Processing of titaniferous ores and minerals

A process for separating a soluble vanadium derivative, rare earths and scandium from a leaching solution, wherein the leaching solution comprises iron(II) chloride and/or iron(III) chloride, the process comprising the steps of:

• a) extracting iron(II) chloride and/or iron(III) chloride from the leaching solution by liquid-liquid extraction with a solvent mixture comprising between about 15% and about 25% diisobutyl ketone (DIBK) and/or methyl isobutyl ketone (MIBK), between about 50% and about 70% EXXAL-13, and between about 10% and about 30% ShellSoITM D-80;
• b) extracting the soluble vanadium derivative from the leaching solution by liquid/liquid extraction with a solvent mixture comprising between about 10% and about 30% Cyanex 923, between about 10% and about 30% EXXAL-13, and between about 50% and about 70% CF 231 to produce a vanadium derivative-containing liquid/liquid extraction phase;
• and
• c) extracting the soluble scandium derivative and other rare earths from the leaching solution by liquid/liquid extraction with a adsorbent functionalized with glycol amic acid groups. Scandium recovery is performed at a concentration ranging from 5 to 12% HCI, as it is generally the case after the leaching step of the DSO process. Collecting scandium with the resin is performed at temperature at least above about 80° C., i.e. after cooling the leaching solution which is generally operated at about 130° C.

A process for separating a soluble scandium or a rare-earth derivative from a titaniferous ore or mineral, the process comprising the steps a) to f):

• a) calcinating titaniferous particles having a size of at least about 75 cubic microns at a temperature between about 750° C. and about 1250° C. during between about 30 minutes and about 8 hours;
• b) leaching the titaniferous particles with a leaching solution to produce leached scandium or rare-earth derivatives;
• c) separating the leached scandium or rare-earth derivatives from the leaching solution with a resin at a temperature between about 80° C. and about 130° C.;
• d) eluting soluble scandium or rare earth derivatives from the resin at a temperature of between about 20° C. and 80° C., preferably between 50° C. and 85° C., with a hydrochloric acid solution having a concentration between about 2M and about 6M;
• e) Mixing the soluble scandium or rare-earth with caustic soda or sodium hydroxide to produce scandium or rare-earth hydroxide at a temperature of about 100° C.;
• and
• f) calcinating the scandium hydroxide or rare-earth at a temperature of about 400° C. to produce scandium(III) oxide or rare-earth oxide.

A process for selectively leaching out impurities from titanium rich slag , which com prises:

• a. grinding slag (synthetic rutile) from smelting process to 150 microns and generally has a chemistry of 80% TiO2 and MgO of 2 to 5%;
• b. leaching for 4 hours at between room temperature to 115° C. with 65% Nitric acid which attacks Mg, Ca and its derivatives without affecting TiO2 and iron oxides;
• c. TiO2 rich material is filtered as solids and washed;
• d. TiO2 filter cake is dried at 60° C. to produce a synthetic rutile with less than 0.3% MgO ready to be used by the chloride process industry of pigment production;
• e. the used solution of step b for selective leaching of the impurities is sent to fertilizer plant to produce nitrate, phosphate, and potassium combinations of fertilizer with Mg rich solution.

A process for separating a soluble scandium or rare-earth derivative from a titaniferous ore or mineral, the process comprising the steps a) to f):

• a) calcinating titaniferous particles having a size of at least about 75 cubic microns at a temperature between about 750° C. and about 1250° C. during between about 30 minutes and about 8 hours;
• b) leaching the titaniferous particles with a leaching solution comprising hydrochloric acid to produce a leached solution containing scandium or rare-earth derivatives, iron and magnesium;
• c) separating leached scandium or rare-earth derivatives by filtration;
• d) submitting the leached solution to hydrochloric acid regeneration to produce hematite;
• e) leaching the hematite with a leaching solution comprising nitric acid at a concentration above 65%;
• and
• f) eluting soluble scandium or rare-earth from a resin contacted with a leaching solution comprising nitric acid at a concentration above 65%.

A process for producing titanium dioxide feedstock for use in the production of titanium metals and alloys, the process comprising the steps a) to e):

• a) obtaining a titanium dioxide starting material;
• b) leaching of titanium dioxide particles with a leaching solution having hydrofluoric acid (HF) at a concentration between about 5% and about 60% and at a leaching temperature of about 70° C.;
• c) filtering out solids;
• d) heating the leaching solution to temperature between about 100° C. and 120° C.;
• and
• e) crystalizing (NH4)2TiF6 by adding a crystalizing agent of about 1% in concentration, wherein the crystalizing agent is selected from the group consisting of lithium, sodium, and chloride salts thereof, potassium chloride salt, NH4F, NH4 and NH4Cl.

A process for producing titanium metal, titanium metal alloys, titanium and 3D printing quality for titanium metal and its alloys, the process comprising the steps a) to f):

• a) leaching a high-purity titanium dioxide with leaching solution having hydrofluoric acid (HF) at a concentration between about 5% and about 60%, and at a leaching temperature of about 70° C.
• b) heating the leaching solution to temperature between about 100° C. and about 120° C.;
• c) crystalizing (NH4)2TiF6 by adding a crystalizing agent of about 1% in concentration, wherein the crystalizing agent is selected from the group consisting of lithium, sodium, and chloride salts thereof, potassium chloride salt, NH4F, NH4 and NH4Cl;
• d) performing a pre-reduction of (NH4)2TiF6 to produce Ti(III) derivatives by
• d.1) using a reducing agent to reduce (NH4)2TiF6;
• or
• d.2) electrolytically reducing (NH4)2TiF6;
• e) decomposing the Ti(III) derivatives at a temperature between about 400° C. and about 700° C. to produce TiF3;
• and
• f) reducing the TiF3 to titanium metal powder by contacting TiF3 with a plasma atomization technology.

A process for producing titanium metal and titanium, the process comprising the steps a) to f):

• a) using a high purity titanium dioxide as a metal precursor;
• b) leaching a high-purity titanium dioxide with leaching solution having hydrofluoric acid (HF) at a concentration between about 5% and about 60%, and at a leaching temperature of about 70° C.
• b) heating the leaching solution to temperature between about 100° C. and about 120° C.;
• c) crystalizing Fe(TiF6) in the form of (NH4)2TiF6 by adding a crystalizing agent of about 1% in concentration, wherein the crystalizing agent is selected from the group consisting of lithium, sodium, and chloride salts thereof, potassium chloride salt and NH4Cl;
• d) reducing (NH4)2TiF6 to produce Ti(III) derivatives and aluminum(III) fluoride (AlF3) by heating the reduction product until AlF3 on the surface of titanium metal powder comprises between about 0,005% and about 40% of the mass of the material, preferably between about 0,05% and about 10%, and more preferably between about 0,1% and about 6,0%;
• and
• f) reducing the TiF3 to titanium metal powder by aluminum/iron exchange in a furnace configured so that the titanium and fluoride are prevented from reacting with oxygen, nitrogen, carbon or hydrogen.