Patent GB-1104262-A (GB)
Title: Purification of titaniferous ores
Inventor: REEVES JAMES W
IPC: C22B3/14
Filed: 1965-04-28
Abstract: Iron is separated from ferrotitaniferous ores by reducing the iron in the ore to the metallic state by heating the ore to 700 DEG -1300 DEG C. in the presence of a reducing agent, oxidizing the metallic iron to the ferrous complex then to hydrated ferric oxide in the presence of an aqueous ammonia-ammonium carbonate solution and separating the ferric oxide from the titanium oxide.  The ore may be initially roasted in a rotary kiln or fluidized bed in free oxygen containing atmosphere at a temperature from 600 to 1000 DEG C. for 1/2 to 1 hr. The reduction of the ore may be effected by (a) a 3 stage fluidized bed using H2 pre-heated to 800 to 1100 DEG C. and the ore pre-heated to 800-1200 DEG C. with the bed being maintained at 800 to 1200 DEG C. and at 1-10 atmosphere pressure (b) in a rotary kiln maintained at 1100 DEG -1200 DEG C.  charge with a ferrotitaniferous ore mixture containing 10 to 50% by weight of coke and conducting the reducing step till no more than 75% of the iron is in the metallic state then completing the reduction in a fluidized bed heated from 900 to 1100 DEG C. using H2, water gas, partially oxidized natural gas or mixtures thereof preferably pre-heated to 100-1100 DEG C., as reducing and fluidizing gas or (c) by charging an electrically-heated fluidized bed maintained at 900 DEG C. to 1300 DEG C. with the ore crushed to 40-100 mesh and containing from 10-50% carbon and carrying out the reducing step using H2, water gas or partially oxidized natural gas or mixtures thereof, preferably pre-heated to 100 to 1200 DEG C., as reducing and fluidizing gas.  Ore sintering round the electrodes of the electrically-heated fluidized bed is prevented by maintaining a low temperature differential between the heaters and the bed, by maintaining the lowest possible bed temperature by using heaters with a large surface area, and by bed dilution with coke. The separation of ferric oxide and TiO2 is accomplished by floatation.ALSO:Iron is separated from ferrotitaniferous ores reducing the iron in the ore to the metallic state by heating the ore to 700-1300 DEG  C. in the presence of a reducing agent, oxidizing the metallic iron to the ferrous complex then to hydrated ferric oxide in the presence of an aqueous ammonia-ammonium carbonate solution and separating the ferric oxide from the titanium oxide. The ore may be initially roasted in a rotary kiln or fluidized bed in free oxygen containing atmosphere at a temperature from 600 DEG  to 1000 DEG  C. for one half to one hour.  The reduction of the ore may be effected by (a) a 3-stage fluidized bed using H2 preheated to 800 DEG  to 1100 DEG  C. and the ore preheated to 800-1200 C DEG ., with the bed being maintained at 800 DEG  to 1200 DEG  C. and at 1-10 atmospheres pressure; (b) in a rotary kiln maintained at 1100-1200 DEG  C. charged with a ferrotitaniferous ore mixture containing 10 to 50% by weight of coke and conducting the reducing step till no more than 75% of the iron is in the metallic state then completing the reduction in a fluidized bed heated from 900 DEG  to 1100 DEG  C. using H2, water gas, partially oxidized natural gas or mixtures thereof, preferably preheated to 100-1100 DEG  C., as reducing and fluidizing gas; or (c) by charging an electrically-heated fluidized bed maintained at 900 DEG  C. to 1300 DEG  C. with the ore crushed to 40-100 mesh and containing from 10-50% carbon and carrying out the reducing step using H2, water gas or partially oxidized natural gas or mixtures thereof, preferably preheated to 100 DEG  to 1200 DEG C., as reducing and fluidizing gas.  The aqueous ammonia-ammonium carbonate solution may contain 5-30% of NH3 and 3-25% by weight CO2. Ore sintering round the electrodes of the electrically-heated fluidized bed is prevented by maintaining a low-temperature differential between the heaters and the bed, by maintaining the lowest possible bed temperature by using heaters with a large surface area and by bed dilution with coke.  The oxidation step may proceed at 20 DEG  to 80 DEG  C. and at pressures of 2 to 55 p.s.i.g. (NH4)2S may be present in this solution in amounts from 0.05 to 0.20% by weight.  Any CO2 or NH3 recovered from this solution may be recycled. The separation of ferric oxide and TiO2 is accomplished by flotation.