AbstractSelective and simultaneous separation of H2S and CO2 from CH4 was accomplished in a hollow‐fiber membrane contactor (HFMC). The absorption of both H2S and CO2 using an aqueous solution of methyldiethanolamine (MDEA) was almost complete and acid gases were totally removed. Despite the large difference between H2S and CO2 concentrations, the rate of H2S absorption was not significantly influenced by CO2 absorption. The independent effect and interactions of several process variables on the separation performance of H2S and CO2 were investigated. The results indicated that the membrane contactor could be a highly efficient choice for removal of almost all H2S in the presence of a large CO2 content even at high gas/liquid flow ratio. The selectivity of H2S was about three times higher compared to the conventional absorption packed towers.