The photocatalytic properties of MoS2 samples including nano-ball, nano-slice and bulk 2H-MoS2 were evaluated and compared with that of the anatase TiO2 using the degradation reaction of methyl orange under visible light. The catalytic behaviors of the samples were also characterized using transmission electron microscopy, Brunauer-Emmett-Teller (BET) surface area, ultraviolet-visible spectroscopy, and FTIR spectroscopy. The results show that the bulk MoS2 and the anatase TiO2 were almost inactive under visible light. The nano-slice presented the most positive catalytic effect because it has a wide absorption at 400–700 nm and a high BET surface area. Though the BET surface area of the nano-ball was lower than that of the nano-slice, it has an active curved basal surface and presented a catalytic activity close to that of the nano-slice. Moreover, the MoS2 nano-slice catalyst could be conveniently regenerated after filtration and drying.