CN115710731A - Method for preparing metal titanium by utilizing electrolytic separation of aluminum-titanium alloy - Google Patents
Method for preparing metal titanium by utilizing electrolytic separation of aluminum-titanium alloy Download PDFInfo
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- 239000010936 titanium Substances 0.000 title claims abstract description 69
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims abstract description 52
- 238000000034 method Methods 0.000 title claims abstract description 51
- 229910052719 titanium Inorganic materials 0.000 title claims abstract description 46
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 38
- 239000002184 metal Substances 0.000 title claims abstract description 37
- 229910001069 Ti alloy Inorganic materials 0.000 title claims abstract description 30
- UQZIWOQVLUASCR-UHFFFAOYSA-N alumane;titanium Chemical compound [AlH3].[Ti] UQZIWOQVLUASCR-UHFFFAOYSA-N 0.000 title claims abstract description 26
- 238000000926 separation method Methods 0.000 title claims abstract description 9
- 238000005868 electrolysis reaction Methods 0.000 claims abstract description 40
- 229910010038 TiAl Inorganic materials 0.000 claims abstract description 29
- 239000000203 mixture Substances 0.000 claims abstract description 24
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 17
- 230000008569 process Effects 0.000 claims abstract description 17
- 239000003792 electrolyte Substances 0.000 claims abstract description 13
- 230000009467 reduction Effects 0.000 claims abstract description 12
- 150000003839 salts Chemical class 0.000 claims abstract description 12
- 229910000838 Al alloy Inorganic materials 0.000 claims abstract description 11
- 239000010405 anode material Substances 0.000 claims abstract description 8
- 239000012535 impurity Substances 0.000 claims abstract description 5
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 18
- 239000011734 sodium Substances 0.000 claims description 13
- 238000004519 manufacturing process Methods 0.000 claims description 12
- 238000006243 chemical reaction Methods 0.000 claims description 11
- 229910052593 corundum Inorganic materials 0.000 claims description 10
- 239000010431 corundum Substances 0.000 claims description 10
- 229910016569 AlF 3 Inorganic materials 0.000 claims description 9
- 229910052708 sodium Inorganic materials 0.000 claims description 9
- 239000011780 sodium chloride Substances 0.000 claims description 9
- 238000001704 evaporation Methods 0.000 claims description 8
- 230000008020 evaporation Effects 0.000 claims description 6
- 239000010439 graphite Substances 0.000 claims description 6
- 229910002804 graphite Inorganic materials 0.000 claims description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 5
- 239000010406 cathode material Substances 0.000 claims description 5
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical group 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 claims description 4
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 4
- 239000011591 potassium Substances 0.000 claims description 4
- 229910052700 potassium Inorganic materials 0.000 claims description 4
- 239000003638 chemical reducing agent Substances 0.000 claims description 3
- 239000000126 substance Substances 0.000 abstract description 7
- 239000006227 byproduct Substances 0.000 abstract description 4
- 238000009835 boiling Methods 0.000 abstract description 3
- 238000007670 refining Methods 0.000 abstract description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 abstract 1
- 238000007133 aluminothermic reaction Methods 0.000 abstract 1
- 229910001610 cryolite Inorganic materials 0.000 abstract 1
- 229910052782 aluminium Inorganic materials 0.000 description 7
- 230000006872 improvement Effects 0.000 description 6
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 description 4
- 238000005265 energy consumption Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 description 4
- 229910000831 Steel Inorganic materials 0.000 description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 3
- 229910045601 alloy Inorganic materials 0.000 description 3
- 239000000956 alloy Substances 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 238000005660 chlorination reaction Methods 0.000 description 3
- 239000000460 chlorine Substances 0.000 description 3
- 239000011777 magnesium Substances 0.000 description 3
- 229910052749 magnesium Inorganic materials 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 238000011946 reduction process Methods 0.000 description 3
- 239000010959 steel Substances 0.000 description 3
- 229910018575 Al—Ti Inorganic materials 0.000 description 2
- 238000003723 Smelting Methods 0.000 description 2
- 229910010413 TiO 2 Inorganic materials 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 2
- 229910001629 magnesium chloride Inorganic materials 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 229910052720 vanadium Inorganic materials 0.000 description 2
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 1
- 235000015842 Hesperis Nutrition 0.000 description 1
- 235000012633 Iberis amara Nutrition 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 238000010894 electron beam technology Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000010310 metallurgical process Methods 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 238000005065 mining Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000003832 thermite Substances 0.000 description 1
- NMJKIRUDPFBRHW-UHFFFAOYSA-N titanium Chemical compound [Ti].[Ti] NMJKIRUDPFBRHW-UHFFFAOYSA-N 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
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- Manufacture And Refinement Of Metals (AREA)
- Electrolytic Production Of Metals (AREA)
Abstract
The invention discloses a method for preparing metallic titanium by utilizing an electrolytic separation aluminum-titanium alloy, and mainly relates to a method for refining spongy TiAl and TiAl by using fluotitanate through an aluminothermic reduction method 3 、Ti 3 Al alloy or its mixture, fluotitanate evaporated at high temp, and other low-boiling impurities not reacted completely. Spongy TiAl and TiAl prepared by aluminothermic reaction through molten salt electrolysis method 3 、Ti 3 Al alloy or its mixture is used as anode material, molten salt of cryolite and chloride system is used as electrolyte, al in the anode is separated out by electrolysis, high-purity metal Al is obtained at the cathode, and high-purity sponge titanium is obtained at the anode. The invention fully utilizes the method of preparing the metal sponge titanium at high temperature and preparing the high-purity metal sponge titanium and the by-product by molten salt electrolysisHigh purity metallic aluminum. Compared with the traditional Kroll method for preparing Ti, the method is energy-saving and environment-friendly, has simple process and does not discharge harmful substances.
Description
Technical Field
The invention belongs to the field of metal smelting extraction, and particularly relates to a smelting and purifying method for preparing high-purity Ti and Ti alloy, in particular to a method for preparing metallic titanium by utilizing electrolytic separation of aluminum-titanium alloy.
Background
Titanium is a strategic resource, and metal titanium has excellent physical and chemical properties, has a density 43% lower than that of steel, high specific strength, high melting point, high temperature corrosion resistance and no toxicity, and is widely applied to aerospace, war industry and chemical industry. As "space metal", titanium alloys are used as engine materials, structural materials for aircraft, rockets, and various pipe joint materials. The metal titanium has the characteristics of light weight, high strength, high hardness, corrosion resistance and the like. The titanium resource reserves of China are the first in the world. The vanadium titano-magnetite is mainly stored in the Panxi area of Sichuan and distributed in mining areas such as Taihe, white horse, hongge and Panzhihua, wherein the white horse, the Hongge and the Panzhihua are located in Panzhihua city, and the Taihe iron ore is located in Wenchang city. The reserve of vanadium titano-magnetite resource is about 90 hundred million tons (the potential evaluation of mineral resources predicts 190 hundred million tons of iron ore resource), and the titanium resource is TiO 2 In) reserves of approximately 6 hundred million tons, accounting for approximately 87% of national reserves. However, the price of titanium greatly limits the use of titaniumBy virtue of this, despite the abundance of titanium in the earth's crust (0.44%, 8 th in all metallic elements, second only to 2.0% of magnesium), the price cannot be reduced due to the cumbersome current metallurgical processes for titanium.
At present, the method for preparing metallic titanium which is generally adopted by industry is a magnesiothermic reduction process (Kroll method), and the produced titanium sponge can be purified by electron beam melting. The Kroll process for producing metallic titanium first prepares titanium tetrachloride (TiCl) from titanium dioxide by carbon-adding chlorination 4 ) The titanium sponge is obtained by using magnesium metal through thermal reduction, the magnesium metal is obtained by electrolyzing magnesium chloride, chlorine obtained by electrolysis is used for preparing titanium chloride, the whole production process comprises three main parts of magnesium chloride electrolysis, titanium oxide chlorination and magnesium thermal reduction, the steps are complicated, the energy consumption is high, the core magnesium thermal reduction step is intermittent operation, the production efficiency is very low, the price of the titanium metal is high due to the reasons, the price of the titanium metal is far higher than that of steel, and the unit weight price of the titanium metal is more than 3 times that of aluminum metal. In addition, the chlorination process generates a serious corrosive environment, which has great harm to production equipment and environment, so that the method is a great problem faced by the Kroll method at present, and the storage and transportation of titanium tetrachloride are also very difficult.
At present, several representative titanium preparation processes such as FFC method, OS method, USTB method and the like in the process of producing metal titanium by molten salt electrolysis. The three methods are mainly TiO 2 When the titanium-titanium alloy is used as an anode material for electrolysis, oxygen in the material is difficult to remove in the electrolysis process, more than 99.9 percent of metallic titanium is difficult to produce, and the current efficiency is not high. Although the preparation of metallic titanium by molten salt electrolysis has obvious cost and technical advantages, large-scale industrial production cannot be realized at present, and a plurality of problems are still solved if large-scale industrial production is realized. The FFC method and the OS method both require long time of electrolysis to reduce the solid solution oxygen content in the metal titanium, and the current efficiency is only about 15 percent, so that the key points of reducing the oxygen content of the metal titanium, shortening the electrolysis time for preparing the metal titanium and improving the current efficiency in the industrialization of the production of the electrolytic titanium are known.
Disclosure of Invention
Aiming at the problems in the prior art, the technical problems to be solved by the invention are as follows: how to provide a method for preparing metallic titanium with high deoxidation rate, short preparation time and high current efficiency.
In order to solve the technical problems, the invention adopts the following technical scheme: a method for preparing metal titanium by utilizing electrolytic separation aluminum-titanium alloy, metal aluminum powder is used as a reducing agent, and fluotitanate is subjected to aluminothermic reduction for 2 to 3 hours at the temperature of 750 to 850 ℃ in a corundum crucible with a cover under the inert atmosphere environment; after the reaction is fully carried out, lifting the cover of the corundum crucible, adjusting the temperature to 1050-1250 ℃ for evaporation, and removing unreacted fluotitanate, fluoroaluminate generated by the reaction and other unreacted low-boiling-point impurities; obtaining a spongy aluminum-titanium alloy mixture with low purity in a corundum crucible after evaporation; the spongy aluminum-titanium alloy mixture is used as an anode, electrolysis is carried out in a molten salt electrolyte, and high-purity metal titanium sponge is obtained at the anode.
The improvement is that the fluotitanate is sodium fluotitanate or potassium fluotitanate.
As an improvement, the spongy aluminum-titanium alloy mixture is spongy TiAl or TiAl 3 、Ti 3 Al or mixtures thereof.
As an improvement, baCl is used in the electrolytic process 2 、Na 3 AlF 6 、AlF 3 And NaCl as electrolyte and is made of spongy TiAl or TiAl 3 、Ti 3 Al alloy or its mixture is used as anode material for electrolysis, and graphite is used as cathode material.
As an improvement, the electrolyte is 60wt% 2 、22wt％Na 3 AlF 6 、14wt％AlF 3 And 4wt% NaCl.
As an improvement, the electrolysis temperature in the electrolysis process is 1000-1100 ℃.
As an improvement, the addition amount of the metal aluminum powder is 2 to 4 weight percent more than the amount needed for generating Ti.
Compared with the prior art, the invention has at least the following advantages:
1. the invention proposes a method for electrolysis of molten salts, in order toTiAl and TiAl prepared by aluminothermic reduction method 3 、Ti 3 Al alloy or a mixture thereof as anode material, with 60wt% 2 ，22wt％Na 3 AlF 6 ，15wt％AlF 3 4wt% of NaCl is taken as electrolyte, high-purity aluminum is obtained at the cathode after electrolysis, and high-purity metal sponge titanium is obtained at the anode. Compared with the traditional process for preparing the titanium sponge by the Kroll method, the method has the advantages of obviously reducing energy consumption, saving energy, protecting environment, simple process and high added value of the byproduct high-purity aluminum.
2. The invention adopts the combination of an aluminothermic reduction method and a molten salt electrolysis method, and the aluminothermic reduction process can generate porous spongy TiAl and TiAl 3 、Ti 3 Al or mixtures thereof. Al in the anode is dissolved under the electrolysis condition and is precipitated at the cathode, thereby achieving the purpose of refining metallic titanium. The electrolysis process greatly reduces the energy consumption, and the current efficiency in the process is also high.
Drawings
FIG. 1 is a flow chart of the method of the present invention.
FIG. 2 shows an experimental apparatus for producing titanium by electrolysis according to the present invention.
In the figure, 1-steel bar, 2-graphite crucible, 3-aluminum-titanium alloy, 4-corundum tube, 5-molten salt and 6-pure aluminum.
Detailed Description
The present invention will be described in further detail below.
A process for preparing Ti metal from Al-Ti alloy by electrolytic separation features that the fluotitanate (sodium fluotitanate or potassium fluotitanate) is aluminothermally reduced to prepare TiAl or TiAl 3 、Ti 3 Al alloy or other mixture, fluotitanate evaporated at high temperature and other low boiling point impurities which are not reacted completely. Then 60wt% of BaCl 2 、22wt％Na 3 AlF 6 、15wt％AlF 3 And 4wt% NaCl as electrolyte, and sponge TiAl and TiAl prepared by thermite reaction 3 、Ti 3 Al alloy or the mixture thereof is used as the anode material for electrolysis, high-purity aluminum is obtained at the cathode after electrolysis, and metal titanium with higher purity is obtained at the anode. The invention fully utilizes the high-temperature aluminothermic reduction to prepare the aluminum-titanium alloy, and further adopts the molten salt electrolysis methodThe method prepares high-purity metal Ti and high-purity metal Al as a byproduct. Compared with the traditional Kroll method for preparing Ti, the method is energy-saving and environment-friendly, has simple process and does not discharge harmful substances.
Referring to fig. 1 and 2, a method for preparing metal titanium by separating aluminum-titanium alloy through electrolysis, wherein metal aluminum powder is used as a reducing agent, and fluotitanate is subjected to aluminothermic reduction for 2-3 hours at 750-850 ℃ in a corundum crucible with a cover under an inert atmosphere environment; in specific implementation, the aluminothermic reduction temperature can be selected from 750 ℃, 760 ℃, 770 ℃, 780 ℃, 790 ℃, 800 ℃, 810 ℃, 820 ℃, 830 ℃, 840 ℃ or 850 ℃; the reaction time can be selected from 2.0h, 2.2h, 2.5h, 2.8h or 3.0h.
After the reaction is fully carried out, lifting the cover of the corundum crucible, adjusting the temperature to 1050-1250 ℃ for evaporation, and removing unreacted fluotitanate, fluoroaluminate generated by the reaction and other unreacted low-boiling-point impurities; the 1050-1250 ℃ is used for evaporating other low boiling point substances except Ti and Al after reaction, including unreacted reactant fluotitanate, fluoride and fluotitanate generated by reaction, and when the specific implementation is carried out, the evaporating temperature can be 1050 ℃, 1080 ℃, 1100 ℃, 1130 ℃, 1150 ℃, 1180 ℃, 1200 ℃ or 1250 ℃.
Obtaining a spongy aluminum-titanium alloy mixture with low purity in a corundum crucible after evaporation; the spongy aluminum-titanium alloy mixture is used as an anode, electrolysis is carried out in an inert atmosphere environment, and high-purity metal titanium sponge is obtained by the anode.
In specific implementation, the fluotitanate is sodium fluotitanate or potassium fluotitanate.
The Al-Ti alloy mixture is TiAl or TiAl 3 、Ti 3 Al alloys or mixtures thereof.
BaCl is used in the electrolytic process 2 、Na 3 AlF 6 、AlF 3 And NaCl as electrolyte and spongy TiAl or TiAl 3 、Ti 3 Al alloy or its mixture is used as anode material for electrolysis, and graphite is used as cathode material. For the titanium sponge, the spongy TiAl and the Ti 3 Al、TiAl 3 Electrolyzing the alloy or the mixture thereof by using a molten salt electrolysis method to electrolyze sponge TiAl and TiAl 3 、Ti 3 Al alloy or its mixture as anode material, graphite as cathode material, and DC voltage to oxidize Al on anode to Al 3+ Into the molten electrolyte, al at the cathode 3+ The ions are separated out by electron to form simple substance Al, so that high-purity metal Al is formed, and the rest part of the anode is high-purity metal titanium.
The addition amount of the metal aluminum powder is 2-4wt% more than the amount required for generating Ti, and the addition amount of the specific metal aluminum powder is 2.0wt%, 2.2wt%, 2.5wt%, 2.8wt%, 3wt%, 3.2wt%, 3.5wt%, 3.8wt% or 4.0wt% more than the amount required for generating Ti.
As shown in figure 1, the anode is smelted into spongy TiAl and TiAl with low purity by an aluminothermic reduction method 3 、Ti 3 Al alloy or a mixture thereof, and obtaining high-purity metal sponge titanium after electrolysis; graphite as cathode material and BaCl 2 、Na 3 AlF 6 、AlF 3 And NaCl as electrolyte at 1000-1100 deg.c, and the electrolysis temperature may be 1000 deg.c, 1010 deg.c, 1020 deg.c, 1040 deg.c, 1050 deg.c, 1060 deg.c, 1070 deg.c, 1080 deg.c, 1090 deg.c or 1100 deg.c. The electrolyte was 60wt% BaCl 2 、22wt％Na 3 AlF 6 、14wt％AlF 3 And 4wt% NaCl.
The reaction equation specifically involved:
3Na 2 TiF 6 +4Al+6NaF＝3Ti+4Na 3 AlF 6
3Na 2 TiF 6 +7Al+6NaF＝3AlTi+4Na 3 AlF 6
3Na 2 TiF 6 +13Al+6NaF＝3AlTi 3 +4Na 3 AlF 6
3K 2 TiF 6 +4Al+6KF＝3Ti+4K 3 AlF 6
3K 2 TiF 6 +7Al+6KF＝3AlTi+4K 3 AlF 6
3K 2 TiF 6 +13Al+6KF＝3AlTi 3 +4K 3 AlF
Al+7AlCl 4 - ＝4Al 2 Cl 7 - +3e -
4Al 2 Cl 7 - +3e - ＝Al+7AlCl 4 -
in the invention, various aluminum-titanium alloys can be subjected to electrolytic separation in the aluminothermic reduction process, the aluminum-titanium alloys are not limited to one type of aluminum-titanium alloys, and the aluminum-titanium alloys are mostly sponge-shaped, so that a larger available space is provided for the electrolysis process of the second step, the reaction efficiency is increased, the reaction time is shortened, and the crystallized byproducts can be continuously used for industrial aluminum electrolysis. In the electrolytic process, high-purity aluminum can be obtained at the cathode, high-purity titanium sponge can be obtained at the anode, the energy consumption is reduced, the energy is saved, the environment is protected, the process is simple, and no harmful substance is discharged.
Finally, although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that various changes and modifications may be made therein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (7)
1. A method for preparing metal titanium by utilizing electrolytic separation aluminum-titanium alloy is characterized in that metal aluminum powder is used as a reducing agent, and fluotitanate is subjected to aluminothermic reduction for 2-3 h at 750-850 ℃ in an inert atmosphere environment in a corundum crucible with a cover;
after the reaction is fully carried out, lifting the cover of the corundum crucible, adjusting the temperature to 1050-1250 ℃ for evaporation, and removing unreacted fluotitanate, fluoroaluminate generated by the reaction and other unreacted low-boiling-point impurities;
obtaining a spongy aluminum-titanium alloy mixture with low purity in a corundum crucible after evaporation;
the spongy aluminum-titanium alloy mixture is used as an anode, electrolysis is carried out in molten salt electrolyte, and high-purity metal titanium sponge is obtained at the anode.
2. The method for producing metallic titanium by separating aluminum-titanium alloy through electrolysis as recited in claim 1, wherein: the fluotitanate is sodium fluotitanate or potassium fluotitanate.
3. The method for producing metallic titanium by electrolytic separation of aluminum-titanium alloy according to claim 1 or 2, wherein: the spongy aluminum-titanium alloy mixture is spongy TiAl or TiAl 3 、Ti 3 Al or mixtures thereof.
4. The method for producing metallic titanium by separating aluminum-titanium alloy through electrolysis as recited in claim 3, wherein: baCl is used in the electrolytic process 2 、Na 3 AlF 6 、AlF 3 And NaCl as electrolyte and is made of spongy TiAl or TiAl 3 、Ti 3 Al alloy or their mixture is used as anode material for electrolysis, and graphite is used as cathode material.
5. The method for producing metallic titanium by separating aluminum-titanium alloy through electrolysis as recited in claim 4, wherein: the electrolyte was 60wt% BaCl 2 、22wt％Na 3 AlF 6 、14wt％AlF 3 And 4wt% NaCl.
6. The method for producing metallic titanium by separating aluminum-titanium alloy through electrolysis as recited in claim 4, wherein: the electrolysis temperature in the electrolysis process is 1000-1100 ℃.
7. The method for producing metallic titanium by separating aluminum-titanium alloy through electrolysis as recited in claim 5, wherein: the addition amount of the metal aluminum powder is 2-4wt% more than the amount needed for generating Ti.
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