KR820001546B1 - Production of titanium metal valves - Google Patents

Abstract

A titanium recovery process comprises (a) oxidizing a Ti source, which also contains Fe, V, Ni and Cr values, at from ambient to 800 ≰C to convert Fe values to the oxide; (b) reductively roasting part of the product, (c) leaching the reduced product with a HCl source at 80-100 ≰C, (d) contacting the resulting leached slurry with the rest of the product from stage (a) at 75-105 ≰C to separate Ti oxides; (e) treating the separated solution to recover the other metal values and form a HCl source which is recycled to stage (c). Reactions are effected in a short time and all process stages can be carried out at atmosphere pressure.

Description

How to recover titanium from titanium and other metal-containing materials

The accompanying drawings are flow diagrams of the process of the present invention.

The present invention relates to a method for recovering titanium metal from a titanium metal containing source, and more particularly, to a method for recovering titanium from a titanium containing source such as ilmenite.

An advantage of the present invention is that the reaction can be carried out in a relatively short time, and the method can all be carried out under atmospheric pressure, thus avoiding the use of expensive and complicated equipment.

In addition to the advantages described above, high titanium recovery can also be achieved using low quality ores such as ilminite as starting materials.

Another advantage of the present invention is that the leaching solution has a strong reducing power, so it is excellent in stability even at a relatively high temperature and titanium dioxide (TiO ₂ ) such as rutile is recovered below the boiling point of the leaching solution. In addition, the need for industrial water is reduced because there is no need to dilute the acid to be used as a leaching solution to precipitate titanium dioxide.

It is therefore an object of the present invention to provide an improved method for producing titanium metal.

It is still another object of the present invention to provide a wet smelting method capable of obtaining titanium metal from a titanium containing source in high yield.

As an example of the present invention, first, the first titanium-containing source is reduced roasted at high temperature, the reduced substance obtained above in the leaching zone is leached with hydrogen chloride, and the second titanium-containing source containing iron is oxidized therein. Converts the contained iron into iron oxide, precipitates the leached titanium containing source with at least a portion of the above-described oxide containing iron oxide, separates and recovers the precipitated titanium from the soluble metal material, and Is a method for recovering titanium from a titanium-containing source containing other metals, which is composed of recovering other metals, producing hydrogen chloride, and then recycling the aforementioned hydrogen chlorides to the leaching zone.

The method of the present invention is explained in more detail by reducing roasting the first titanium-containing source at a high temperature in the range of 600-1000 ° C. in the reducing atmosphere, and leaching the reduced material obtained above in the leaching zone with hydrochloric acid at a temperature in the range of 80-100 ° C. The second titanium-containing source containing iron is introduced into an oxidation process in an oxidizing atmosphere at a temperature ranging from room temperature to 800 ° C, and the leached titanium-containing source is at least a portion of the oxide containing iron oxide and 75-105. The precipitate is contacted at a temperature in the range of ℃, and the precipitated titanium dioxide is separated and recovered, and the soluble metal content is treated to recover other metals, generating hydrogen chloride, and then recycled to the leaching zone.

As described above, the present invention relates to an improved method for obtaining titanium metal from titanium metal-containing sources such as ore including illite, rutile, etc., and using this method, relatively low cost equipment and low quality The ore can also be used to obtain the target in high yield.

The method is carried out by heating the first titanium containing source in a reducing atmosphere to a temperature of about 600-1000 ° C. to reduce roasting. More preferably, the reducing component used for roasting purposes uses a mixture of about 2-3 times the amount necessary to completely reduce the iron present in the system to the metal. However, hydrogen and carbon monoxide may be used alone rather than in mixtures.

The titanium metal-containing source is reduced roasted and then placed in an aqueous solution of hydrogen chloride and leached for 0.25-1 hour or longer at a temperature in the range of 80-100 ° C. The aqueous hydrogen chloride solution has the same characteristics as hydrochloric acid, but contains about 20% to 37% hydrogen chloride. After completion of the leaching process, the leaching slurry (Slurry) is precipitated without removing the gangue in order to prevent insoluble titanium from being lost during the separation process. Precipitation of titanium, such as titanium dioxide, is accomplished by treating the leaching slurry with at least a portion of a second titanium containing source containing other metals such as iron, vanadium, chromium, nickel, etc. which have been subjected to oxidation. In the present invention, it is more preferable to grind the ore to a size smaller than about 100 mesh. The oxidation step in which the iron in the ore is converted to iron oxide can be carried out by contacting the ore with water for several days at room temperature or by roasting it in an oxidizing atmosphere in the presence of air or oxygen at a temperature in the range of about 600-800 ° C. for about 1-10 hours. have. The oxidized ore is added to the leaching solution at a high temperature in the range of 75-105 ° C. and the mixture is stirred for about 2 minutes-1 hour or longer. After completion of the precipitation step, the solid is separated from the solution by conventional methods such as filtration or decantaton and the solid titanium dioxide is recovered. The waste liquid is sent to a treatment zone where the liquid is crystallized with ferrous chloride hydrate or spray dried to produce ferric oxide together with oxides of dissolved metals such as vanadium, nickel and chromium.

The formation of other metals in the treatment zone results in the formation of a solution for concentrated hydrochloric acid, which is recycled and sent to the leaching zone for use as a leachate. It is preferred to introduce a single titanium containing source into the oxidation step, separate it into two parts, reduce one part and roast it with hydrochloric acid. Titanium precipitation, such as titanium dioxide, is then performed by contacting the leaching slurry with the remaining portion of the oxidized ore.

The present invention will be described in detail below with reference to the accompanying drawings.

In this method, a titanium-containing source such as ilminite pulverized to a predetermined size is charged into the oxidation zone 2 through the conduit 1. In this device, ore is oxidized by contact with water at room temperature or by contact with oxidizing gas such as oxygen or air at high temperature. Such iron is converted to ferric oxide and the contained material is discharged from the oxidation zone 2 through the conduit 3. Part of the oxide material is introduced into the reduction zone 5 through the conduit 4. Here, the oxidized ore is reduced roasted in the above-mentioned temperature range in the presence of a reducing agent composed of hydrogen, carbon monoxide, or mixtures thereof, wherein the reducing agent is fed to the reduction zone 5 via a conduit 6.

After reduced roasting for a predetermined time, the titanium-containing ore is discharged from the reduction zone 5 through the conduit 7 and introduced into the leaching zone 8.

In the leaching zone (8), the ore is subjected to the action of hydrogen chloride, and a portion of the hydrogen chloride can be introduced into the aforementioned zone through the conduit (9). The leaching step is carried out at a high temperature in the range of 80-100 ° C. for a predetermined time during which the metal can be sufficiently converted to chloride of the dimetal. After completion of the leaching, the leaching liquid is discharged from the leaching zone 8 and introduced into the settling zone 11 through the conduit 10.

In the precipitation zone 11 the leachate is brought into contact with some of the ore remaining from the oxidation zone 2 and the oxidized light described above is introduced into the precipitation zone 11 through the conduit 12.

In the precipitation zone 11, titanium is converted into titanium dioxide and precipitated, while iron present in the photooxidation ring is converted to ferrous chloride and then dissolved in the leaching solution. The amount of oxidized ore used to precipitate titanium chloride into titanium dioxide depends on the amount of titanium chloride present in the leachate, and the optimal weight of ferric oxide required to precipitate titanium into titanium dioxide is the amount of ferric oxide and precipitate The weight ratio of titanium dioxide is in the range of about 1.5: 1 to 2: 1. The already used leachate containing solid titanium dioxide is discharged from the precipitation zone 11 and introduced into the separation zone 14 through the conduit 13. Here, the solid titanium dioxide is separated from the already used leachate containing dissolved metal chlorides by conventional methods such as filtration or decantation as described above.

Solid titanium dioxide is discharged through the conduit 15, washed, recovered and used. The leachate used is discharged from the separation zone 14 and introduced into the treatment zone 17 through the conduit 16. Here, the leachate is crystallized with ferrous chloride hydrate or spray dried to produce ferric oxide together with vanadium oxide, nickel oxide, chromium oxide and the like.

Solid oxide is discharged through conduit 18 in treatment zone 17. A concentrated hydrochloric acid solution is produced in the treatment zone 17 together with the oxide, and the solution is discharged through the conduit 19 and recycled to the leaching basin 8 for use as part of the leaching liquor.

Example 1

Norwegian ilminite ore, which was analyzed to contain 30% iron and 28% titanium, was crushed to a -35 mesh Tyler size and the crushed ore (140 grams) was reduced to all metals for 1 hour. Reduction was carried out using a reducing agent approximately 2.5 times the stoichiometric requirements of the reducing atmosphere (50% hydrogen, 50% carbon monoxide). American ilminite ores analyzed with 35% iron and 33% titanium were ground to a -35 mesh size and roasted at 750 ° C. for 4 hours in a humid oxygen atmosphere. 35 grams of reduced ilminite ore were leached under reflux for 15 minutes at 100 ° C. using 300cc concentrated hydrochloric acid. Analysis of the product by filtration of the solution showed that 11.5 grams of solid contained 29% titanium and 3.4% iron. In addition, the solution contained 26 grams of titanium per liter. A portion of the solution, 100 cc, was heated to 80 ° C. and 18.5 grams of oxidized ilminite was added. The mixture was left without stirring for 5 minutes and then stirred at a temperature of 80 ° C. for 55 minutes. A precipitate of 13.5 grams was obtained, which showed that it contained 55% titanium and 11% iron, and the 88 cc solution contained 15 grams of titanium per liter of solution. Thus, as a result, 89% of iron was removed with the solution and 87% of titanium was obtained as a solid.

Example 2

Canadian ilminite was crushed to -28 mesh Tyler size and reduced at 750 ° C. for 1 hour with sufficient reducing agent twice the required amount of reducing agent containing a mixture of 50% carbon monoxide and 50% hydrogen. .

The reduced ilminite was leached with 300 cc hydrochloric acid at 100 ° C. for about 15 minutes. Analysis of gangue and solution revealed that 97% titanium was extracted. Then 100 cc of solution containing 48 grams of titanium per liter of solution were heated at 80 ° C. and mixed with oxidized ilminite ground to -270 mesh size. The oxidized ilminite analyzed with 27% titanium and 31% iron was oxidized by standing in carbonated water for 48 hours. The oxidized ilminite slurry and soluble titanium were reacted for 1 minute without stirring and for 4 minutes with stirring. Titanium dioxide was precipitated to separate the solid from the solution and analyzed to find that the solid contained 38% titanium and 19% iron and the solution contained 39 grams of titanium per liter.

Claims (1)

As described above in the text and shown in the drawings, the first titanium-containing source is reduced roasted at a high temperature, leached it with hydrogen chloride in the leaching zone, and then the second titanium-containing ring containing iron is oxidized to form iron contained therein. Conversion to iron oxide, precipitation of the leached titanium-containing source in contact with at least a portion of the oxide containing iron oxide, separation of the precipitated titanium from the soluble metal source, and treatment of the soluble metal source to Recovering and producing hydrogen chloride, and then recycling the hydrogen chloride to the leaching zone, wherein the titanium is recovered from the titanium and other metal-containing materials.

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