For CO2/CH4 separation, a number of mixed matrix membranes (MMMs) were created using semi-fluorinated polyamide (PA) as the basis polymer and Ni-MOF-74 as a filler. Scanning electron microscopy (SEM) and Fourier transform infrared (FTIR) spectra were used to characterize MMMs. By measuring one, the behavior of gas separation was examined. Using a constant-volume variable pressure approach, the gas permeability of four distinct gases CH4, N2, O2, and CO2 was assessed for both pure and composite membranes. The optimal selectivity of several gas pairs was computed and contrasted with mixed matrix membranes that have been described. The MMMs combined with 20 weight percent Ni-MOF-74 (Ni-MOF-74/PA) had a CH4 permeability of 63 Barrer for the single gas, which was greater than that of Polyamide (PA), but its optimum selectivity stayed the same. When the temperature rises to 35 °C, CH4 permeability might further increase to 35 Barrer.