This paper is an experimental study on the freezing protection valve used for solar water heating, air-conditioning systems, and plumbing systems. When the phase change occurs from liquid to solid, most of the substances except water volumetrically shrink. And referred to as PCM(Phase Change Material) a substance with such properties, the phase change temperature varies depending on the material. To prevent the freezing of the plumbing system, such as air-conditioning system in the winter season, we developed a several types of freezing protection valve using PCM whose freezing temperature are $2-4^{circ}C$. The working principle of the freezing protection valve is that the fluid inside the pipe is released to prevent the system-collapse when fluid temperature reaches the freezing temperature of the PCM. And then the valve is closed and returned to the original position automatically when the temperature of the operating fluid rises. In this paper, the operating temperatures, discharge flow rate and the response characteristics of the valve during the operation are tested and investigated. From the results of this research the freezing protection valves employing PCM are expected to be commercialized in the near future.