A series of cleavable aryl sulfonate anionic surfactants were synthesized from cyanuric chloride, aliphatic amine and H-acid mono sodium salt. Their structures were identified by 1H NMR, Infrared Spectrum (IR) and Elementary Analysis (EA). Their critical micelle concentrations (CMC) in aqueous solutions at 25 °C were determined by a steady-state fluorescence probe method and a surface-tension method. With the increasing length of the carbon chain, the value of their CMCs and surface tensions under CMC (γ CMC) initially decreased and then reached a minimum (respectively 2.63 × 10−5 mol L−1 and 28.29 mN m−1) when the carbon number was 10. The CMC and γ CMC then increased when the carbon number was increased to 12. The results showed that, compared with sodium dodecyl benzene sulfonate (SDBS), such kinds of surfactants have much lower surface adsorption amounts and greater molecular areas on the aqueous surface.