AU744752B2 - Process of producing synthetic rutile from ilmenite - Google Patents
Process of producing synthetic rutile from ilmenite Download PDFInfo
- Publication number
- AU744752B2 AU744752B2 AU63575/98A AU6357598A AU744752B2 AU 744752 B2 AU744752 B2 AU 744752B2 AU 63575/98 A AU63575/98 A AU 63575/98A AU 6357598 A AU6357598 A AU 6357598A AU 744752 B2 AU744752 B2 AU 744752B2
- Authority
- AU
- Australia
- Prior art keywords
- ilmenite
- fine grain
- grain fraction
- aeration
- ash
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Ceased
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- YDZQQRWRVYGNER-UHFFFAOYSA-N iron;titanium;trihydrate Chemical compound O.O.O.[Ti].[Fe] YDZQQRWRVYGNER-UHFFFAOYSA-N 0.000 title claims description 20
- 238000000034 method Methods 0.000 title claims description 16
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims description 10
- 238000005273 aeration Methods 0.000 claims description 20
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims description 19
- 239000000243 solution Substances 0.000 claims description 16
- 235000013980 iron oxide Nutrition 0.000 claims description 13
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 12
- 229910052799 carbon Inorganic materials 0.000 claims description 12
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 11
- 239000000203 mixture Substances 0.000 claims description 11
- 238000012216 screening Methods 0.000 claims description 11
- 239000000725 suspension Substances 0.000 claims description 11
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 10
- 239000007787 solid Substances 0.000 claims description 10
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 8
- 238000000926 separation method Methods 0.000 claims description 8
- VBMVTYDPPZVILR-UHFFFAOYSA-N iron(2+);oxygen(2-) Chemical class [O-2].[Fe+2] VBMVTYDPPZVILR-UHFFFAOYSA-N 0.000 claims description 7
- 230000005484 gravity Effects 0.000 claims description 6
- 235000019270 ammonium chloride Nutrition 0.000 claims description 4
- 239000003638 chemical reducing agent Substances 0.000 claims description 2
- 235000009917 Crataegus X brevipes Nutrition 0.000 claims 1
- 235000013204 Crataegus X haemacarpa Nutrition 0.000 claims 1
- 235000009685 Crataegus X maligna Nutrition 0.000 claims 1
- 235000009444 Crataegus X rubrocarnea Nutrition 0.000 claims 1
- 235000009486 Crataegus bullatus Nutrition 0.000 claims 1
- 235000017181 Crataegus chrysocarpa Nutrition 0.000 claims 1
- 235000009682 Crataegus limnophila Nutrition 0.000 claims 1
- 235000004423 Crataegus monogyna Nutrition 0.000 claims 1
- 240000000171 Crataegus monogyna Species 0.000 claims 1
- 235000002313 Crataegus paludosa Nutrition 0.000 claims 1
- 235000009840 Crataegus x incaedua Nutrition 0.000 claims 1
- 239000007864 aqueous solution Substances 0.000 claims 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 6
- 239000003245 coal Substances 0.000 description 6
- 229910052717 sulfur Inorganic materials 0.000 description 6
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 5
- 238000007885 magnetic separation Methods 0.000 description 5
- 239000011593 sulfur Substances 0.000 description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 229910052742 iron Inorganic materials 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 229910004298 SiO 2 Inorganic materials 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000002386 leaching Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229940032330 sulfuric acid Drugs 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000000571 coke Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 239000000498 cooling water Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- JTJMJGYZQZDUJJ-UHFFFAOYSA-N phencyclidine Chemical class C1CCCCN1C1(C=2C=CC=CC=2)CCCCC1 JTJMJGYZQZDUJJ-UHFFFAOYSA-N 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 150000003464 sulfur compounds Chemical class 0.000 description 1
- 238000011144 upstream manufacturing Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Inorganic Compounds Of Heavy Metals (AREA)
Description
'/UUI/ 1 28/e91 Regulation 3.2(2)
AUSTRALIA
Patents Act 1990
ORIGINAL
COMPLETE SPECIFICATION STANDARD PATENT Application Number: 63575/98 Lodged: 23 APRIL 1998 Invention Title: PROCESS OF PRODUCING SYNTHETIC RUTILE FROM ILMENITE The following statement is a full description of this invention, including the best method of performing it known to us I Process of Producing Synthetic Rutile from Ilmenite *Description This invention relates to a process of producing synthetic granular, carbonaceous reducing agent is charged into a rotary tube, and.by supplying air in the rotary tube the ilmenite is reduced at temperatures in the range from 1000 to o 13000C, the mixture containing reduced ilmenite is cooled to temperatures in the range from 50 to 200*C, and from the cooled mixture a fine grain fraction containing reduced ilmenite with grain sizes of 0 to not more than i mm is separated by screening, which fine grain fraction contains carbon, ash and gangue.
Such process is described in the U.S. Patent No. 5,403,379, where together with screening a magnetic separation is effected in addition, as the reduced ilmenite is strongly magnetic and can be separated from nonmagnetic impurities such as ash and gangue.
as ash and gangue.
2 The object underlying the invention is to provide a rather inexpensive process of producing synthetic rutile, where a magnetic separation is omitted. In accordance with the invention this is achieved in the above-mentioned process in that the fine grain fraction is supplied to an aeration stage, in which the fine grain fraction is stirred in an aqueous chloride solution by supplying air, where iron oxides are formed, that from the aeration stage a suspension containing synthetic rutile, iron oxides, carbon, ash and gangue is withdrawn, which is passed through a gravity separation, where a product phase and a phase rich in iron oxide are obtained, the solids of the product phase comprise at least 85 wt-% TiO 2 and the phase rich in iron oxide contains at least wt-% of the carbon, at least 90 wt-% of the ash and at least 80 wt-% of the gangue, which are contained in the fine grain fraction coming from the screening and supplied to the aeration zone.
The process in accordance with the invention operates without the expensive magnetic separation, and the mixture containing go the reduced ilmenite is supplied from the cooler directly S" into the screening, and from the screening the fine grain fraction is supplied directly to the aeration stage. Carbon, ash and gangue are only separated from the product phase by Sgravity separation. Usually, screening is effected such that the desired fine grain fraction has grain sizes up to not more than 1 mm.
It is recommended to use an ammonium chloride solution as aqueous chloride solution in the aeration stage. The chloride concentration of the solution usually lies in the range from 7 to 30 g/l.
For the gravity separation of the suspension coming from the aeration stage there is advantageously used at least, one hydrocyclone, at least one hydroseparator or at least one cen- 3 trifuge. It is also possible to connect a plurality of these different apparatuses in parallel or in series. The hydroseparators known per se are also referred to as upstream classifiers, when they operate with water flowing upwards.
When the gravity separation is effected by one or several hydrocyclone stages, it is recommended to employ cyclones with a relatively small diameter. With a higher pressure loss there are also achieved higher centrifugal forces, which improves the separation of solids. The number of the cyclone .stages connected in series usually lies in the range from 2 to 4 cyclone stages. The number of the hydrocyclones per stage, which are connected in parallel, expediently lies in the range from 1 to 5 and preferably 1 to 2 hydrocyclones.
*i Further embodiments of the process will be explained with S reference to the drawing, which represents a schematic flow diagram.
To the rotary tube 1 coal, ilmenite, sulfur and recirculated coke (char) are supplied through the charging tube 2. Sulfur or sulfur-containing material may also be introduced from the discharge end of the rotary tube. The grain sizes usually lie below 50 mm. The addition of sulfur per kg ilmenite usually S is about 5 to 25 g, and there may not only be added elementary sulfur, but also a sulfur compound. The temperatures in the rotary tube lie in the range from 1000 to 1300 0 C and preferably 1100 to 1200 0 C. Blowers 5 connected with the rotary tube deliver combustion air into the interior of the rotary tube, and by means of the coal injection system 6 coal is additionally supplied to the rotary tube by means of air.
In the rotary tube 1, the iron oxide content of the ilmenite is reduced.
Hot exhaust gas leaves the rotary tube through the duct.8 and the chimney 9. Separated dust is removed through lin e'.11; it 4 is mostly recirculated to the rotary tube in a manner not represented here.
In the rotary tube 1 a hot mixture is formed, which contains reduced ilmenite. This mixture is delivered through the transfer chute 15 to a rotary tube cooler 16, onto the shell of which cooling water is directed from the outside through line 17. From the cooler 16 through the cooler discharge chute 18 a cooled solids mixture with temperatures in the range from 50 to 200 0 C and preferably not more than 90oc is withdrawn and delivered to a screening means 20, where a coarse fraction is separated, which contains coal and is discharged via line 21. The remaining fine grain fraction, which has grain sizes up to not more than 1.0 mm and preferably not o ~more than 0.8 mm, chiefly consists of reduced ilmenite. The I: fine grain fraction in addition contains carbon, ash and gangue.
The fine grain fraction from the screening 20 is dosed and delivered through line 22 to a pump condensate tank 23, to which there is also supplied an aqueous chloride solution So through line 24. The mixture of the tank 23 then flows into an aeration stage 25; air is supplied via line 27. Metallic iron is oxidized by stirring. Usually, several tanks are emee ployed, which are operated continuously or discontinuously, which is, however, not represented in the drawing for simplification. The chloride solution preferably is an ammonium chloride solution, where the chloride concentration lies in the range from 7 to 30 g/l. Oxygen in the form of air is introduced in a hyperstoichiometric amount, with reference to the desired oxidation reactions, where per mol metallic iron 2 to 5 mol 02 are calculated.
From the aeration stage 24 through line 26 a suspension is withdrawn, which contains synthetic rutile, iron oxides, carbon, ash and gangue. This suspension is first introduced into the intermediate tank 28. From here, the suspension is supplied to a separating means 30, which preferably operates according to the principle of gravity. The product phase rich in TiO 2 which was recovered through the separation 30, is withdrawn via line 38, the phase poor in Ti02, which chiefly contains iron oxides, carbon, ash and gangue, is delivered through line 37 to a settling tank 45, where the solids are deposited and, if necessary, can be withdrawn through line 46. A largely clarified chloride solution is withdrawn from the tank 45 through line 25, mixed with fresh solution from line 49, and first of all introduced into the storage tank from where the solution flows into the pump condensate S: tank 23.
o In the product phase rich in TiO 2 in line 38 the solids comgo prise at least 85 wt-% and preferably at least 90 wt-% TiO 2 By filtering and drying this product might be recovered as saleable material already at this point. Usually, a higher purity of the product is desired. This can be achieved in a manner known per se by leaching in an aqueous sulfuric-acid solution. In the drawing, the leaching 55 is shown in a sim-
V.
plified representation with its addition of dilute sulfuric acid through line 56. In the suspension withdrawn via line 57 the synthetic rutile is contained, which is dehydrated and ooo* recovered, for instance, after filtering and drying (not represented). Exhaust gas is withdrawn via line 58.
Example: For operating on a laboratory scale, an Australian ilmenite has been provided, which was reduced with coal in the rotary tube furnace at 1200 0 C. The screened fine grain fraction with grain sizes of not more than 0.7 mm has the following chemical analysis: 6 TiO 2 63.4 wt-% Fe 24.9 wt-% Iron oxides 2.1 wt-% C 2.0 wt-% S 0.7 wt-% Mn 0.9 wt-% SiO 2 A1 2 0 3 MgO 5.7 wt-% other substances 0.3 wt-% The aeration is effected in a stirred tank by supplying air in an aqueous ammonium chloride solution with a chloride content of 20 g/l for 8 hours. The pH value of the suspension is about 6, the temperature rises to 80°C as a result of exo- S: thermal reactions. After the aeration, the suspension is passed through 5 series-connected hydrocyclones of porcelain, which each have a maximum inside diameter of 50 mm. At the entrance into the below-mentioned hydrocyclone, the suspension has the following weight per liter: 1st cyclone 1.35 kg 2nd cyclone 1.45 kg 3rd cyclone 1.45 kg 4th cyclone 1.45 kg cyclone 1.25 kg The phases poor in TiO 2 which leave the respective cyclone, are collected and not used any further, they contain coal and ash. The product phase coming from the 5th hydrocyclone has the following chemical analysis of the solids indicated in column A (in 7 A B TiO 2 91.1 91.4 Fe (total) 2.9 2.7 SiO 2 1.1 1 A1 2 0 3 1.2 1.2 MgO 0.24 0.23 Mn 0.84 0.85 C 0.35 0.26 S 0.74 0.73 97 wt-% of the Tio 2 delivered to the aeration are obtained in the phase rich in TiO 2 (product phase) of the 5th hydrocyclone. When for comparison purposes the screened fine grain fraction is subjected to a magnetic separation prior to the aeration, for separating carbon and ash, the aeration is per- S formed as described above, and aerated suspension is passed through a hydrocyclone, the solids of the heavy phase have the composition indicated in column B of the above table.
There are recovered 95 wt-% of the TiO 2 supplied to the magnetic separation.
*0 0•
Claims (4)
1. A process of producing synthetic rutile from ilmenite, where granular ilmenite together with granular, carbona- ceous reducing agent is charged into a rotary tube, and by supplying air in the rotary tube the ilmenite is re- duced at temperatures in the range from 1000 to 1300 0 C, the mixture containing reduced ilmenite is cooled to tem- peratures in the range from 50 to 200oC, and from the cooled mixture a fine grain fraction containing reduced ilmenite with grain sizes of 0 to not more than 1 mm is separated by screening, which fine grain fraction con- tains carbon, ash and gangue, characterized in that the fine grain fraction is supplied to an aeration stage, in S: which the fine grain fraction is stirred in an aqueous chloride solution by supplying air, where iron oxides are formed, that from the aeration stage a suspension con- taining synthetic rutile, iron oxides, carbon, ash and gangue is withdrawn, which is passed through a gravity separation, where a product phase and a phase rich in iron oxide are obtained, the solids of the product phase comprise at least 85 wt-% TiO 2 and the phase rich in iron oxide contains at least 90 wt-% of the carbon, at least 90 wt-% of the ash and at least 80 wt-% of the gangue, which are contained in the fine grain fraction coming from the screening and supplied to the aeration zone.
2. The process as claimed in claim 1, characterized in that the solids content of the aqueous solution in the aera- tion stage is maintained in the range from 25 to 50 wt-%.
3. The process as claimed in claim 1, characterized in that by means of screening a fine grain fraction containing reduced ilmenite with grain sizes from 0 to 1.0 mm is 9 separated from the cooled mixture and supplied to the aeration stage.
4. The process as claimed in claim 1 or any of the preceding claims, characterized in that as aqueous chloride solu- tion an ammonium chloride solution with a chloride con- centration of 7 to 30 g/l is used in the aeration stage. The process as claimed in claim 1 or any of the preceding claims, characterized in that for gravity separation at least one hydrocyclone, at least one hydroseparator or at least one centrifuge is used. The process as claimed in claim 1 or any of the preceding claims, characterized in that from the phase rich in iron oxide solids are separated, and the chloride solution is recovered, which is recirculated to the aeration stage at least in part. 0* 9* DATED this 23rd day of April 1998. METALLGESELLSCHAFT AKTIENGESELLSCHAFT WATERMARK PATENT TRADEMARK ATTORNEYS 290 BURWOOD ROAD HAWTHORN. VIC. 3122. I oer y t t t::i and the preceding 1 pages ape a tru ,he originally, lodged ithi i6" originally lodgedo I,
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| AU63575/98A AU744752B2 (en) | 1998-04-23 | 1998-04-23 | Process of producing synthetic rutile from ilmenite |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| AU63575/98A AU744752B2 (en) | 1998-04-23 | 1998-04-23 | Process of producing synthetic rutile from ilmenite |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| AU6357598A AU6357598A (en) | 1999-11-04 |
| AU744752B2 true AU744752B2 (en) | 2002-02-28 |
Family
ID=3748370
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| AU63575/98A Ceased AU744752B2 (en) | 1998-04-23 | 1998-04-23 | Process of producing synthetic rutile from ilmenite |
Country Status (1)
| Country | Link |
|---|---|
| AU (1) | AU744752B2 (en) |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1991013180A1 (en) * | 1990-03-02 | 1991-09-05 | Wimmera Industrial Minerals Pty. Ltd. | Production of synthetic rutile |
| AU3859593A (en) * | 1992-05-15 | 1993-11-18 | Iluka Midwest Limited | An improvement to the reduction of titaniferous ores |
| AU3676099A (en) * | 1998-06-25 | 2000-01-13 | Iluka Resources Limited | Production of synthetic rutile by low temperature reduction of ilmenite |
-
1998
- 1998-04-23 AU AU63575/98A patent/AU744752B2/en not_active Ceased
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1991013180A1 (en) * | 1990-03-02 | 1991-09-05 | Wimmera Industrial Minerals Pty. Ltd. | Production of synthetic rutile |
| AU3859593A (en) * | 1992-05-15 | 1993-11-18 | Iluka Midwest Limited | An improvement to the reduction of titaniferous ores |
| AU3676099A (en) * | 1998-06-25 | 2000-01-13 | Iluka Resources Limited | Production of synthetic rutile by low temperature reduction of ilmenite |
Also Published As
| Publication number | Publication date |
|---|---|
| AU6357598A (en) | 1999-11-04 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| FGA | Letters patent sealed or granted (standard patent) | ||
| PC | Assignment registered |
Owner name: OUTOKUMPU OYJ Free format text: FORMER OWNER WAS: METALLGESELLSCHAFT AKTIENGESELLSCHAFT |