Elaboration of the new preparation methods of active photo-catalysts with highly developed surface based on the fine-disperse dironoxides, using the nano-sized TiO2, is a perspective way to create a highly active photo-catalyst. The surface of the material produced can be modified in order to ensure the spatial charge separation within the particles and shift the absorption spectrum towards the lower energy area. An advantage of nano-particles, as compared to the microparticles, is higher probability of the charges exit on the catalyst’ surface. A modified technological process has been elaborated based on the earlier proposed sol-gel process of nanostructured goetite preparation [1]. The stabilized hydrophylic goetite (feooh) particles are produced in the rotating reactor, in which the galvano-chemical dissolving of iron occurs in the field of the shortcut galvanic element iron-coke in water environment, due to the galvanic pair elements’ alternating contacting with each other. The main redox reaction running on the coke surface under aeration within the ph range Ph=6÷10, is oxygen reduction reaction: O2+ 2H2O + 4e = 4OH- accompanied with the solution alkalinization. However, within this ph range, iron surface can be passivated so it become unavaliable for further dissolving. To prevent pasivation and provide the constant activation of iron surface, Cl- ions are introduced. Anodic dissolving of iron follows the general-type reaction: Fe+2OH- = Fe(OH)2+2e, and then, goetite formation occurs as a result of oxidation and hydrolysis processes: 4Fe(OH)2+O2 = 4FeOOH+2H2O. The process is carried out in the solution flow in the galvano-coagulator rotating with the speed of 10-15 rot/min, filled with the package of iron shavings and coke with the ratio 1 : (2-3), forming the galvanic pair. As a result of the series of processes running within the reactor, the gelatinous sediment is formed, which is separated with flocculation treatment and subsequent sedimentation or centrifugation. As a flocculant, a mixture of polyacrylamide with NaCl has been used. The sediments thus obtained are not ferromagnetic and have a roentgen-amorphous structure, with high dispersion. The nano-dispersed goetite is a perspective catalyst for the photocatalytic treatment of water systems polluted with the persistent organic components. Under the UV-irradiation, a photocatalytic reaction mechanism is realized, connected with the formation of hydroxyl-radical (•OH) and superoxide-radical •O2-formed as a result of the FeO(OH) photodissociation:Active radicals thus formed promote the efficient decomposition of the polluting organic molecules up to the formation of inoffensive simple salts and gas molecules.