US1695341A - Method of obtaining titanium oxide - Google Patents
Method of obtaining titanium oxide Download PDFInfo
- Publication number
- US1695341A US1695341A US121058A US12105826A US1695341A US 1695341 A US1695341 A US 1695341A US 121058 A US121058 A US 121058A US 12105826 A US12105826 A US 12105826A US 1695341 A US1695341 A US 1695341A
- Authority
- US
- United States
- Prior art keywords
- titanium
- iron
- titanium oxide
- acid
- temperature
- 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
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- 238000000034 method Methods 0.000 title description 19
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title description 13
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 title description 13
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 30
- 239000010936 titanium Substances 0.000 description 21
- 229910052719 titanium Inorganic materials 0.000 description 21
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 20
- 229910052742 iron Inorganic materials 0.000 description 15
- 239000002253 acid Substances 0.000 description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 13
- 239000000203 mixture Substances 0.000 description 12
- 238000010438 heat treatment Methods 0.000 description 10
- 239000000243 solution Substances 0.000 description 10
- 239000012141 concentrate Substances 0.000 description 9
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 8
- 150000001875 compounds Chemical class 0.000 description 8
- 238000002156 mixing Methods 0.000 description 8
- 239000007787 solid Substances 0.000 description 8
- 239000001117 sulphuric acid Substances 0.000 description 8
- 235000011149 sulphuric acid Nutrition 0.000 description 8
- 229910052936 alkali metal sulfate Inorganic materials 0.000 description 7
- 238000001816 cooling Methods 0.000 description 7
- 239000002904 solvent Substances 0.000 description 6
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 4
- 229910052783 alkali metal Inorganic materials 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 230000001376 precipitating effect Effects 0.000 description 4
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 4
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 3
- 150000001340 alkali metals Chemical class 0.000 description 3
- 230000008030 elimination Effects 0.000 description 3
- 238000003379 elimination reaction Methods 0.000 description 3
- 230000004927 fusion Effects 0.000 description 3
- 230000007062 hydrolysis Effects 0.000 description 3
- 238000006460 hydrolysis reaction Methods 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 229910021653 sulphate ion Inorganic materials 0.000 description 3
- 150000003609 titanium compounds Chemical class 0.000 description 3
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 2
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 2
- 230000003301 hydrolyzing effect Effects 0.000 description 2
- -1 ilmenite Chemical compound 0.000 description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- 239000011707 mineral Substances 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 239000003513 alkali Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000002845 discoloration Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 159000000014 iron salts Chemical class 0.000 description 1
- YDZQQRWRVYGNER-UHFFFAOYSA-N iron;titanium;trihydrate Chemical compound O.O.O.[Ti].[Fe] YDZQQRWRVYGNER-UHFFFAOYSA-N 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical group [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- WBHQBSYUUJJSRZ-UHFFFAOYSA-M sodium bisulfate Chemical compound [Na+].OS([O-])(=O)=O WBHQBSYUUJJSRZ-UHFFFAOYSA-M 0.000 description 1
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 235000011152 sodium sulphate Nutrition 0.000 description 1
- 150000003608 titanium Chemical class 0.000 description 1
- 239000012463 white pigment Substances 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
- C22B34/1259—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 treatment or purification of titanium containing solutions or liquors or slurries
Definitions
- This invention relates to the treatment of minerals and products thereof containing titanium, such as ilmenite, rutile after the elimination of impurities and a large portion of the iron content, and particularly titanium concentrates such as are obtained by the process described in U. S. Patent No. 1,543,250,
- the object of my invention is to convert such refractory compoundsof titanium into a water soluble compound, or compounds.
- This I propose to do ,by the use of a mixture of sulphuric acid with an alkali metaLsulphate, at a temperature lower than that at tanium oxide especially suited for use as a.
- the solution obtained by my invention possesses new and desirable qualities whereby is assured the precipitation of titanium compounds entirely free from ims purities, such as iron, which causes discoloration of the final product.
- the solution obtained is novel in itself, as hydrolysis may be carried out at a very low temperature. Providing the iron present has previously been reduced to the ferrous state, the compound of titanium obtained on hydrolysis is entirely free from impurities.
- the temperature employed is so low that the ferrous iron is not oxidized during the process, and no hydrolysis of iron salts takes place.
- the melt obtained from the employment of such substances as concentrated sulphuric acid or sodium bisulphate, or combinations of these two, does not produce a large proportion of water soluble sulphates if a high temperature is used.
- WVhen rutile, or other refractory minerals and products thereof have been subjected to a temperature around 1000 C.
- the process of direct treatment with concentrated sulphuric acid decomposes only a small percentage of the titanium present, and fusion of the residue at comparatively high temperatures with salts of alkali metals does not result in the production of a large percentage of titanium compounds soluble in water.
- This invention relates to a process in which one continuous operation only is carried out at a temperature much lower than is required when an alkali metal salt is used alone. .Furthermore, no other addition of acid is required in order to bring the titanium into aqueous solution.
- the process differs from that using sulphuric acid only, as in addition to sul-' phuric acid large quantities of sodium sulphate are employed.
- the acid alone reacts with only a small percentage of the titanium present,whereas the use of the sodium acid sulphate and sulphuric acid mixture, as described, effects acomplete decomposition of the titanium oxides.
- the process differs from fusion with acid alkali metal sulphates-alone, since in addition to such sulphates, sulphuric acid is also employed, and during the treatment the op-' timum temperature leading to the formation of soluble titanium compound is employed. This temperature is about 160 C. below that at which the sodium acid sulphate fuses,
- l Vhat I claim is i 1.
- the method of converting refractory compounds of titanium after the elimination of impurities and a large portion of the iron content into'water soluble sulphates comprising mixing'the comminuted compound with an alkali-metal sulphate and an acid solvent, heating the mixture at a temperature from 120 to 000 C., until a solid cake is formed, cooling and crushing the cake.
- the method of obtaining titanium oxide from concentrates containing titanium and iron which comprises, mixing the comminuted material with an alkali-metal sulphate and an acid solvent, heating the mixture at a temperature from 120 to 300 C. until a solid cake is formed, cooling and crushing the cake and lixiviating with cold water, and
- the method of obtaining titanium oxide from concentrates containing titanium and iron which comprises, mixing the comminuted substance with an alkali-metal sulphate and an acid solvent, heating the mixture below 140 C. transferring the mass to a tray and raising the temperature to about 260 C. until a solid cake is formed, cooling and crushing the cake, lixiviating with cold water and precipitating the titanium oxide from the solution.
- the method of obtaining titanium oxide from concentrates containing titanium and iron which comprises, mixing the comminuted substance with an alkali-metal sulphate and an acid solvent, heating the mixture below 140 C. transferring the mass to a tray and raising the temperature to about 260 C. until a solid cake is formed, cooling and crushing the cake, lixiviating with cold water, reducing the iron to the ferrous state and precipitating'the titanium oxide from the solution.
- the method of obtaining titanium oxide from concentrates containing titanium and iron which comprises, mixing the comminuted material with approximately one and one half times by weight of an alkalianeta] sulphate and double the weight of sulphuric acid, heating the mixture to below 140 C. until it begins to solidify, heating on a fiat tray up to 260 C. till a solid cake is formed, cooling and crushing the cake and then lixiviating withcold water and precipitating the titanium oxidefrom the solution.
- the method of obtaining titanium oxide from concentrates containing titanium and iron which comprises, mixing the comminuted, material with approximately one and a half times by weight of an alkali-metal sulphateand double the weight of sulphuric acid, heating the mixture to below 140 C. until it begins to solidify, heating on a flat tray up to 260 C. till a solid cake is formed, coolingand crushing the cake and then lixiviating with cold water and hydrolyzing the solution at not over C. and gradually to about 95 C.
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- Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Description
Patented Dec. 18, 1 928.
UNITED STATES PATENT OFFICE.
REGINALD-HILL MONK, OF MONTREAL, QUEBEC, CANADA.
METHOD OF OBTAINING TITANIUM OXIDE.
No Drawing.
This invention relates to the treatment of minerals and products thereof containing titanium, such as ilmenite, rutile after the elimination of impurities and a large portion of the iron content, and particularly titanium concentrates such as are obtained by the process described in U. S. Patent No. 1,543,250,
16th June 1925.
The object of my invention is to convert such refractory compoundsof titanium into a water soluble compound, or compounds. This I propose to do ,by the use of a mixture of sulphuric acid with an alkali metaLsulphate, at a temperature lower than that at tanium oxide especially suited for use as a.
white pigment. The solution obtained by my invention possesses new and desirable qualities whereby is assured the precipitation of titanium compounds entirely free from ims purities, such as iron, which causes discoloration of the final product. a
The solution obtained is novel in itself, as hydrolysis may be carried out at a very low temperature. Providing the iron present has previously been reduced to the ferrous state, the compound of titanium obtained on hydrolysis is entirely free from impurities.
' The temperature employed is so low that the ferrous iron is not oxidized during the process, and no hydrolysis of iron salts takes place.
I am aware that various patents have been granted for the sulphating of titanium ores and the products thereof, but these processes are invariably carried out at relatively high temperatures at which fusion occurs.
The melt obtained from the employment of such substances as concentrated sulphuric acid or sodium bisulphate, or combinations of these two, does not produce a large proportion of water soluble sulphates if a high temperature is used.
This is more particularly shown in the case of the above mentioned titanium concentrates obtainedby the process described in Letters Patent No. 1,543,250.
Application filed July 7, 1926. Serial No. 121,058.
WVhen rutile, or other refractory minerals and products thereof, have been subjected to a temperature around 1000 C. the process of direct treatment with concentrated sulphuric acid decomposes only a small percentage of the titanium present, and fusion of the residue at comparatively high temperatures with salts of alkali metals does not result in the production of a large percentage of titanium compounds soluble in water.
This invention relates to a process in which one continuous operation only is carried out at a temperature much lower than is required when an alkali metal salt is used alone. .Furthermore, no other addition of acid is required in order to bring the titanium into aqueous solution. The process differs from that using sulphuric acid only, as in addition to sul-' phuric acid large quantities of sodium sulphate are employed. The acid alone reacts with only a small percentage of the titanium present,whereas the use of the sodium acid sulphate and sulphuric acid mixture, as described, effects acomplete decomposition of the titanium oxides.
The process differs from fusion with acid alkali metal sulphates-alone, since in addition to such sulphates, sulphuric acid is also employed, and during the treatment the op-' timum temperature leading to the formation of soluble titanium compound is employed. This temperature is about 160 C. below that at which the sodium acid sulphate fuses,
which'is 300 C.
Furthermore, practically no acid isdriven off, and the titanium is entirely solublein water without any addition of acid. At the low temperature employed no alkali titanites are formed. v
In order to fully describe my invention I state the following example: a
From a titanium concentrate, obtained by the process described in Patent N 0. 1,543,250, containing 19.93% total iron, .7 metallic iron, and 54.62% TiO I take 400 grams, mix this with 600 grams of NaI-ISO and 840 grams H 66.43%. This mixture is now heated to 120 (3., being agitated the meanwhile. The mass is kept-below 140 C. for three hours. When it shows a tendency to solidify it is transferred on to a flat tray,
ously reduced to the ferrous state.
Resulting solution contains:
Grams pcrlitre.
no, 71.2 S0 80ml)"; 33 Na S 4 99 perature gradually, and finally bring it up to 95 (1., or thereabouts, for the last 20 to 30 minutes. I In this manner a pure compound of titanium is precipitated, and all the iron is kept in solution.
l Vhat I claim is i 1. The method of converting refractory compounds of titanium after the elimination of impurities and a large portion of the iron content into'water soluble sulphates, comprising mixing'the comminuted compound with an alkali-metal sulphate and an acid solvent, heating the mixture at a temperature from 120 to 000 C., until a solid cake is formed, cooling and crushing the cake.
2. The method of. converting refractory compounds of titanium after the elimination of impurities and a large portion of the iron content into water soluble sulphates, comprising mixing the comminuted compound with an alkali-metal sulphate and an acid solvent, heating the mixture at first below 140 C. transferring to a tray and raising the temperature to about 260 C. until a solid cake is formed, cooling and crushing the cake and lixiviatin'g with cold water.
The method of obtaining titanium oxide from concentrates containing titanium and iron which comprises, mixing the comminuted material with an alkali-metal sulphate and an acid solvent, heating the mixture at a temperature from 120 to 300 C. until a solid cake is formed, cooling and crushing the cake and lixiviating with cold water, and
precipitating the titanium oxide from the solution.
4. The method of obtaining titanium oxide from concentrates containing titanium and iron which comprises mixing the comreoaeai minuted material with an alkali-metal sulphate and an acid solvent, heating the mixture at a temperature from 120 to 300 C. until a solid cake is formed, cooling and crushing the cake, lixiviating with cold water and hydrolyzing the solution at a low temperature.
5. The method of obtaining titanium oxide from concentrates containing titanium and iron which comprises, mixing the comminuted substance with an alkali-metal sulphate and an acid solvent, heating the mixture below 140 C. transferring the mass to a tray and raising the temperature to about 260 C. until a solid cake is formed, cooling and crushing the cake, lixiviating with cold water and precipitating the titanium oxide from the solution. p
6. The method of obtaining titanium oxide from concentrates containing titanium and iron which comprises, mixing the comminuted substance with an alkali-metal sulphate and an acid solvent, heating the mixture below 140 C. transferring the mass to a tray and raising the temperature to about 260 C. until a solid cake is formed, cooling and crushing the cake, lixiviating with cold water, reducing the iron to the ferrous state and precipitating'the titanium oxide from the solution.
7 The method of obtaining titanium oxide from concentrates containing titanium and iron which comprises, mixing the comminuted material with approximately one and one half times by weight of an alkalianeta] sulphate and double the weight of sulphuric acid, heating the mixture to below 140 C. until it begins to solidify, heating on a fiat tray up to 260 C. till a solid cake is formed, cooling and crushing the cake and then lixiviating withcold water and precipitating the titanium oxidefrom the solution.
8. The method of obtaining titanium oxide from concentrates containing titanium and iron which comprises, mixing the comminuted, material with approximately one and a half times by weight of an alkali-metal sulphateand double the weight of sulphuric acid, heating the mixture to below 140 C. until it begins to solidify, heating on a flat tray up to 260 C. till a solid cake is formed, coolingand crushing the cake and then lixiviating with cold water and hydrolyzing the solution at not over C. and gradually to about 95 C.
REGINALD HILL MONKI
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US121058A US1695341A (en) | 1926-07-07 | 1926-07-07 | Method of obtaining titanium oxide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US121058A US1695341A (en) | 1926-07-07 | 1926-07-07 | Method of obtaining titanium oxide |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| US1695341A true US1695341A (en) | 1928-12-18 |
Family
ID=22394220
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| US121058A Expired - Lifetime US1695341A (en) | 1926-07-07 | 1926-07-07 | Method of obtaining titanium oxide |
Country Status (1)
| Country | Link |
|---|---|
| US (1) | US1695341A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5591506A (en) * | 1995-05-10 | 1997-01-07 | Kemicraft Overseas Limited | Non-polluting alkali-metal bisulfate system for producing titanium dioxide pigment |
-
1926
- 1926-07-07 US US121058A patent/US1695341A/en not_active Expired - Lifetime
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5591506A (en) * | 1995-05-10 | 1997-01-07 | Kemicraft Overseas Limited | Non-polluting alkali-metal bisulfate system for producing titanium dioxide pigment |
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