The symmetrical urea substituted by Quinoline ring was synthesized by the reaction of 6-aminoQuinoline with triphosgene in the presence of triethylamine in 88% yield. This symmetrical urea reacted respectively with three type of bromoalkanes to produce three of bis-Quinolineaternary ammonium bromides a novel Gemini surfactants with Quinoline ring in 74% yield, which structure was confirmed by FT-IR, 1H NMR, 13CNMR and ESI-MS. The optimum reaction conditions for the symmetrical urea are as follows: methylene chloride as reaction solvent; mole ratio of 6-aminoQuinoline and triphosgene, 5∶1, reaction time, 6 h. The optimum procedure for the synthesis of the Gemini surfactants are as follows: DMF as solvent, 110 ℃, 8 h, mole ratio of intermediate and bromoalkane, 1∶14. The interfacial tension of the Gemini surfactants were measured in the chloroform-water system. The results show that the diffusion of the Quinoline Gemini surfactants from the chloroform solution into the chloroform-water interface is controlled by pure diffusion adsorption.