Metal-organic frameworks (MOFs) received considerable attention to adsorption and removal of various environmental pollutants because of some inherent advantages. However, it is challenging but meaningful to design and fabricate hierarchical mixed-dimensional MOFs with synergistic effects to enhance the performance for removal and preconcentration of environmental pollutants. Herein, a new hierarchical two-dimensional (2D)-three-dimensional (3D) mixed-dimensional cactus‐like MOF@MOF hybrid material (PCN-134@Zr-BTB) was prepared by in-situ growth of 2D MOF nanosheets (Zr-BTB) on the surface of 3D MOF (PCN-134). The PCN-134@Zr-BTB composites combine the advantages of 2D and 3D MOFs with extensive mesoporous structures and large surface area for effective removal and enrichment of bisphenols (BPs). In comparison with pristine PCN-134 and Zr-BTB materials, the PCN-134@Zr-BTB hybrid material presented excellent adsorption performance for BPs. The adsorption isotherms are consistent with the Langmuir model, and the maximum adsorption capacity of four bisphenols (BPs) ranged from 135.1 mg/g to 628.9 mg/g. The adsorption kinetics are in accordance with the pseudo-second-order model. The recoveries ranged from 72.8% to 108%. The limits of detection were calculated at 0.02–0.03 ng/mL. The enrichment factors were calculated in the range of 310–374. According to FT-IR and XPS analysis, the main adsorption mechanisms are hydrogen bonding and π-π stacking. Nevertheless, this work provides a new and convenient strategy for the preparation of new hierarchical mixed-dimensional MOF@MOF (PCN-134@Zr-BTB) hybrid material for extraction and enrichment of BPs from aqueous matrix.

金属有机框架（MOF）由于一些固有的优势，在吸附和去除各种环境污染物方面受到了广泛的关注。然而，设计和制造具有协同效应的分层混合维MOFs以提高环境污染物的去除和预富集性能具有挑战性但有意义。在此，通过原位生长2D MOF纳米片制备了一种新的分层二维（2D）-三维（3D）混合维仙人掌状MOF@MOF杂化材料（PCN-134@Zr-BTB）（ Zr-BTB）位于 3D MOF (PCN-134) 表面。PCN-134@Zr-BTB复合材料结合了2D和3D MOF的优点，具有广泛的介孔结构和大表面积，可有效去除和富集双酚（BP）。与原始PCN-134和Zr-BTB材料相比，PCN-134@Zr-BTB杂化材料对BPs表现出优异的吸附性能。吸附等温线与Langmuir模型一致，四种双酚(BPs)的最大吸附容量范围为135.1 mg/g至628.9 mg/g。吸附动力学符合准二级模型。回收率为 72.8% 至 108%。检测限计算为 0.02–0.03 ng/mL。富集因子的计算范围为 310-374。根据FT-IR和XPS分析，主要吸附机制为氢键和π-π堆叠。尽管如此，这项工作为制备新型分层混合维 MOF@MOF (PCN-134@Zr-BTB) 杂化材料提供了一种新的、便捷的策略，用于从水基体中提取和富集 BP。