This study investigates the thermal insulation performance of a hybrid nanocomposite material composed of synergistically blended nanosilica, graphene oxide, and expanded perlite within a polymeric matrix. The experimental analysis focuses on thermal conductivity, heat resistance, and structural integrity under varying thermal loads. The composite samples were fabricated using solution casting and hot-press techniques, and their properties were evaluated through thermogravimetric analysis (TGA), differential scanning calorimetry (DSC), and guarded hot plate methods. Results demonstrate a significant reduction in thermal conductivity and enhanced thermal stability, indicating the composite's suitability for energy-efficient insulation systems in industrial and residential applications. The hybrid nanocomposite exhibited improved dispersion of nanoparticles and interfacial bonding, which contributed to its superior performance. This research highlights the potential of nano-engineered composites in advancing the design of high-performance thermal insulation materials.