Abstract: Preparation and surface activity of 2-methyl-2-[perfluoro-2-methyl-3-oxocaproyloxyl] ethoxycarbonyl ethylmethyldipolyethoxylsilicane (V) were investigated. 2-methyl-2-[perfluoro-2- methyl-3-oxocaproyloxyl] ethoxycarbonyl ethylmethyldichlorosilicane (III) was synthesized from 2-[perfluoro-2-methyl-3-oxocaproyloxyl] ethyl methacrylate （I）and methyldichlorosilicane (II) by hydrosilication in the presence of Karstedt catalyst. III reacted with polyglycol （IV）to give non-surfactant V which was characterized by FTIR and MS and its surface activities were investigated. The reaction conditions of hydrosilication were optimized. n (I ): n (II) = 1.2∶1, I and II reacted in THF at 50℃ in the presence of 0.5% Karstedt catalyst( calculated by quality of I ) for 28h to give III at conversatin 68.2 %. The critical micelle concentration (CMC) of aqueous solution of V was 0.52 g/L, surface tension of which at CMC (γcmc) was 22.8 mN/m. Glass surface treated by THF solution of V shows excellent hydrophobic and good oilphobic performances.