Three novel surfactants, p-(n-alkyl)-benzyl Polyoxyethylene ether Carboxybetaine ,were synthesized from fatty acid ,benzene and Triethylene Glycol through Friedel-Crafts acylation, Huang-Minlon reduction, chloromethylation, Williamson reaction, halogenation and quaterisation reaction. The structures of the products were characterized by IR, 1HNMR and ESI-MS methods. The critical micelle concentration (CMC) and the surface tension at the CMC (γCMC) of the surfactants in aqueous solution at 30℃ were measured by means of the Wilhelmy-plate method. The results showed that the values of CMC (mol/L) reached to the order of magnitude of 10–4~10-6 and the values of γCMC were 27-30mN/m. The CMC (respectively 1.12×10-4、1.51×10-5、6.21×10-6 mol/L) was observed to decrease, as the change of carbon atom number (n=8,10,12) of the substituted hydrophobic chain of benzene ring, however, γCMC(respectively 27.9，28.4，29.9 mN/m) increased as the number of carbon atoms increases. The experiment results showed that these surfactants have high surface activities.