Bi2S3/2D-Bi2WO6 composite materials which combined 2D-Bi2WO6 with Bi2S3 nanoparticles were prepared via ion exchange method. The mass ratio of Bi2S3 nanoparticle could be modulated by changing the quantity of thioacetamide (TAA). For Bi2S3/2D-Bi2WO6 composite materials, Bi2S3 nanoparticles dispersed on the surface of Bi2WO6 nanosheets. The photocatalytic activity was evaluated by photodegradation rhodamine B (RhB) under visible light. RhB was photodegraded nearly completely by BWS-2, while only 67% was photodegraded by Bi2WO6 nanosheet after 5 h' visible light irradiation. Based on the optical and electrochemical measurements, Bi2S3/2D-Bi2WO6 composite materials have prolonged carriers' lifetime, improved carriers' separation efficiency and decreased carriers' recombination efficiency. These results endow Bi2S3/2D-Bi2WO6 composite materials with high photocatalytic activities.