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A zinc-based Metal-Organic Framework (MOF) has been prepared by utilizing adipic acid as an aliphatic ditopic linker via both solvothermal and sonochemical methods. The ultrasound irradiation has reduced the reaction time and has led to smaller particle size. The samples were evaluated for their catalytic efficiency by the electrochemical reduction of CO₂, with carbon monoxide and hydrogen being the sole products. At lower potentials (−1.5 V to −1.7 V) the ultrasound sample achieved up to 10% better faradaic efficiency towards CO (FE_CO). At more negative potentials (−1.8 V to −1.9 V) the FE_CO of the two samples start to equalize to a maximum of around 58%. The proposed work contributes to circular economy and the results may be useful for further investigation of the opportunities created by the usage of MOFs in the framework of energy recovery and efficiency, waste reduction, responsible consumption of …