Iron-based metal–organic frameworks (MOFs) have aroused extensive concern as prospective photocatalysts for antibiotic (e.g., tetracycline, TC) degradation. However, efficiencies of single and simple Fe-based MOFs still undergo restricted light absorption and weak charge separation. Assembly of different iron-based MOF building blocks into a hybrid MOF@MOF heterostructure reactor could be an encouraging strategy for the effective capture of antibiotics from the aqueous phase. This paper reports a new-style MIL-101(Fe)@MIL-100(Fe) photocatalyst, which was groundbreakingly constructed to realize a double win for boosting the performances of adsorption and photocatalysis. The optical response range, surface open sites, and charge separation efficiency of MIL-101(Fe)@MIL-100(Fe) can be regulated through accurate design and alteration. Attributed to the synergistic effects of double iron-based MOFs, MIL-101(Fe)@MIL-100(Fe) exhibits an excellent photocatalytic activity toward TC degradability compared to MIL-101(Fe) and MIL-100(Fe), which is even superior to those reported previously in the literature. Furthermore, the main active species of •O2 – and h+ were proved through trapping tests of the photocatalytic process. Additionally, MIL-101(Fe)@MIL-100(Fe) possesses remarkable stability, maintaining more than 90% initial photocatalytic activity after the fifth cycle. In brief, MIL-101(Fe)@MIL-100(Fe) was highly efficient for TC degradation. Our work offers a new strategy for visible-light photodegradation of TC by exploring the double Fe-based MOF composite.

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