Recycling of niobium and titanium from their superconductor scraps was studied introducing the operation of bench scale plant of the recycling process. The scrap of Nb-Ti alloy was chlorinated at 300°C forming NbCl2-TiCl4 mixed chloride. The TiCl4 was removed from NbCl5 by the distillation at 200-250°C under flowing nitrogen. Then NbCl5 was converted to Nb(OBun )5 by the reaction with n-BuOH in benzene at ambient temperature. The purification of Nb(OBun)5 using a distillation method was not sufficient for the further purification of niobium. Selective reduction of NbCl5 by hydrogen and distillation of TaCl5 was proved to be effective for the tantalum removal resulting in the production of NbCl5 of 99.99%. The yield of the Nb(OBun)5 from the Nb-Ti alloy scraps during the operation of bench scale plant was 82.3%.