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Nanofiltration (NF) membrane is of great significance for desalination of light brine and purification of drinking water. Although the development of novel preparation methods and membrane materials has improved the separation performance, it is still a major challenge to promote NF membrane toward industrial production with simpler and more controllable process. Herein, the polyphenol intermediate layer was designed by 5,5′,6,6′-tetrahydroxy-3,3,3′,3′-tetramethyl-1,1′-spirobisindane (TTSBI) with twist structure and polyethyleneimine (PEI) co-deposition to increase the surface hydrophilicity and electropositivity of the polysulfone ultrafiltration substrate. Subsequently interfacial polymerization (IP) was carried out on the polyphenol intermediate layer to assemble a polyamide ultrathin selective layer using trimesoyl chloride and piperazine monomer. Through adjusting the co-deposition time of TTSB and PEI, a unique nano-pleated structure was successfully formed on the thin-film composite membrane surface. The water permeance of the membrane was determined as 23.7 L m−2 h−1 bar−1 with 99.4% Na 2 SO 4 rejection, which was almost triple fold of the flux of the controller membrane without the intermediate layer. Our results provide an efficient and convenient way to fabricate the advanced NF membrane with higher divalent/monovalent ion selectivity and water permeance simultaneously, which will provide advices for the gas separation and pervaporation membranes with the IP method. • Novel TTSBI-PEI interlayer-based polyamide membrane was fabricated by interfacial polymerization. • The nano-pleated structure on the selective layer improved the water flux without deterioration of Na 2 SO 4 rejection. • The novel nanofiltration membrane exhibited excellent long-term stability. [ABSTRACT FROM AUTHOR]