Abstract: Four isomers of alklybenzenesulfonate salts，Gemini surfactents，were synthesized from dodecylbenzene，triethanolamine，dichloromethane，1,2-dichloroethane and sodium hydroxide through a three-step process，which involves Fried-Crafts reaction，sulfonation and neutralization. The structures of intermediates were characterized by FTIR and 1H NMR. The surface tension of dilute aqueous solution of the product was measured at 25℃ by drop-volume method，and then the critical micelle concentration(CMC) was determined. One of the Gemini surfactants was employed as emulsifier in emulsion polymerization. The results indicated that the γCMC decreases with increasing the carbon atoms in the side alkyl or the bridge chains. It was also found that the surface tension value of Gemini surfactent neutralized with triethanolamine is the lowest in all the alklybenzenesulfonate salts. With the increase of emulsifier concentration，the latex particle size reduces in average，the polymerization equilibrium is improved and the conversion is increased.