According to the difference of chemical deposition behavior of arsenic and iron ion in the different pH value solution, valuable element Fe was first recovered by the selective deposition from bio-oxidation wastewater and then it was used to prepare nano-iron oxide red pigment powders. The effect of purifying conditions, calcinations temperature and calcinations time on the product color, the average partical size had been investigated. The crystal structure, particle-size and properties of the nanoparticles were characterized by means of XRD, TEM. The optimal process conditions of the preparation of iron oxide red were: calcinations temperature was 900°C, calcinations time was 120min. Under these conditions, the color of production was bright red. The particles were fully developed, and the average diameter of nanometer particle was about 70.8nm. In the visible light region of 380 to 780nm, the particle possessed good transparency, achieving the standard of GB1863 – 89.