The industrialization of the world and the shift from non-renewable to the renewable energy is demanding advanced energy storage devices having high energy and power density. The conventional activated carbon can high power density based on fast adsorption/desorption of electrolyte however suffers from low energy density. In this work, we have synthesized hybrid composites of TiO₂/Carbon/MoS₂ (TCM) from MIL-125 (Ti) having TiO₂ nanoparticles and layered MoS₂ as a redox active agent and a 3D porous carbon structure for the adsorption of electrolyte. MIL-125 (Ti) which is basically a Ti-based MOF has been used to derive uniformly infused TiO₂ nanoparticles in spherical 3D carbon structure. The uniformly doping of TiO₂ in carbon structure will provide superior redox activity with minimum probability of aggregation of TiO₂ whereas the 3D porous structure of carbon can provide conductive pathways with adsorption sites for electrolyte. Further the TiO₂/Carbon structure has been integrated with 2D MoS₂ structure through ultrasonication mixing. The MoS₂ layers will provide the effective pathways for the electrolyte diffusion for the thick electrode system with extra benefit of redox activity, mechanical stability, and layer to inhibit the aggregation of TiO₂/carbon spherical structure. After various characterization, including XRD, Raman, FTIR, FESEM, and BET, the TCM has been applied for aqueous supercapacitor application using 1M H₂SO₄ as an electrolyte. The high performance of tri-composite (TCM) (100 F/g at 3 A/g) when compared to TiO₂/Carbon (50 F/g) and MoS₂ (40 F/g) can be attributed to the improved electrolyte diffusion, redox activity, and conductive pathways.