Abstract: MoS2/γ－Al2O3 ceramic composite membrane is successfully synthesized by the sol-gel method based on the inorganic salt route. The aluminum hydrate sol derived from the inorganic salt Al(NO3)3, whose transparence and viscosity are 97% and 1.2 × 10-3 Pa. s, respectively, can be formed through adjusting the ratio of the peptizing agent H+ to Al3+ to 0.3. The aluminum hydrate gel at 110℃ is amorphous in structure and is heat-treated in air at 800℃ to form γ－Al2O3. The precursor derived from the mixture solution of ammonium molybdate, thioacetamide and a reducing agent, can be transformed into crystal MoS2 under reducing condition at 800℃. MoS2/γ－Al2O3 composite membrane is an organic whole and bps no gradation from MoS2 layer to γ－Al2O3 Iayer. The separation factor a H2/H2S through the MoS2/γ－Al2O3 composite membrane increase with rising temperature and a H2/H2S at 600℃ is 4.45 higher than the theoretical separation factor produced by the ideal Knudsen diffusion.