Lack of clean water is a major global challenge. Membrane separation technology is an ideal choice for the treatment of industrial, domestic sewage owing to its low energy consumption and cost. However, membranes are highly susceptible to contamination, particularly during wastewater treatment, which has limited their practical applications in this field. Similarly, the flux of the membrane decreases with prolonged use due to its reduced interlayer spacing. Preparation of membranes with anticontamination properties and stable flux is the key to addressing this problem. In this study, a 2D heterostructure membrane with visible‐light‐driven self‐cleaning performance is prepared via a self‐assembly process. Notably, the addition of palygorskite increases the interlayer spacing of the graphene and heterojunction structures, which increases the flux of the membrane and avoids a decrease of the interlayer spacing of the membrane under pressure. The presence of a heterojunction with visible light catalytic properties effectively avoids membrane fouling and avoids a sharp decrease of the permeation flux. Importantly, the prepared 2D membrane has excellent separation performance for oil–water emulsions with both high flux and efficiency. These features suggest great potential for the prepared 2D membrane in wastewater treatment applications.

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The introduction of porous nanofillers into the polyamide selective layer of thin-film composite membranes is a promising strategy towards improved water flux and salt rejection for reverse osmosis membranes. However, the incorporation of filler particles is constrained by the poor compatibility between particle fillers and a polyamide layer. In this study, we report the rationally chosen zirconium metal–organic cages (Zr-MOCs) with ideal stability, solubility, and porosity characteristics as molecular fillers for thin-film nanocomposite (TFN) membranes. In addition, we use monoamino compounds to fine-tune the structure of the polyamide selective layer and the performance of the TFN membranes following the “defective ligand” strategy. The optimized TFN membranes exhibit up to a fourfold increment in water flux without compromising the salt rejection, underlining the promising potential of Zr-MOCs as molecular fillers in TFN membranes.