Multivariate metal-organic frameworks (MTV-MOFs) are expected as catalyst to apply to the advanced oxidation processes (AOPs) based on sulfate radical (SO4·−) to treat wastewater containing organic pollutants. Mixing metals de novo method was combined with stringent solvothermal conditions to synthesize macaroon-like NbCo-MOF catalyst. NbCo-MOF catalyst prepared with different atom ratios and growth time presented various morphology, structure, performance, and distinctive MTV-MOFs growth law which were confirmed by SEM, TEM, EDS, XRD, FTIR, ...