Semi-continuous magnesium-hydrogen reduction process for manufacturing of hydrogenated, purified titanium powder

A semi-continuous magnesium-hydrogen reduction process for manufacturing of hydrogenated, purified titanium powder including the steps of:

• (a) magnesium-thermic reduction of titanium chlorides in a reactor in the temperature range of 830-880° C. in a hydrogen atmosphere at a pressure of 5-10 kPa resulting in a formation of a hollow block of a reaction mass having an open cavity in a center of the block,
• (b) heating hydrogen in a input pipe connected to a gas compressor using an electric heater and purging hot hydrogen into the reactor for heating of the reaction mass to the temperature in a range of 980-1020° C. which is optimal for a followed up vacuum separation and for maintaining a uniform temperature along the reactor sufficient to keep magnesium and magnesium chloride in a molten state,
• (c) full thermal-vacuum separation of a porous titanium compound in the reaction mass from excessive magnesium and magnesium chloride at 850-980° C. and residual pressure of 26-266 Pa (10−2-10−3 mm Hg), using a multi-step cycle including:
• (i) purging hydrogen at 800-950° C. into the reactor at a pressure 10 kPa to 24.5 kPa, (ii) directive squeezing-out of a separated liquid phase containing magnesium and magnesium chloride into an additional vessel, and (iii) application of alternate pressure to small portions of the liquid phase in pores of the porous titanium compound from different sides of the liquid phase which provides removal of the liquid phase from small pores of the titanium compound and fast evaporation of said liquid,
• (d) simultaneous controlled hydrogenation and cooling of the porous titanium compound down to 600° C. or lower temperature by purging cold hydrogen having temperature 25-35° C. into the reactor for a speedy cooling of the block of reaction mass using multiple recirculation of hydrogen in and out of the reactor, whereby a control of temperature of the block of reaction mass is carried out by adjusting the amount of purged hydrogen,
• (e) holding the hydrogenated porous titanium compound in a hydrogen atmosphere at 450-600° C. for 20-70 minutes using multiple recirculation of hydrogen that has a stable temperature,
• (f) directing hydrogen in a gas refrigerator and cooling the reactor down to 150-200° C. using this cold gas,
• (g) removing the hydrogenated porous titanium compound from the reactor,
• (h) crushing the hydrogenated porous titanium block, and
• (i) grinding the crushed hydrogenated titanium pieces into the powder having a predetermined particle size.