Abstract: The modification and optimization of porous carbon electrodes is key to achieving high-performance supercapacitors. Oxygen-rich porous carbon nanosheets (OPCNs) with a two-dimensional (2D) structure produced from the solid by-products of the coal industry were prepared by taking advantage of the rigid confinement of 2D MgAl-layered double hydroxides (MgAl-LDH) combined with KOH activation. The influence of carbonization temperature on the microstructure and surface properties of the OPCNs was investigated. The surface morphologies/compositions and surface textures of the prepared OPCNs were observed and analyzed by SEM, TEM, N₂ adsorption and desorption, elemental analysis, etc. The optimized carbon sample activated at 700 °C (OPCN-700) had a high oxygen content of 24.4 wt%, a large specific surface area of 2 388 m² g⁻¹, and good wettability. In addition, the abundant micropores and 2D nanosheet structure of OPCN-700 provide efficient storage and transport for electrolyte ions. Because of this, when used as the electrode for a supercapacitor it has a high specific capacitance of 382 F g⁻¹ at 0.5 A g⁻¹, an excellent rate performance and cycling stability.