Patent GB-768124-A (GB)
Title: Improved method and apparatus for obtaining ductile titanium or zirconium
Inventor: HILL KENNETH MARSH
IPC: C22B34/14
Filed: 1953-06-13
Abstract: 768,124. Producing titanium or zirconium. SPENCE & SONS, Ltd., P. Sept. 9, 1954 June 13, 1953], No. 16336/53. Class 82(1) An apparatus for the preparation by halide reduction and purification of titanium or zirconium comprises a reaction vessel, a condensing vessel inverted with respect to and mounted on the reaction vessel, heating means for the reaction vessel, temperature control means for the condensing vessel, evacuating means for for the space enclosed by the reaction and condensing vessels and means for inverting the reaction and condensing vessels so that their relative positions are interchangeable. In the form shown suitable for the production of titanium, the reaction vessel 3 has a flange 4 which is welded to a flange 7 of the condensing vessel 8 and a vacuum conduit 9, connected via a conduit 12 and a valve 13 to a vacuum pump 14, projects into the condensing vessel. The reaction vessel 3 surrounded by a tank 27 containing an electric vacuum furnace 28, the tank having an evacuuating conduit 29. The condensing vessel 8 is surrounded by a jacket 21, constituting the temperature control means, through which coolant e.g. water is passed. The flanges 25 of the condensing vessel 8 support trunnions (not shown) the common axis of which is normal to the plane of the Figure so that by rotating the trunnions in the bearings provided the whole apparatus is turned and the relative position of the reaction and condensing vessels are interchanged. A steel liner 5, mounted within the reaction vessel and covered by a grill 3a, is fitted with a drainage conduit 34 closed by a cap 38 and the condensing vessel is fitted with a drainage conduit 42 closed by a cap 43. The titanium tetrachloride is fed to the reaction vessel through a delivery conduit 10 mounted within the vacuum conduit 9, the conduits 9 and 10 carrying a series of baffles 9d, 10b of the " disc and doughnut " type. In operation a charge of magnesium is placed in the liner 5, which contains enough anhydrous magnesium chloride to ensure that the cap 38 contacts magnesium chloride and not magnesium, and the space enclosed by the vessels 3 and 8 is evacuated and filled with argon. The charge is heated to 750‹C. by the furnace 28 and titanium tetrachloride is fed from a feed system 18, via the conduit 10, to a conical cap 20 where radiant heat from the reaction vesconduit 42 closed by a cap 43. The titanium tetrachloride which reacts with the magnesium to form titanium sponge. Magnesium chloride may be drained from the vessel during the reaction by the conduit 34 and on completion of the reaction surplus titanium tetrachloride is removed to the scrubbing system 19. The apparatus is inverted on the trunnions, so that some magnesium chloride and excess magensium drain into the condensing vessel, and the spaces enclosed by the vessels 3, 8 and the furnace 28 are each evacuated. Water is circulated through the jacket 21 and at a temperature of 800‹C. the space enclosed by the vessels 3, 8 is further evacuated to a vacuum of the order of a few microns and the reactor heated to 900‹C. so that distilled magnesium chloride and magnesium collect in the condensing vessel. After ten hours the furnace is switched off and when the temperature has fallen to 800‹C. the vacua in the enclosed space and the furnace are simultaneously relieved with argon and air respectively prior to draining the condensing vessel, via the conduit 42, and removing the liner. A larger type reactor is also referred to in the Specification, this reactor having mechanical loading and unloading of the liners. In this type of reactor further reducing agent is preferably added during the reaction. According to the Provisional Specification, fused salt at 200‹C. is used as a coolant for the jacket 21 and the magnesium chloride and magnesium is distilled from the titanium sponge at 925‹C. Reference has been directed by the Comptroller to Specification 638,840.