In this study, Cu3(BTC)2 and Ni1.5-Cu1.5(BTC)2 were synthesized in the presence of microwave irradiation. The morphology and the structure of the prepared MOFs were characterized by XRD, TEM, TGA, FTIR, Raman, and nitrogen adsorption/desorption methods. The adsorption activities of the samples towards the phenols from aqueous solutions were achieved including kinetic and equilibrium approaches with different nonlinear models for modeling. The experimental data clarified that the adsorption of phenols on Cu3(BTC)2 and Ni1.5Cu1.5(BTC)2 had been processed via a pore-filling mechanism. Thermodynamic parameters were also determined. Furthermore, a three levels-four factor half-factorial design was successfully employed for experimental design and analysis of the results through response surface methodology (RSM). The significance of the independent variables was tested and optimized by the analysis of variance (ANOVA) and t-test statistics. The optimum pH, adsorbent dose, and temperature were found to be 5.0, 1 g/l, and 30 °C, respectively, for both samples. Under these conditions, the predicted removal efficiency of 50 mg/l phenols was found to be 71.32% (35.65 mg/g) and 78.95% (39.47 mg/g), respectively. Display omitted •Cu3(BTC)2 and Ni1.5-Cu1.5(BTC)2 were synthesized and characterized.•The affinities of MOFs towards the phenols in the aqueous medium were evaluated.•NiCu MOF removed ∼79% of 50 mg/L phenols at the optimum experimental conditions.