Electrodeposition of composite coatings based on copper is a promising direction in the creation of advanced materials for multifunctional purposes. An important area of composites application is to use them in the treatment systems for gas emissions and wastewater. It is advisable to use semiconductor oxide materials, in particular titanium dioxide, as the photocatalysts in the photo destruction of organic pollutants of wastewater. The structural features of wastewater treatment equipment require that titanium dioxide particles should be fixed in a rigid matrix. Resolving the task of fixing photosensitive elements at the surface of a certain configuration implies the electrodeposition of coatings by composites, in particular Cu–TiO2. An important factor affecting the functional characteristics of composites and their manufacturing technology is the nature of the electrolyte. It has been shown that the electrodeposition of Cu–TiO2 composites from methane-sulfonate electrolytes makes it possible to reduce the coagulation of the dispersed phase and to obtain coatings with a high content of titanium dioxide from a suspension solution containing no more than 4 g/l of TiO2. It was established that the content of the dispersed phase in the composite made at a current density of 2 A/dm2 and the concentration of titanium dioxide in the electrolyte at the level of 4 g/l is 1.3 % by weight, which is twice as much as when using a sulfate electrolyte. It has been shown that the increase in the content of the dispersed phase in the coatings from 0.1 to 1.3 % by weight is accompanied by an increase in the degree of photo destruction of the colorant from 6 to 15.5 %. The micro-hardness of coatings increases, in this case, by 30 %. The proposed electrolyte to make the Cu–TiO2 composites is an important contribution to the development of the synthesis of wear-resistant high-performance photocatalysts for treating wastewater from organic pollutants