Graphene oxide - molybdenum disulfide hybrid membranes were prepared using vacuum filtration technique. The thickness and the MoS2 content in the membranes were varied and their H-2 permeance and H-2/CO2 selectivity are reported. A 60 nm hybrid membrane containing similar to 75% by weight of MoS2 exhibited the highest H-2 permeance of 804 x 10(-9) mol/m(2) s Pa with corresponding H-2/CO2 selectivity of 26.7; while a 150 nm hybrid membrane with similar to 29% MoS2 showed the highest H-2/CO2 selectivity of 44.2 with corresponding H-2 permeance of 287 x 10(-9) mol/m(2) s Pa. The hybrid membranes exhibited much higher H-2 permeance compared to graphene oxide membranes and higher selectivity compared to MoS2 membranes, which fully demonstrated the synergistic effect of both nanomaterials. The membranes also displayed excellent operational long-term stability.