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The thermal rearrangement of polyimides of ortho‐positioned functional group membranes improves the gas permselectivity properties of the polyimide precursor. For this experiment, HAB‐6FDA polyimide was synthesized from 3,3 dihydroxy‐4,4‐diamino‐biphenyl (HAB) and 2,2‐bis‐(3,4‐dicarboxyphenyl) hexafluoropropane dianhydride (6FDA) by chemical imidization. A sample was modified from a pure polymer to silica nanoparticle composition. Furthermore, a modification was carried out by thermal rearrangement reaction at temperatures of 350, 400, and 450°C. The thermal property of these membrane films was characterized by differential scanning calorimetry (DSC), FTIR, opacity experiment, and free volume analysis. Permeability decreases with an increase in the kinetic diameter of gasses, which is normal behavior for glassy polymers. The composition of silica nanoparticles slightly changes the permeability in the polyimide. The combined effect of silica nanoparticles and thermal rearrangement of the HAB‐6FDA membrane has shown an excellent performance. The thermal rearrangement with nanocomposite shows a significant impact on a larger effect on permeation for lighter gases, that is, H2, CO2, and O2, compared with N2 and CH4. Particularly for H2/CH4 gas pair, it lies over Robeson's 2008 upper bound limit, which fits the composition in the novel class for the gas separation membranes.