 90.01%. The catalytic mechanism was studied and the optimal reaction conditions were investigated by the experiments. The optimum material ratio of n(hydrazine hydrate):n(carbon disulfide):n(KOH) is 1.0∶3.5∶2.0, suitable reaction temperature is 80℃, and triethylamine 40?mg is required. The construction of the product was analyzed by infrared spectrum, and nitrogen content and melting point of the product was measured, the results were accorded with the theoretical value. The results show that the claimed route of synthesizing 2,5-dimercapto-1,3,4-thiadiazole is viable, and the method of synthesis is of practical use.