In this work, the absorption-hydration hybrid method was used to recover (hydrogen + nitrogen) from (hydrogen + nitrogen + methane + argon) tail gas mixtures of synthetic ammonia plant through hydrate formation/dissociation. A high-pressure reactor with magnetic stirrer was used to study the separation efficiency. The influences of the concentration of anti-agglomerant, temperature, pressure, initial gas-liquid volume ratio, and oil-water volume ratio on the separation efficiency were systematically investigated in the presence of tetrahydrofuran (THF). Anti-agglomerant was used to disperse hydrate particles into the condensate phase for water-in-oil emulsion system. Since nitrogen is the material for ammonia production, the objective production in our separation process is (hydrogen + nitrogen). Our experimental results show that by adopting appropriate operating conditions, high concentration of (hydrogen + nitrogen) can be obtained using the proposed technology based on forming hydrate.