To provide a purifying process and vacuum separating equipment having a separating vessel protected from deformation when titanium sponge is processed at a high temperature and under reduced pressure to separate magnesium chloride and magnesium metal remaining in titanium sponge and subsequently feed the separated chloride and metal into a condensing vessel for condensation and removal.

This purifying process uses a separating vessel 5 contained in a heating furnace to eliminate impurities from titanium sponge obtained as a result of the chemical reaction of magnesium metal and titanium tetrachloride. The process features that the heating furnace 1 and the separating vessel 5 are kept under reduced pressure while the pressure of the inside of the separating vessel 5 is retained higher than that of the space 1a between the separating vessel 5 and the heating furnace 1.