US2980508A - Oxidation of trivalent titanium compounds contained in solid titaniferous materials - Google Patents
Oxidation of trivalent titanium compounds contained in solid titaniferous materials Download PDFInfo
- Publication number
- US2980508A US2980508A US624505A US62450556A US2980508A US 2980508 A US2980508 A US 2980508A US 624505 A US624505 A US 624505A US 62450556 A US62450556 A US 62450556A US 2980508 A US2980508 A US 2980508A
- Authority
- US
- United States
- Prior art keywords
- oxidation
- concentrate
- titanium
- trivalent
- trivalent titanium
- 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.)
- Expired - Lifetime
Links
- 239000000463 material Substances 0.000 title claims description 42
- 238000007254 oxidation reaction Methods 0.000 title claims description 34
- 230000003647 oxidation Effects 0.000 title claims description 31
- 239000007787 solid Substances 0.000 title claims description 7
- 150000003609 titanium compounds Chemical class 0.000 title description 11
- 239000012141 concentrate Substances 0.000 claims description 31
- 238000000034 method Methods 0.000 claims description 22
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 22
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 21
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 21
- 239000010936 titanium Substances 0.000 claims description 21
- 229910052719 titanium Inorganic materials 0.000 claims description 21
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 14
- 230000029087 digestion Effects 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 150000001875 compounds Chemical class 0.000 claims description 9
- 239000002245 particle Substances 0.000 claims description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 4
- 239000001301 oxygen Substances 0.000 claims description 4
- 229910052760 oxygen Inorganic materials 0.000 claims description 4
- 238000009877 rendering Methods 0.000 claims description 4
- 239000001117 sulphuric acid Substances 0.000 claims description 3
- 235000011149 sulphuric acid Nutrition 0.000 claims description 3
- 239000002002 slurry Substances 0.000 claims description 2
- 239000002253 acid Substances 0.000 description 11
- 230000008569 process Effects 0.000 description 11
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 10
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 8
- 229910052500 inorganic mineral Inorganic materials 0.000 description 7
- 239000011707 mineral Substances 0.000 description 7
- 239000008188 pellet Substances 0.000 description 6
- 150000007513 acids Chemical class 0.000 description 5
- 239000007789 gas Substances 0.000 description 5
- 229910052742 iron Inorganic materials 0.000 description 5
- 230000009467 reduction Effects 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- 230000015572 biosynthetic process Effects 0.000 description 3
- 239000003792 electrolyte Substances 0.000 description 3
- 230000001590 oxidative effect Effects 0.000 description 3
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical class [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 description 3
- 238000005453 pelletization Methods 0.000 description 3
- 239000004408 titanium dioxide Substances 0.000 description 3
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 238000000184 acid digestion Methods 0.000 description 2
- 239000003638 chemical reducing agent Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 235000011837 pasties Nutrition 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 239000002893 slag Substances 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L sodium carbonate Substances [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- 230000003068 static effect Effects 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- XTEGARKTQYYJKE-UHFFFAOYSA-M Chlorate Chemical class [O-]Cl(=O)=O XTEGARKTQYYJKE-UHFFFAOYSA-M 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000010306 acid treatment Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- QBWCMBCROVPCKQ-UHFFFAOYSA-N chlorous acid Chemical class OCl=O QBWCMBCROVPCKQ-UHFFFAOYSA-N 0.000 description 1
- 239000000571 coke Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000008151 electrolyte solution Substances 0.000 description 1
- 229940021013 electrolyte solution Drugs 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- YDZQQRWRVYGNER-UHFFFAOYSA-N iron;titanium;trihydrate Chemical compound O.O.O.[Ti].[Fe] YDZQQRWRVYGNER-UHFFFAOYSA-N 0.000 description 1
- 238000011005 laboratory method Methods 0.000 description 1
- 229920000126 latex Polymers 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000012452 mother liquor Substances 0.000 description 1
- DCKVFVYPWDKYDN-UHFFFAOYSA-L oxygen(2-);titanium(4+);sulfate Chemical compound [O-2].[Ti+4].[O-]S([O-])(=O)=O DCKVFVYPWDKYDN-UHFFFAOYSA-L 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000008707 rearrangement Effects 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 230000007928 solubilization Effects 0.000 description 1
- 238000005063 solubilization Methods 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 229910000348 titanium sulfate Inorganic materials 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B34/00—Obtaining refractory metals
- C22B34/10—Obtaining titanium, zirconium or hafnium
- C22B34/12—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08
- C22B34/1236—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08 obtaining titanium or titanium compounds from ores or scrap by wet processes, e.g. by leaching
- C22B34/124—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08 obtaining titanium or titanium compounds from ores or scrap by wet processes, e.g. by leaching using acidic solutions or liquors
- C22B34/125—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08 obtaining titanium or titanium compounds from ores or scrap by wet processes, e.g. by leaching using acidic solutions or liquors containing a sulfur ion as active agent
-
- G—PHYSICS
- G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
- G21F—PROTECTION AGAINST X-RADIATION, GAMMA RADIATION, CORPUSCULAR RADIATION OR PARTICLE BOMBARDMENT; TREATING RADIOACTIVELY CONTAMINATED MATERIAL; DECONTAMINATION ARRANGEMENTS THEREFOR
- G21F9/00—Treating radioactively contaminated material; Decontamination arrangements therefor
- G21F9/007—Recovery of isotopes from radioactive waste, e.g. fission products
Definitions
- a carbonaceous reducing agent such as coke
- Such reduction operations may take place 'in a smelting furnace and in such cases the titanium dioxide rich slag and the metallic iron are normally tapped separately.
- the reduction may be carried out without any smeltering or sintering, for instance, in a rotating furnace. In this case the reduced "concentrate is normally crushed, subsequently washed and separated magnetically or by other mechanical means in order to recover a titanium dioxide rich concentrate and a concentrate of metallic iron.
- Such concentrates rich in titanium dioxide can also be produced by mixing a crushed titaniferous ore concentrate and small amounts of fluxes, such as sodium chloride and/or sodium carbonate, agglomerating the mixture so formed and heating the same in the presence of reducing agents so as to achieve formation of finely divided metallic iron which is subsequently separated from the titanium oxide concentrate by mechanical means.
- fluxes such as sodium chloride and/or sodium carbonate
- an object of the instant invention is to provide a process for rendering materials containing solid trivalent titanium containing values to a form amenable to digestion in concentrated mineral acids. Another object is to provide a simple method for converting the trivalent titanium compounds contained in materials of the type described to tetravalent compounds.
- the instant invention relates to a method for rendering materials containing solid trivalent titanium compounds amenable to digestion with concentrated mineral acids which comprises admixing such materials in a finely divided state with sufficient water to form a wet mass, contacting the wet mass with oxidizing gas to oxidize trivalent compounds to tetravalent compounds while maintaining the temperature during the oxidationbelow 100 C.
- the oxidation is efiected in the presence of oxi- 'dation catalysts.
- trivalent titanium compounds contained in solid titaniferous materials may be subjected to oxidation under controlled temperatures in the presence of electrolytes such as dilute solutions of mineral acids or dilute solutions of mineral salts with the result that there is obtained a high recovery of acid soluble titanium compounds.
- the oxidation of the trivalent titanium compounds takes place in the presence of controlled amounts of water or steam and an oxygen containing gas such as air while maintaining the oxidation temperature below about 100 C.
- Addition of water or steam should be made in such a way to maintain the mass to be oxidized in a thoroughly wet condition; however,
- the process may be retarded or even stopped. It is however possible to admix the amount of water required in the oxidation reaction with the material in advance.
- the material which is being oxi .dized is normally maintained in the form of a static layer of some suitable thickness. In representative cases, a moisture content of 20-30 percent of the dry weight of the concentrate has been found suitable.
- the rate of oxidation is accelerated when the material is stirred or ploughed since this action facilitates access of air and exposes fresh unoxidized material.
- the manner of-stirring and aerating the material is of importance when choosing the most effective thickness of the layer of material. Experiments have indicated that a suitable thickness of a static bed when no stirring or agitation is employed is between 10 and 25 millimeters.
- Theoxidation rate also increases with increased temperatures below 100 C. It has been observed that effective oxidation takes place between 40 and C. and
- the water addition to the mass may be done in one step as has been described or may also be extended over the whole period of oxidation, that is from the start to the interruption of the oxidation reaction. In such practice, it becomes important to closely control the moisture content of the material, that is to take steps to see that the material neither becomes too wet or too dry but rather that it maintains a moisture content dependent upon the specific material being handled and the temperature which it is proposed to maintain during oxidation.
- the material may be moistened by spraying a liquid over the surface in the form of small droplets using a spray nozzle and at the same time pelletizing the moist material. Pellets which are moistened throughout without having a pasty consistency may be prepared in this manner. These pellets should have a size between 1 and 10 millimeters and should preferably be in the 2-5 millimeter range. Such moist pellets of the particle size indicated have proved suitable for quick oxidation and are conveniently placed in layers of suitable thickness.
- the particlesize of the concentrate has been found to be significant in actual operation of the oxidation process. Initially finely divided material is preferred although thismay be pelletized as just indicated.
- the concentrate should have a particle size not in excess of about 50 microns and should preferably be in the range of 2 to 10 microns.
- X-ray diffraction patterns indicate that when the oxidation is carried out according to the present invention there is no latice rearrangement. Material both before and 'after the oxidation is identified as (Fe, Mg) -2TiO admixed with substantial quantities of titanium oxides. Anatase, rutile, and free Tigog could not be traced. It is known that compounds of the type indicated by the formula (Fe,.Mg)-2TiQ are easily digested by sulfuric acid treatment as is known to the art.
- Still another unexpected advantage of the method of the present invention is the observation that material in the oxidized trivalent state as produced may be subsequently heated at temperatures up to about 250 C. without any apparent formation of free T10 or other physical or chemical changes in the material, which would result in subsequent low recoveries when the material is subjected to sulfuric acid digestion.
- Example I -in tne trivalent state (calculated as T i was thoroughly wetted with dilute sulfuric acid (1:20) and the material was then spread out in a layer of 12 millimeters thickness. Upon contact with air the oxidation of the trivalent compounds began and the oxidation was accompanied by an increase in temperature, the temperature of the material reaching a peak of .84" C. in about fifteen minutes. At this time it was determined that after the oxidation the amount of trivalent titanium had fallen from 55.0 percent to 24.7 percent of the total amount of titanium. This corresponded to about 18.5 percent trivalent titanium calculated as TiO in the final product.
- the oxidized concentrate was digested'with sulfuric acid according to known laboratory methods using a thermos flask as the digestion chamber. Upon analysis it was determined that about 96.8 percent of the TiO, was acid soluble. This high content of soluble TiO was proof of the easily digestible. compounds which are. in the oxidized material.
- Example II This corresponded to about 19.5 percent trivalent titanium calculated as TiO- Digestion tests of this material were conducted as indicated in Example I and it was determined that about 96.0 percent of the titanium values in the oxidized prod-- not were acid soluble TiO
- Example '11 A sample of the oxidized concentrate described in Example II was furtherheated to 200 C. and kept at this temperature for half an hour. The heated material was then found to contain 25.2 percent of total titanium in the form of trivalent titanium (calculated as TiO Sulfuric acid digestion of thismaterial indicated that about 95.6 percent of the titanium was present as acid soluble TiO
- the sample of the same Ti0 rich concentrate as was employed in Example I was initially heated in air to about C. The temperature of the material increased further in a.
- the oxidized concentrate was digested with sulfuric acid according to the same technique as described in Example I.
- the content of soluble Ti0 was determined to be as low as 52 percent of the total amount of titanium oxides calculated as Ti0 in the concentrate. This result indicated considerable formation of sparingly soluble TiO during the oxidation period.
- Method for rendering a material consisting essentially of a finely divided titanium concentrate having a particle size not in excess of about 50 microns and containing solid trivalent titanium oxide amenable to digestion with concentrated sulphuric acid which comprises wetting the finely divided concentrate with water and a small amount of oxidation accelerator without dissolving the concentrate and without forming a slurry, contacting the so wetted concentrate, prior to digestion, with oxygen containing gas to oxidize the trivalent compounds to tetravalent while maintaining the temperature during oxidation below 100 C.
- oxida- 6 tion accelerator is sulphuric acid, said acid being present not in excess of 2 percent calculated on the weight of the material under treatment.
Landscapes
- Engineering & Computer Science (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Geology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- Manufacturing & Machinery (AREA)
- High Energy & Nuclear Physics (AREA)
- Physics & Mathematics (AREA)
- General Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Manufacture And Refinement Of Metals (AREA)
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| NO2980508X | 1955-12-05 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| US2980508A true US2980508A (en) | 1961-04-18 |
Family
ID=19915283
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| US624505A Expired - Lifetime US2980508A (en) | 1955-12-05 | 1956-11-27 | Oxidation of trivalent titanium compounds contained in solid titaniferous materials |
Country Status (3)
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3252275A (en) * | 1961-08-23 | 1966-05-24 | Titan Gmbh | Apparatus for the agglomeration and separation of finely divided titanium dioxide from its gaseous vehicle |
| US3368870A (en) * | 1963-12-06 | 1968-02-13 | Soloducha Nicolas | Method of producing titanium hydroxide and high grade pigments produced therefrom |
| US3868441A (en) * | 1973-05-02 | 1975-02-25 | Ethyl Corp | Process for reducing trivalent titanium content in slag |
| US3929962A (en) * | 1972-08-29 | 1975-12-30 | Chyn Duog Shiah | Titanium purification process |
| US4325920A (en) * | 1980-11-12 | 1982-04-20 | Qit-Fer Et Titane Du Quebec, Inc. | Method to oxidize Ti+3 during the sulfuric acid digestion of titaniferous slags |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE2024907C3 (de) * | 1970-05-22 | 1978-07-06 | Bayer Ag, 5090 Leverkusen | Verfahren zur Herstellung von Titandioxidkonzentraten aus ilmenithaltigen Materialien |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US1656572A (en) * | 1926-04-10 | 1928-01-17 | Firm I G Farbenindustrie Ag | Method of agglomerating pulverulent materials |
| US2125340A (en) * | 1936-01-09 | 1938-08-02 | Du Pont | Oxidation of titanous salts |
| US2149370A (en) * | 1936-01-09 | 1939-03-07 | Du Pont | Treatment of titanium liquors |
| US2339808A (en) * | 1940-03-16 | 1944-01-25 | Titan Co Inc | Process of treating ferrotitaniferous materials |
| US2589910A (en) * | 1949-03-24 | 1952-03-18 | New Jersey Zinc Co | Production of titanium dioxide |
| US2724636A (en) * | 1951-08-31 | 1955-11-22 | Nat Lead Co | Treatment of titaniferous ore concentrates to form titanium sulfate |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE510200C (de) * | 1926-08-03 | 1930-10-17 | Titan Co As | Nutzbarmachung eisenhaltiger Titanmaterialien |
| US1902203A (en) * | 1931-01-21 | 1933-03-21 | Bichowsky Foord Von | Process of preparing titanium dioxide |
-
0
- BE BE553156D patent/BE553156A/xx unknown
-
1956
- 1956-11-27 US US624505A patent/US2980508A/en not_active Expired - Lifetime
- 1956-12-03 DE DET12948A patent/DE1041021B/de active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US1656572A (en) * | 1926-04-10 | 1928-01-17 | Firm I G Farbenindustrie Ag | Method of agglomerating pulverulent materials |
| US2125340A (en) * | 1936-01-09 | 1938-08-02 | Du Pont | Oxidation of titanous salts |
| US2149370A (en) * | 1936-01-09 | 1939-03-07 | Du Pont | Treatment of titanium liquors |
| US2339808A (en) * | 1940-03-16 | 1944-01-25 | Titan Co Inc | Process of treating ferrotitaniferous materials |
| US2589910A (en) * | 1949-03-24 | 1952-03-18 | New Jersey Zinc Co | Production of titanium dioxide |
| US2724636A (en) * | 1951-08-31 | 1955-11-22 | Nat Lead Co | Treatment of titaniferous ore concentrates to form titanium sulfate |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3252275A (en) * | 1961-08-23 | 1966-05-24 | Titan Gmbh | Apparatus for the agglomeration and separation of finely divided titanium dioxide from its gaseous vehicle |
| US3368870A (en) * | 1963-12-06 | 1968-02-13 | Soloducha Nicolas | Method of producing titanium hydroxide and high grade pigments produced therefrom |
| US3929962A (en) * | 1972-08-29 | 1975-12-30 | Chyn Duog Shiah | Titanium purification process |
| US3868441A (en) * | 1973-05-02 | 1975-02-25 | Ethyl Corp | Process for reducing trivalent titanium content in slag |
| US4325920A (en) * | 1980-11-12 | 1982-04-20 | Qit-Fer Et Titane Du Quebec, Inc. | Method to oxidize Ti+3 during the sulfuric acid digestion of titaniferous slags |
Also Published As
| Publication number | Publication date |
|---|---|
| DE1041021B (de) | 1958-10-16 |
| BE553156A (GUID-C5D7CC26-194C-43D0-91A1-9AE8C70A9BFF.html) |
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