A high internal phase emulsion (HIPE) method was used to produce adsorbents with an interconnected porous structure. HIPE was prepared using vinyl benzyl chloride (VBC), divinylbenzene (DVB), tert -butyl acrylate, and Span80 as the organic phase and water with K 2 S 2 O 8 and CaCl 2 as the water phase. The polymerization of the organic phase produced highly porous polymers called polyHIPE, carrying two functional groups. As a result of the template method, polyHIPEs have a low surface area. To overcome this drawback, polyHIPE was hyper-cross-linked through VBC to create meso- and micropores, resulting in a higher surface area. Then the polymer surface was tailored with carboxylic acid groups by simple hydrolysis of tert -butyl acrylate. The adsorption performances of the acidic functional hyper-cross-linked polyHIPEs prepared for the various reaction times of 0, 15, and 60 min were compared for methylene blue. The hyper-cross-linked polyHIPEs showed an enhanced adsorption kinetics for methylene blue, and the 15 min hyper-cross-linking reaction increased the rate of methylene blue adsorption significantly. It was proven that the polyHIPE adsorbent can be reused by treating it with an aqueous acidic solution in ethanol.

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