This study presents a hierarchical carbon nanosheet array electrode with a single-atom Ni catalyst synthesized from organic molecule-intercalated layered double hydroxides. The electrode exhibits superior 2e⁻ ORR performance under alkaline conditions, achieving high H₂O₂ yield rates of 0.73 mol g_cat⁻¹ h⁻¹ in the H-cell and 5.48 mol g_cat⁻¹ h⁻¹ in the flow cell. The Ni atoms selectively adsorb O₂, while carbon nanosheets generate reactive hydrogen species, synergistically enhancing H₂O₂ production. The coupling of the 2e⁻ ORR with ethylene glycol oxidation further increases the H₂O₂ yield rate to 7.30 mol g_cat⁻¹ h⁻¹ while producing valuable glycolic acid. Additionally, the alkaline electrolyte containing H₂O₂ can be directly converted into sodium perborate, reducing separation costs. Techno-economic analysis validates the economic viability of this system, demonstrating its potential for industrial application.This study presents a hierarchical carbon nanosheet array electrode with a single-atom Ni catalyst synthesized from organic molecule-intercalated layered double hydroxides. The electrode exhibits superior 2e⁻ ORR performance under alkaline conditions, achieving high H₂O₂ yield rates of 0.73 mol g_cat⁻¹ h⁻¹ in the H-cell and 5.48 mol g_cat⁻¹ h⁻¹ in the flow cell. The Ni atoms selectively adsorb O₂, while carbon nanosheets generate reactive hydrogen species, synergistically enhancing H₂O₂ production. The coupling of the 2e⁻ ORR with ethylene glycol oxidation further increases the H₂O₂ yield rate to 7.30 mol g_cat⁻¹ h⁻¹ while producing valuable glycolic acid. Additionally, the alkaline electrolyte containing H₂O₂ can be directly converted into sodium perborate, reducing separation costs. Techno-economic analysis validates the economic viability of this system, demonstrating its potential for industrial application.