Abstract: In order to improve the hydration separation effect of high concentration CH₄ gas, the separation experiment of high concentration CH₄ gas hydrate under the influence of spray nozzle angle was carried out by using the gas rapid hydrating spray experiment device. The influence of nozzle angle on recovery and separation factor of CH₄ was discussed by combining gas hydration with the end gas-solid chromatography. The results show that: CH₄ gas samples with concentration of 60% and nozzle angles of 30°, 45°, 60°, 90° corresponding CH₄ recovery rates are 20.69%, 24.23%, 16.83% and 15.39%, respectively, and the separation factors are 1.69, 1.89, 1.55, 1.49; CH₄ gas samples with concentration of 70% and nozzle angles of 30°, 45°, 60° 90° corresponding recovery rates of CH₄ are 22.44%, 25.27%, 19.63% and 17.87%, respectively, the separation factors are 1.67,1.83, 1.52, 1.4; CH₄ gas samples with concentration of 80% and nozzle angles of 30°, 45°, 60° and 90° corresponding recovery rates of CH₄ are 22.36%, 24.51%, 18.81% and 16.14%, respectively, and the separation factors were 1.90, 1.95, 1.76, 1.75. The three kinds of CH₄ gas recovery and separation factors increase first and then decrease with the increase of the nozzles angle, and the influence sequence is 45°> 30°> 60°> 90°.