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Layered bimetallic oxide composite films (ZnCr-Zr-LBMO/PANCMA) were constructed with high photocatalytical performance and reusability and applied for highly efficient removal of tetracycline hydrochloride (TC) from real water samples. [Display omitted] • Novel Zr-doped layered bimetallic oxide (Zr-LBMO) composite film was prepared. • Zr-LBMO film can be highly useful in the photocatalytical degradation of tetracycline hydrochloride (TC). • Zr-LBMO film exhibited superior photocatalytical degradation performance and excellent reuse stability. • The degradation pathway and mechanism of TC were explored. To fabricate novel photocatalytic materials is critical to the removal of emerging pharmaceutical pollutants from water samples. However, the photocatalytic materials still face the challenges of degradation performance and reusability. Here, layered bimetallic oxide (LBMO) composites were constructed by using hydrothermal synthesis method of layered double hydroxides (LDH) as precursors, and the LBMO films were prepared by dispersing the LBMO composites in poly(acrylonitrile-co-maleic acid) (PANCMA) solution. The obtained LBMO/PANCMA films exhibited high removal efficiency and good reusability for tetracycline (TC) degradation. Under the optimal conditions, the removal rate of LBMO/PANCMA composite film (20 mg) for TC (20 μg/mL) was 99.34 % within 40 min of light exposure, and retain above 85 % of removal rate even after 10 consecutive uses. Moreover, the possible TC degradation pathways were deduced by analyzing the TC degradation intermediates with LC-MS method, and the toxicity evolution of the TC degradation products was appraised by using density functional theoretical (DFT) method. This study provides a simple and feasible synthesis strategy for membrane-based photocatalytical materials to remove environmental pollutions. [ABSTRACT FROM AUTHOR]