In the present study, efficiency of electro-coagulation-flotation (EC-F) process using waste metal scrap of Al and Fe collected from construction and demolition waste of Indian Institute of Technology Madras (IIT M) campus for the removal of double azo bond dye Acid Red 66 (AR66) was studied. The key operating parameters such as current density and electrical conductivity were optimized individually with an initial dye concentration of 50 mg/L, at pH 7. Different electrode combinations and connection modes (parallel MP-P, series (MP-S, BP-S)) were tested, at pre-optimized conditions, in order to achieve better removal of AR66 dye with minimum energy consumption. Series connection in bipolar electrode mode (BP–S) showed better COD reduction from 164 mg/L to 26.2 mg/L with complete decolourization (BDL). Hybrid electrode system of Fe–Al–Fe–Al–Fe–Al showed maximum reduction of COD from 164 mg/L to 11.3 mg/L along with 86.3% TSS reduction and complete decolourization. LC-MS analysis showed the formation of intermediates with m/z 195, m/z 210.6 and m/z 159.3 due to the destruction of AR66 dye during electrolysis. Highest current efficiency (CE φ = 107%) was observed in case of hybrid electrode system compared to Al (φ = 30.1%) and Fe (φ = 98.3%) electrode system at similar operating conditions. Compared to the same electrode material as anode and cathode, use of appropriate hybrid electrode combination can improve the removal efficiency and reduce the energy consumption (ENC). The influence of aeration on the performance of the system was also studied. Aeration significantly improved the COD removal efficiency (98.3%) along with complete decolourization (100%). The use of waste metal scrap as electrodes reduced the overall cost of the treatment process from 1.6 $/m3 to 0.06 $/m3. Using waste metal scrap as electrodes not only reduces the metal accumulation in the environment but also reduces the cost of EC-F process. © 2020 Elsevier Ltd