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Uniform hierarchical MoS 2 microspheres have been successfully synthesized via facile hydrothermal method with the aid of nonionic surfactant polyethylene glycol (PEG). The products were analyzed by XRD, SEM, TEM, XPS, BET and FTIR. Results indicated that PEG 6000 played a crucial role in the formation of the hierarchical MoS 2 microspheres and the obtained MoS 2 microspheres with diameters of 5–10 µm are organized by numerous ultrathin nanosheets assembled nanospheres. Interestingly, the MoS 2 architectures displayed remarkable performance towards removal of methylene blue (MB) from aqueous solution. More importantly, the hierarchical MoS 2 microspheres were easy to separate from the reaction system because of the hierarchical structure and large sizes. This resulting hierarchical MoS 2 microspheres are very promising adsorbent for adsorb organic pollutants and other applications. [ABSTRACT FROM AUTHOR]