Thermal behaviors, compositions and structures of silver laurate prepared in wateralcohol system with double jet method has been investigated via DSC, FTIR, XRD and SEM, respectively. Silver nitrate, sodium hydroxide and lauric acid were used as reactants and PVP as protective agent. Results show that the highly ordered layer structures of as prepared samples were weakened at 173oC and 212oC and then decomposed at 238oC. The morphology changed from fiber-like to lamellar when the silver laurate was calcined at 212oC.