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MoS2 nanostructures with different morphologies were synthesized using a simple in‐situ hydrothermal process by different surfactants like hexadecyl trimethyl ammonium bromide (CTAB) and polyvinyl pyrrolidone (PVP), and the effect of morphologies on the adsorption property for Cr(VI) were investigated. It can be found that flower‐like and spherical MoS2 nanostructures were synthesized and their morphologies largely effected the adsorption performance toward Cr(VI) ions. Flower‐like MoS2 exhibited the surface area of 41.9 m2 g−1 with fairly high adsorption capacity of 66.1 mg g−1 toward Cr(VI), fitting well to pseudo‐second order kinetic model and Langmuir isotherm model. Moreover, this as‐prepared nanostructured MoS2 also presented satisfying reusability for removal of Cr(VI) and were even suitable for the selective removal of Cr(VI) in the presence of NO3−. It may provide a potential route to enhance the adsorption property of MoS2 toward heavy metal ions through adjusting the morphology of the MoS2 sample, which would expand the applications of MoS2 in the field of treatment of the heavy metal wastewater. [ABSTRACT FROM AUTHOR]