CN103422122A - Method utilizing titanium dioxide to directly prepare metallic titanium - Google Patents
Method utilizing titanium dioxide to directly prepare metallic titanium Download PDFInfo
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- CN103422122A CN103422122A CN2013103854396A CN201310385439A CN103422122A CN 103422122 A CN103422122 A CN 103422122A CN 2013103854396 A CN2013103854396 A CN 2013103854396A CN 201310385439 A CN201310385439 A CN 201310385439A CN 103422122 A CN103422122 A CN 103422122A
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 134
- 239000004408 titanium dioxide Substances 0.000 title claims abstract description 63
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims abstract description 61
- 229910052719 titanium Inorganic materials 0.000 title claims abstract description 58
- 239000010936 titanium Substances 0.000 title claims abstract description 58
- 238000000034 method Methods 0.000 title claims abstract description 47
- 239000002608 ionic liquid Substances 0.000 claims abstract description 25
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000000843 powder Substances 0.000 claims abstract description 11
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 6
- 239000010439 graphite Substances 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000000463 material Substances 0.000 claims abstract description 3
- 229910052751 metal Inorganic materials 0.000 claims description 34
- 239000002184 metal Substances 0.000 claims description 34
- 239000000203 mixture Substances 0.000 claims description 22
- 238000005453 pelletization Methods 0.000 claims description 21
- 238000005868 electrolysis reaction Methods 0.000 claims description 20
- 238000002360 preparation method Methods 0.000 claims description 18
- 229910052799 carbon Inorganic materials 0.000 claims description 11
- 230000009467 reduction Effects 0.000 claims description 11
- 239000000428 dust Substances 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 8
- 239000008151 electrolyte solution Substances 0.000 claims description 8
- -1 1-butyl-3-methyl imidazolium tetrafluoroborate Chemical compound 0.000 claims description 4
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminum chloride Substances Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims description 4
- 125000001309 chloro group Chemical group Cl* 0.000 claims description 4
- IBZJNLWLRUHZIX-UHFFFAOYSA-N 1-ethyl-3-methyl-2h-imidazole Chemical compound CCN1CN(C)C=C1 IBZJNLWLRUHZIX-UHFFFAOYSA-N 0.000 claims description 2
- BTBUEUYNUDRHOZ-UHFFFAOYSA-N Borate Chemical compound [O-]B([O-])[O-] BTBUEUYNUDRHOZ-UHFFFAOYSA-N 0.000 claims description 2
- 230000008569 process Effects 0.000 abstract description 11
- 238000004519 manufacturing process Methods 0.000 abstract description 10
- 238000005265 energy consumption Methods 0.000 abstract description 5
- 238000009856 non-ferrous metallurgy Methods 0.000 abstract description 2
- 239000011230 binding agent Substances 0.000 abstract 2
- 239000003792 electrolyte Substances 0.000 abstract 1
- 150000003839 salts Chemical class 0.000 description 9
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 6
- 238000001354 calcination Methods 0.000 description 6
- 239000011777 magnesium Substances 0.000 description 6
- 229910052749 magnesium Inorganic materials 0.000 description 6
- 239000001301 oxygen Substances 0.000 description 6
- 229910052760 oxygen Inorganic materials 0.000 description 6
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 6
- IQQRAVYLUAZUGX-UHFFFAOYSA-N 1-butyl-3-methylimidazolium Chemical compound CCCCN1C=C[N+](C)=C1 IQQRAVYLUAZUGX-UHFFFAOYSA-N 0.000 description 5
- 230000004087 circulation Effects 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 229910052697 platinum Inorganic materials 0.000 description 3
- NJMWOUFKYKNWDW-UHFFFAOYSA-N 1-ethyl-3-methylimidazolium Chemical compound CCN1C=C[N+](C)=C1 NJMWOUFKYKNWDW-UHFFFAOYSA-N 0.000 description 2
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 2
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 description 2
- 229910003074 TiCl4 Inorganic materials 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- 239000000460 chlorine Substances 0.000 description 2
- 229910052801 chlorine Inorganic materials 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 description 2
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 1
- 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 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- LCKIEQZJEYYRIY-UHFFFAOYSA-N Titanium ion Chemical compound [Ti+4] LCKIEQZJEYYRIY-UHFFFAOYSA-N 0.000 description 1
- QGZNMXOKPQPNMY-UHFFFAOYSA-N [Mg].[Cl] Chemical compound [Mg].[Cl] QGZNMXOKPQPNMY-UHFFFAOYSA-N 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 239000001110 calcium chloride Substances 0.000 description 1
- 229910001628 calcium chloride Inorganic materials 0.000 description 1
- 235000011148 calcium chloride Nutrition 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000002659 electrodeposit Substances 0.000 description 1
- 238000004070 electrodeposition Methods 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229910052732 germanium Inorganic materials 0.000 description 1
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910001629 magnesium chloride Inorganic materials 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 238000011946 reduction process Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium(II) oxide Chemical compound [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 238000005292 vacuum distillation Methods 0.000 description 1
Abstract
The invention relates to a method utilizing titanium dioxide to directly prepare metallic titanium, and belongs to the technical field of nonferrous metallurgy. The method includes the steps that titanium dioxide powder, carbon powder and binding agents are uniformly mixed to prepare a prereduction titanium dioxide electrode, wherein the binding agents are water or PVA; then, the prereduction titanium dioxide electrode is used as the cathode, graphite or other inert materials are used as the anode, electroreduction is conducted for 12-48 h under the condition that an electrolyte is ionic liquid, the electrolytic voltage is 2.8-3.2 V and the electrolytic temperature is 25-120 DEG C, and then the cathode is taken out, flushed and dried to obtain the cathode product metallic titanium. By the adoption of the method, the technological process is shortened, energy consumption is greatly reduced, and clean production is achieved.
Description
Technical field
The present invention relates to a kind of method of titanium dioxide direct Preparation of Titanium, belong to the non-ferrous metallurgy technology field.
Background technology
Titanium has that specific tenacity is large, density is little, high temperature resistant, anticorrosive, be widely used in the fields such as space flight, oil, the energy, traffic, chemical industry, biomedicine without the performance of the excellences such as magnetic, and constantly expansion of its Application Areas.
The production method of titanium mainly contains two kinds at present: magnesium reduction process (Kroll method) and sodium thermoreduction method (Hunter method).Because the Hunter method is higher than Kroll method production cost, so titanium production generally used, be the Kroll method.The Kroll method is to take the titanium sponge production technique that magnesium reduction-vacuum distillation method is representative.It,, by titanium ore enrichment-chlorination-produce TiCl4, then is reduced to titanium sponge with magnesium by TiCl4 in argon gas or helium atmosphere, then carries out vacuum distilling and separates and remove magnesium and MgCl2, finally by crossing product treatment, obtains the finished product titanium sponge.Two important circulations are arranged in this technical process, i.e. magnesium circulation and chlorine circulation, and the outer circulation of magnesium and chlorine circulation obtain by high-temperature molten salt electrolytic chlorine magnesium.Therefore this technical process is long, complicated operation, and production cost is high, and environmental pollution is serious.Through the development of decades, the Kroll method has also been carried out a series of improvement, but research work for many years proves, some local technique improvements can't change expensive this present situation.Therefore, be necessary to study that flow process is short, cost is low and environment amenable preparation method, and metal titanium can be applied in more field.For seeking the new preparation technology of titanium cheaply, all done a large amount of research work both at home and abroad.The novel process of research has fused salt electrolysis process (FFC method).At first the method is fired into negative electrode by TiO2, then adopts CaCl2 high-temperature molten salt system as ionogen, under 800～1000 ℃, by its electrolytic reduction, is directly metal titanium.Because this method directly obtains metal titanium from the TiO2 electrolysis, greatly simplified technical process and equipment, therefore can obviously reduce energy consumption and production costs (according to estimates, the production cost of this method be only the Kroll method 1/3rd).But; up to the present the method just succeeds in laboratory; realize scale operation; at first to solve the preparation of TiO2 negative electrode and the bad problem of electroconductibility; its less important airtight and atmosphere protection of realizing electrolyzer, then also must overcome the impact of titanium ion variation of valence on current efficiency in electrolytic process.And will overcome the above problems, also have in practice very large difficulty. simultaneouslyAnd fused salt electrolysis will carry out at the temperature of 800 ℃, need to consume certain energy etching apparatus.Therefore, in the urgent need to developing, a kind of technique is simple, energy-conservation, titanium new preparation technology cheaply, and the appearance of ionic liquid provides new possibility undoubtedly for this reason.
Ionic liquid is the abbreviation of ionic liquid at room temperature, is a kind ofly to be comprised of the yin, yang ion organic salt be in a liquid state at room temperature or near room temperature.It has that electrochemical window is wide, good conductivity, liquid wide ranges, without excellent properties such as vapour pressure, good stabilities, be a kind of green solvent.Aspect galvanic deposit, ionic liquid has merged the advantage of high-temperature molten salt and the aqueous solution: have wider electrochemical window and good electroconductibility, at room temperature can obtain the ability galvanic deposit goes out in high-temperature molten salt metal and alloy, but there is no the such severe corrosive of high-temperature molten salt; Go back electrodepositable in ionic liquid and obtain most of metals that can obtain simultaneously in the aqueous solution, and without side reaction, thereby the metal quality obtained is better, current efficiency is higher, and the metal and the alloy thereof that particularly aluminium, titanium, silicon and germanium etc. are difficult to obtain at aqueous solution electrodeposition are all the more so.The above-mentioned characteristic of ionic liquid and good specific conductivity thereof make it to become the brand-new liquid of galvanic deposit research, aspect electrodeposit metals, are more and more applied.
Summary of the invention
For problem and the deficiency of above-mentioned prior art existence, the invention provides a kind of method of titanium dioxide direct Preparation of Titanium.With existing metal titanium preparation method, compare, the present invention has shortened technical process, has greatly reduced energy consumption, realizes cleaner production, and the present invention is achieved through the following technical solutions.
A kind of method of titanium dioxide direct Preparation of Titanium, its concrete steps are as follows:
(1) prepare the prereduction titanium dioxide electrodes: at first by titanium dioxide powder, carbon dust and PVA according to mass percent 100:(12～16): (1～2) mixes and is pressed into block mixture, calcines 1～4h under the condition that is then 1200～1300 ℃ by block mixture in temperature and obtain the prereduction titanium dioxide electrodes in reducing atmosphere; Or at first by titanium dioxide powder, water and carbon dust according to mass percent 100:(6～10): (12～16) mix and are pressed into the pelletizing shape mixture that diameter is 1～10mm, then calcine 1～2h under the condition that is 1200～1300 ℃ by pelletizing shape mixture in temperature and obtain prereduction titanium dioxide pelletizing in reducing atmosphere, in the titanium basket of finally pelletizing being packed into, obtain the prereduction titanium dioxide electrodes;
(2) prepare metal titanium: the prereduction titanium dioxide electrodes that the step (1) of take obtains is negative electrode, graphite or other inert material are anode, at electrolytic solution, be that ionic liquid, electrolysis voltage are to carry out electrolytic reduction 12～48h under 2.8～3.2V, the electrolysis temperature condition that is 25～120 ℃, then take out negative electrode, rinse and be drying to obtain the cathode product metal titanium.
The mesh order number of described titanium basket is 100～200 orders.
Described ionic liquid is alkaline chloro 1-butyl-3-Methylimidazole-aluminum chloride (BmimCl-AlCl
3), alkaline chloro 1-ethyl-3-methylimidazole-aluminum chloride (EmimCl-AlCl
3), 1-butyl-3-methyl imidazolium tetrafluoroborate ([Bmim] BF
4), 1-ethyl-3-methylimidazole a tetrafluoro borate ([Emim] BF
4) or 1-butyl-3-Methylimidazole hexafluorophosphate ([Bmim] PF
6).
Above-mentioned ionic liquid is all commercial analytical pure.
The invention has the beneficial effects as follows: (1) the present invention directly is converted into metal titanium by titanium dioxide, and product metal titanium oxygen level is lower, and compares with traditional metal titanium production method, and the present invention has shortened technical process, greatly reduced energy consumption; (2) with the FCC method of existing research, compare, electrolytic reduction temperature of the present invention is low, adopts ionic liquid electrolytic reduction temperature below 130 ℃, and the high temperature fused salt electrolysis temperature is more than 800 ℃, reduced by 670 ℃, to a great extent cost-saving, reduced energy consumption and slowed down the corrosion to equipment; (3) due to the titanium dioxide poorly conductive, the present invention calcines titanium dioxide under the carbon reducing atmosphere, make the deoxidation of titania molecule part become semi-conductor, improve the electroconductibility of negative electrode, improve the electrochemical deoxidising efficiency in electrolytic process, and negative electrode titanium dioxide is adopted to the pelletizing shape, can further accelerate speed of reaction, improve electrochemical deoxidising efficiency.
Embodiment
Below in conjunction with embodiment, the invention will be further described.
Embodiment 1
The method of this titanium dioxide direct Preparation of Titanium, its concrete steps are as follows:
(1) prepare the prereduction titanium dioxide electrodes: at first titanium dioxide powder, carbon dust and PVA are mixed and be pressed into block mixture according to mass percent 100:16:2, under the condition that is then 1200 ℃ by block mixture in temperature in reducing atmosphere, calcining 1h obtains the prereduction titanium dioxide electrodes;
(2) prepare metal titanium: the prereduction titanium dioxide electrodes that the step (1) of take obtains is negative electrode, graphite is anode, at electrolytic solution, be that ionic liquid, electrolysis voltage are to carry out electrolytic reduction 12h under 2.8V, the electrolysis temperature condition that is 25 ℃, then take out negative electrode, rinse and be drying to obtain the cathode product metal titanium.Wherein ionic liquid is [Bmim] Cl-AlCl
3, the oxygen level of metal titanium is less than 1%.
Embodiment 2
The method of this titanium dioxide direct Preparation of Titanium, its concrete steps are as follows:
(1) prepare the prereduction titanium dioxide electrodes: at first titanium dioxide powder, carbon dust and PVA are mixed and be pressed into block mixture according to mass percent 100:12:1, under the condition that is then 1300 ℃ by block mixture in temperature in reducing atmosphere, calcining 4h obtains the prereduction titanium dioxide electrodes;
(2) prepare metal titanium: the prereduction titanium dioxide electrodes that the step (1) of take obtains is negative electrode, platinum electrode is anode, at electrolytic solution, be that ionic liquid, electrolysis voltage are to carry out electrolytic reduction 48h under 3.2V, the electrolysis temperature condition that is 120 ℃, then take out negative electrode, rinse and be drying to obtain the cathode product metal titanium.Wherein ionic liquid is [Bmim] BF
4, the oxygen level of metal titanium is less than 1%.
Embodiment 3
The method of this titanium dioxide direct Preparation of Titanium, its concrete steps are as follows:
(1) prepare the prereduction titanium dioxide electrodes: at first titanium dioxide powder, carbon dust and PVA are mixed and be pressed into block mixture according to mass percent 100:14:1, under the condition that is then 1250 ℃ by block mixture in temperature in reducing atmosphere, calcining 2h obtains the prereduction titanium dioxide electrodes;
(2) prepare metal titanium: the prereduction titanium dioxide electrodes that the step (1) of take obtains is negative electrode, graphite is anode, at electrolytic solution, be that ionic liquid, electrolysis voltage are to carry out electrolytic reduction 24h under 3.0V, the electrolysis temperature condition that is 100 ℃, then take out negative electrode, rinse and be drying to obtain the cathode product metal titanium.Wherein ionic liquid is EmimCl-AlCl
3, the oxygen level of metal titanium is less than 1%.
Embodiment 4
The method of this titanium dioxide direct Preparation of Titanium, its concrete steps are as follows:
(1) prepare the prereduction titanium dioxide electrodes: at first titanium dioxide powder, water and carbon dust are mixed and be pressed into according to mass percent 100:10:16 the pelletizing shape mixture that diameter is 1mm, then under the condition that is 1200 ℃ by pelletizing shape mixture in temperature in reducing atmosphere, calcining 1h obtains the titanium dioxide pelletizing of prereduction, in the mesh 100 purpose titanium baskets with electroconductibility of finally pelletizing being packed into, obtains the prereduction titanium dioxide electrodes;
(2) prepare metal titanium: the prereduction titanium dioxide electrodes that the step (1) of take obtains is negative electrode, platinum electrode is anode, at electrolytic solution, be that ionic liquid, electrolysis voltage are to carry out electrolytic reduction 12h under 2.8V, the electrolysis temperature condition that is 25 ℃, then take out negative electrode, rinse and be drying to obtain the cathode product metal titanium.Wherein ionic liquid is BmimCl-AlCl
3, the oxygen level of metal titanium is less than 1%.
Embodiment 5
The method of this titanium dioxide direct Preparation of Titanium, its concrete steps are as follows:
(1) prepare the prereduction titanium dioxide electrodes: at first titanium dioxide powder, water and carbon dust are mixed and be pressed into according to mass percent 100:6:12 the pelletizing shape mixture that diameter is 10mm, then under the condition that is 1300 ℃ by pelletizing shape mixture in temperature in reducing atmosphere, calcining 2h obtains the titanium dioxide pelletizing of prereduction, in the mesh 200 purpose titanium baskets with electroconductibility of finally pelletizing being packed into, obtains the prereduction titanium dioxide electrodes;
(2) prepare metal titanium: the prereduction titanium dioxide electrodes that the step (1) of take obtains is negative electrode, graphite is anode, at electrolytic solution, be that ionic liquid, electrolysis voltage are to carry out electrolytic reduction 48h under 3.2V, the electrolysis temperature condition that is 120 ℃, then take out negative electrode, rinse and be drying to obtain the cathode product metal titanium.Wherein ionic liquid is [Emim] BF
4, the oxygen level of metal titanium is less than 1%.
Embodiment 6
The method of this titanium dioxide direct Preparation of Titanium, its concrete steps are as follows:
(1) prepare the prereduction titanium dioxide electrodes: at first titanium dioxide powder, water and carbon dust are mixed and be pressed into according to mass percent 100:8:14 the pelletizing shape mixture that diameter is 5mm, then under the condition that is 1250 ℃ by pelletizing shape mixture in temperature in reducing atmosphere, calcining 1.5h obtains the titanium dioxide pelletizing of prereduction, in the mesh 120 purpose titanium baskets with electroconductibility of finally pelletizing being packed into, obtains the prereduction titanium dioxide electrodes;
(2) prepare metal titanium: the prereduction titanium dioxide electrodes that the step (1) of take obtains is negative electrode, platinum electrode is anode, at electrolytic solution, be that ionic liquid, electrolysis voltage are to carry out electrolytic reduction 24h under 3.0V, the electrolysis temperature condition that is 100 ℃, then take out negative electrode, rinse and be drying to obtain the cathode product metal titanium.Wherein ionic liquid is [Bmim] PF
6, the oxygen level of metal titanium is less than 1%.
Claims (3)
1. the method for a titanium dioxide direct Preparation of Titanium is characterized in that concrete steps are as follows:
(1) prepare the prereduction titanium dioxide electrodes: at first by titanium dioxide powder, carbon dust and PVA according to mass percent 100:(12～16): (1～2) mixes and is pressed into block mixture, calcines 1～4h under the condition that is then 1200～1300 ℃ by block mixture in temperature and obtain the prereduction titanium dioxide electrodes in reducing atmosphere; Or at first by titanium dioxide powder, water and carbon dust according to mass percent 100:(6～10): (12～16) mix and are pressed into the pelletizing shape mixture that diameter is 1～10mm, then calcine 1～2h under the condition that is 1200～1300 ℃ by pelletizing shape mixture in temperature and obtain prereduction titanium dioxide pelletizing in reducing atmosphere, in the titanium basket of finally pelletizing being packed into, obtain the prereduction titanium dioxide electrodes;
(2) prepare metal titanium: the prereduction titanium dioxide electrodes that the step (1) of take obtains is negative electrode, graphite or other inert material are anode, at electrolytic solution, be that ionic liquid, electrolysis voltage are to carry out electrolytic reduction 12～48h under 2.8～3.2V, the electrolysis temperature condition that is 25～120 ℃, then take out negative electrode, rinse and be drying to obtain the cathode product metal titanium.
2. the method for titanium dioxide direct Preparation of Titanium according to claim 1, it is characterized in that: the mesh order number of described titanium basket is 100～200 orders.
3. the method for titanium dioxide direct Preparation of Titanium according to claim 1, it is characterized in that: described ionic liquid is alkaline chloro 1-butyl-3-Methylimidazole-aluminum chloride, alkaline chloro 1-ethyl-3-methylimidazole-aluminum chloride, 1-butyl-3-methyl imidazolium tetrafluoroborate, 1-ethyl-3-methylimidazole a tetrafluoro borate or 1-butyl-3-Methylimidazole hexafluorophosphate.
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| CN104131312A (en) * | 2014-07-08 | 2014-11-05 | 昆明理工大学 | Method utilizing eutectic solvent to carry out in-situ reduction on lead oxide to produce lead |
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| CN104451781A (en) * | 2014-12-08 | 2015-03-25 | 中国铝业股份有限公司 | Preparation method of anode for producing metallic titanium by electrolysis |
| CN115161714A (en) * | 2022-08-01 | 2022-10-11 | 青岛国韬钛金属产业研究院有限公司 | Method for preparing metal titanium by molten salt solid-state deoxidation method |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104131312A (en) * | 2014-07-08 | 2014-11-05 | 昆明理工大学 | Method utilizing eutectic solvent to carry out in-situ reduction on lead oxide to produce lead |
| CN104213151A (en) * | 2014-09-05 | 2014-12-17 | 昆明理工大学 | Method for preparing lead-antimony alloy by directly electrolyzing lead-antimony oxide |
| CN104213151B (en) * | 2014-09-05 | 2017-05-10 | 昆明理工大学 | Method for preparing lead-antimony alloy by directly electrolyzing lead-antimony oxide |
| CN104451781A (en) * | 2014-12-08 | 2015-03-25 | 中国铝业股份有限公司 | Preparation method of anode for producing metallic titanium by electrolysis |
| CN115161714A (en) * | 2022-08-01 | 2022-10-11 | 青岛国韬钛金属产业研究院有限公司 | Method for preparing metal titanium by molten salt solid-state deoxidation method |
| CN115161714B (en) * | 2022-08-01 | 2023-07-18 | 青岛国韬钛金属产业研究院有限公司 | Method for preparing metallic titanium by molten salt solid-state deoxidization method |
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