Eco-friendly urethane-based non-F-containing water repellent agents in order to replace F-containing water repellent agents are attracting a lot of interest and many researches have been developed recently. In previous our studies, superhydrophobic type and improved durability type. On our continuing research on synthesis of 3D-water repellent meterial. An Urethane-based non-F-containing water repellent agent having two PEG moiety was prepared to test fish-toxicity. In order to improve emulsifying property were also prepared two water repellent agents using new STO-OH, STS-OH derivatives containing Tween-85 and Tween-65 in NEP in the presence in Ti catalyst.