This study was aimed to investigate the development of a technology for the extraction of niobium pentaoxide and ammonium sulfate from titanium-magnesium production waste, specifically, the sublimates of dust chamber into concentrate in the form of niobium pentoxide. Optimal conditions for washing the niobium hydroxide precipitate by repulpation with hot (60–70°C) distilled water, drying at 200°C for 6 hours were determined. The influence of temperature and duration of the process was studied. Optimal conditions for the dynamic desorption of niobium from saturated ionite (Purolite A100) were determined. The results further indicated that the optimum quantity of the solution of desorption with sulfuric acid was equal to 5.5% and ammonium oxalate was equal to 4 %, while temperature and the flow rate of the desorbing solution were 22–27°C and 6 rpm, respectively. The study of the precipitation of niobium from sulfuric acid desorbates showed that the interaction of niobium ions with ammonia takes place at a low rate. The degree of precipitation of niobium hydroxide equal to 99.6% was achieved in 7 hours of agitation of the suspension at a temperature of 22–25°C.