In order to quickly and effectively control the fire zone formed by natural fire in underground coal mines, the fire area of Xinfa Mine 525 coal mining face was treated with simple process, flexible and easy to operate liquid carbon dioxide technology. A total of 209 t of liquid carbon dioxide was injected, and the fire zone was well controlled. The concentration of carbon monoxide, oxygen concentration and ethylene in the fire zone decreased significantly, and the extinguishment conditions of the fire zone were not repeated for more than 30 d, indicating that the fire zone extinguished. It showed that the perfusion liquid carbon dioxide technology with broad application prospects in the fire area control in this area, especially it was better cooling, inerting, dilution and anti-explosion effects, with obvious fire extinguishing advantages.