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Commercial acrylic fiber samples were first pretreated with hydrazine under various concentrations to give crosslinked structure. Then, the crosslinked fiber samples with different degree of crosslinking were treated with hydroxylamine hydrochloride to develop ion‐exchange fibers. These fibers contain amidoxime, amine, amide, and hydrazide groups simultaneously. The effects of reaction conditions on physical properties, thermal characteristics, surface morphology, ion adsorption quantity, and reusability were investigated. The results show that by increasing the reaction time, temperature, and concentration of hydroxylamine hydrochloride, the content of amidoxime groups in all samples were increased, but with noncrosslinked fibers noticeable drop in the mechanical properties were observed, while in crosslinked sample prepared under optimum conditions of reaction, good ion adsorption capacity with keeping …