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In this study, a novel mixed‐matrix membrane (MMM) based on covalent incorporation of poly(styrene‐alt‐maleic anhydride) (PSMA) with a metal‐organic framework (MOF) UiO‐66‐NH2 was prepared and utilized for dye removal from aqueous solution. The fabrication of PSMA and UiO‐66‐NH2 was carried out by the amidation reaction between the maleic anhydride ring and amino functional group affording crosslinked MOF/PSMA membrane. The separate UiO‐66‐NH2 and PSMA solutions were mixed before cast films were produced. The MMM was prepared with final UiO‐66‐NH2 wt % content from 0 to 30 % in each membrane. The formation of MMM was confirmed with FT‐IR, PXRD, TGA, SEM, and XPS analysis. The MMM having high adsorption capacity was used for the separation of methylene blue (MB) and methyl orange (MO) as organic dye pollutants commonly found in wastewater. The MMM could be recycled and still maintained 75 and 52 % retention of MB and MO on the third reuse cycle, respectively. The results suggest that the MOF incorporated PSMA was an outstanding membrane for the development of filtration techniques for decontamination of water resources. [ABSTRACT FROM AUTHOR]