A new family of dialkylaryl disulfonate Gemini-type anionic surfactant were synthesized based on the reaction of olefin sulfonic acid (C 14 AOS acid) with different aromatics. New synthesis route do not require the conventional alkylation unit and strong acid catalysts, and the resulting Gemini-type anionic surfactant differ from existing products by having the sulfonyl group attached to the alkyl chain rather than the aromatic ring. To optimizing reaction condition, a reliable double-wavelength spectrophotometric method and iodine value method were employed for measurement the conversion of the aromatics. The experimental has confirmed that the reaction time and temperature are mainly the factors of the effect of conversion. Under 150°C, C 14 AOS acid reacts with different aromatics for 4 or 5 hours to form dialkyaryl disulfonic acid, and dialkyaryl disulfonic acid was then neutralized to dialkyaryl disulfonate Gemini-type anionic surfactant. Some surface active property has been investigated too. The critical micelle concentration of ditetradecylbenzene disulfonate, ditetradecylnaphthalene disulfonate, ditetradecylmethylnaphthalene disulfonate, ditetradecylphenanthrene disulfonate, ditetradecyldiphenylether sulfonate, ditetradecyldiphenylmethane sulfonate and ditetradecylbenzophenone sulfonate were 1.7 × 10 −4 , 8.082 × 10 −6 , 2 × 10 −5 , 2.158 × 10 −3 , 5.0 × 10 −6 , 1.0 × 10 −5 and 1.33 × 10 −5 mol l −1 . Above datum showed the aromatics of the surfactant may effect on surface active property obviously. Among these, some dialkylaryl disulfonate gemini anionic surfactant have very higher surface active than conventional dodecylbenzene sulfonate and may be widely used in industry and household.