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A series of cost‐effective hyper‐cross‐linked polymers (HCLPs) are synthesized from naphthalene via the external cross‐linker (ECL) knitting method, the solvent knitting method, and the Scholl coupling reaction, respectively. According to multiple characterizations, the resulting polymers are thermally stable and fluorescent with large specific surface areas (SSAs) and narrow pore distributions. In particular the HCLP synthesized using dimethoxymethane as the ECL exhibits SSAs up to 2870 m2 g−1 and shows a great potential in gas adsorption applications. Naphthol and 1‐methylnaphthalene are used as monomers to synthesize HCLPs by the above three methods to investigate whether introducing functional groups to naphthalene would improve properties of the resulting polymers. Moreover, HCLPs feature high SSAs, outstanding thermal and fluorescent performances, and facile synthesis, making them promising candidates for industrial applications.

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The increasing threat of chloride ions (Cl−) has led researchers to explore efficient removal technologies. Sewage treatment with a double-layer hydroxide/oxide (LDH/LDO) is receiving increasing attention. In this work, Mg-Al LDO adsorbents were produced by the calcination of the Mg-Al LDH precursor, which was constituted by improved coprecipitation. The influence of calcination temperature, calcination time, adsorbent dosage, Cl− initial concentration, contact time, and adsorption temperature on Cl− elimination was investigated systematically. The experimental results showed that a better porous structure endowed the Mg-Al LDO with outstanding adsorption properties for Cl−. The adsorption process was well matched to the pseudo-second-order kinetics model and the Freundlich model. Under optimal conditions, more than 97% of the Cl− could be eliminated. Moreover, the removal efficiency was greater than 90% even after 11 adsorption–desorption cycles. It was found that the electrostatic interaction between Cl− and the positively charged Mg-Al LDO laminate, coupled with the reconstruction of the layer structure, was what dominated the Cl− removal process.