UiO-66-GO hybrids were obtained by hydrothermal synthesis of MOF UiO-66 on graphite oxide (GO). UiO-66-GO were used as fillers to prepare mixed matrix membranes (MMMs). Good filler-polymer interaction was achieved. MMMs were applied to the separation of H2/CH4 and CO2/CH4 mixtures at 35, 60 and 90 °C. The barrier effect of the GO and the microporosity of the MOF dominated the separation properties of the MMMs.