CN109825854A - A kind of molten-salt electrolysis-high temperature distillation prepares the device and method of high-purity titanium - Google Patents
A kind of molten-salt electrolysis-high temperature distillation prepares the device and method of high-purity titanium Download PDFInfo
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Abstract
A kind of molten-salt electrolysis-high temperature distillation prepares the device and method of high-purity titanium, belongs to the field that electrochemical process prepares high purity titanium.Production stage is as follows: titaniferous halide electrolyte being added in electrolytic cell and carries out fritting, is then kept the temperature under an argon atmosphere.With liquid metal (bismuth, tin, lead etc.) for cathode, titanium sponge or solvable titaniferous materials (titanium carbon oxygen solid solution etc.) are anode, are electrolysed.After electrolysis, cathode titanium alloy product finally obtains high-purity titanium through high temperature distillation.The method of the present invention has the characteristics that low energy consumption, device simple, with short production cycle, titanium recovery rate is high.In this way, the impurity in anode can be effectively removed, hypoxemia, superelevation pure titanium metal are obtained, there is stronger application prospect.
Description
Technical field
The present invention relates to a kind of, and molten-salt electrolysis-high temperature distillation based on liquid metal cathode prepares the side of high-purity titanium
Method belongs to electrolysis method production high purity titanium field, high-purity titanium finally can be obtained.
Background technique
Titanium is because of the low (4.5g/cm of density3), it is fusing point high (1660 DEG C), anticorrosive, resistance to oxidation, nontoxic etc. excellent
Anisotropic energy, referred to as " the following metal ".It is in aerospace, chemical, ship naval vessels, biologic medical, civilian building materials and body
The fields such as equipment are educated to have a wide range of applications.On this basis, Ti content is higher than 99.95% or 99.99% (i.e. 3N5 by people
Or 4N) titanium be known as high-purity titanium.High-purity titanium not only possesses excellent performance possessed by common titanium, together
When, the objectionable impurities elements of excellent elongation percentage (50-60%), the contraction percentage of area (70-80%) and super low loading are general
What logical titanium can not be reached.Therefore, high purity titanium is advanced, accurate, sharp in large scale integrated circuit, deep space exploration, flexible display screen etc.
The application in end field is continuously increased, and is increasingly becoming the important leverage of these industries rapid development.
Currently, the industrialized production for only having a small number of enterprises such as the U.S., Japan and China to realize high purity titanium in the world.Its
In, the U.S. and Japan mainly use Kroll method, and this method requires raw material titanium tetrachloride, magnesium metal etc. when preparing high purity titanium
With higher purity, at the same it is harsh to the air-tightness of equipment, precision requirement.Therefore, using high purity titanium obtained by this method at
This is high, and process is tediously long；In addition, high purity titanium oxygen content obtained by kroll method is generally higher, it is difficult to meet current higher-order electronics electricity
The performance requirement of the microelectronic fields such as road.Domestic Ningxia De Yunchuanrun Co., Ltd is realized high-purity using fused salt electrolysis process
The preparation of industrialization of titanium.Using the method for molten-salt electrolysis, products therefrom purity is higher (can > 99.95%), and oxygen content is significant
Reduce (can≤50ppm).Meanwhile this method is lower to material purity requirement, production procedure is simple, and products therefrom is low in cost.
However, conventional electrolysis products therefrom is solid dendritic shape titanium, partial electrolyte is often carried in gained titanium dendrite.To remove
Electrolyte in dendrite needs additionally to obtain dry pure high-purity titanium crystal using the methods of washing, pickling, drying.Washing,
The process of pickling not only results in the secondary oxidation of high purity titanium, while will cause the waste of high-purity titanium particulate, finally reduces high-purity
The recovery rate of titanium.
Summary of the invention
When the present invention prepares high purity titanium for fused salt electrolysis process, because washing, pickling reduce product recovery rate and secondary oxygen
The deficiency of change provides the device and method that a kind of electrolysis-distillation prepares high purity titanium.It is relative to Kroll method or with titanium sponge
The method that the molten-salt electrolysis of raw material prepares high-purity titanium, this method have that low energy consumption, and recovery rate of iron is high, product oxygen content is low
The features such as.
A kind of molten-salt electrolysis-high temperature distillation prepares the device of high-purity titanium, it is characterised in that including fused salt electrolysis apparatus
And distiller:
Fused salt electrolysis apparatus includes anode electrode bar, electrolytic furnace, heating element, is electrolysed crucible, anode titanium plate, electrolyte,
Cathode electrode bar, cathode liquid metal；Anode electrode bar is connect with anode, so that anode conducting；Heating element is located at electrolytic furnace
Side wall and bottom, for heating and keeping the temperature to furnace body；Electrolysis crucible is located in electrolytic furnace, for holding electrolyte；Anode titanium plate
Electrode hole by being electrolysed bell is inserted into electrolytic furnace, and is contacted with the electrolyte in electrolysis crucible；Electrolyte is used for being electrolysed
Reaction solution is placed in electrolysis crucible；Cathode electrode bar is connect with cathode, so that cathode liquid metallic conduction；Liquid metal yin
Pole can be placed in electrolysis crucible bottom, can also be placed in particular cathode crucible, and in final all immersions fused electrolyte；Distiller packet
It includes: alembic, raw material tank, heating device, condenser, cycle argon gas import, high temperature argon outlet, vacuum plant, argon gas recycling
Device, heat-insulating material, argon gas separator, tube head of spraying water, clarifier, bismuth metal, tin, lead collecting chamber；Alembic is the master of distillation
Body equipment is placed in the centre of distillation workshop；Raw material tank is located at the top of alembic, former for adding titanium alloy into alembic
Material；Heating device is located at distillation pot bottom and side bottom, for heating and keeping the temperature；Condenser is located at the top of alembic, is used for
Collect distillation gained impurity element；Circulation argon gas import is located at the top of distiller, for providing the protection of the argon gas in distiller
Atmosphere；High temperature argon outlet is located at alembic top, circulation argon gas entrance location is listed in, for realizing argon gas in alembic
Circulation discharge；Vacuum plant is located at alembic side, for realizing the vacuum in alembic；Argon gas recyclable device is located at vacuum holding
Lower part is set, be mainly used for realization vacuum plant vacuumizes tonifying Qi etc.；Insulating materials is located at alembic in-between, for real
It is heat-insulated between existing heating device and condenser；Argon gas separator is connected with circulation argon gas import, for realizing high-purity argon gas
Circulation；Water pipeline is located at distillation pot bottom, and with raw material tank, circulation argon gas import, the laid out in parallel such as outlet, for realizing cold
The fast cooling of condenser and heat preservation；Clarifier is located at alembic upper right, for removing the gaseous impurity of distillage carrying；
Metal collector chamber is located at the right of alembic, for collecting final high-purity titanium products.
A method of high-purity titanium is prepared using above-mentioned apparatus molten-salt electrolysis-high temperature distillation, mainly includes following step
It is rapid:
1) according to chemical reaction metering than will contain titanium halide and supporting electrolyte mixing it is uniform after, electrolyte fusing point with
Upper 50-200 DEG C of progress fritting, anode are that titanium sponge, titanium carbon oxygen solid solution or titanium carbon nitrogen oxygen solid solution, cathode are liquid metal；
2) anode wait immerse in fused salt is completely dissolved or cathode liquid Metal Phase Transition is stops electrolysis when solid alloy, negative
Pole obtains titanium alloy product；
3) cathode titanium alloy product is fitted into distiller, is carried out using the temperature for being higher than liquid cathode metal boiling point used
Distillation (temperature controls between 1200~2500 DEG C), removes liquid cathode metal impurities, gained liquid metal can be further
It recycles；
4) distillation resultant product is collected, high-purity titanium is finally obtained.
Further, it is characterised in that the heating device (3) is anti-vacuum heater, and when impurity member in titanium alloy
Element stops distillation when being lower than 0.00001-0.001%, is then cooled to 50 DEG C hereinafter, opening rewinding room, Vacuum Package or in height
High-purity titanium products are encapsulated under straight argon gas shielded.
Further, it is characterised in that the anode titanium sponge purity 90% or more, titanium sponge, titanium carbon oxygen solid solution or
Titanium carbon nitrogen oxygen solid solution can be processed as block, rodlike, using metal fixture or is threadedly coupled conductive；It can also be in granular form and be placed in not
It is used as anode in steel or the copper anode material frame of becoming rusty, anode reaction is as follows:
Ti-xe=Tix+(wherein x=2 or 3).
Further, it is characterised in that the TiCl containing titanium halide for purity higher than 90%3、TiCl2Or K2TiF6In one
Kind or two kinds, content containing titanium halide in the electrolyte is 0.1-30%.
Further, it is characterised in that supporting electrolyte is NaCl, KCl, LiCl, MgCl that purity is higher than 95%2、
CaCl2、BaCl2、NaF、KF、LiF、MgF2、CaF2、BaF2In two or more fused salt mixture.
Further, it is characterised in that cathode liquid metal is bismuth of the purity higher than 90%, tin, lead, aluminum metal, can also be with
It is the mixture of two or more in them, cathode reaction is as follows:
Tix++ xe=Ti (titanium alloy) (wherein x=2 or 3).
Compared with the existing technology, the present invention has the advantages that
1), the present invention provides it is a kind of low energy consumption, cost is controllable, the device of separating-purifying high purity titanium with short production cycle with
Method.
2), from the angle of high pure metal titanium, high purity titanium recovery rate is high, good product quality.
3), in terms of distillation equipment, continuous air extraction is carried out to separator using vacuum plant, so that vapo(u)rizing temperature is reduced,
Energy consumption has not only been saved, while having improved titanium purification rate.
Detailed description of the invention
Fig. 1 is fused salt electrolysis apparatus schematic diagram of the present invention；
1. anode electrode bar, 2. electrolytic furnaces, 3. heating elements, 4. electrolysis crucibles, 5. anode titanium plates, 6. electrolyte, 7. yin
Pole electrode stem, 8. cathode liquid metals.
Fig. 2 is that present invention distillation prepares pure titanium schematic device；
9. alembic, 10. raw material tanks, 11. heating devices, 12. condensers, 13. cycle argon gas imports, 14. high temperature argons
Outlet, 15. vacuum plants, 16. argon gas recyclable devices, 17. heat-insulating materials, 18. argon gas separators, 19. water spray tube heads, 20. is net
Change device, the collecting chambers such as 21. bismuth metals, tin, lead.
Specific embodiment
Embodiment 1
By TiCl3With NaCl-KCl (molar ratio 1:1) according to mass ratio 1:25 mixing it is uniform after, be fitted into electrolytic cell,
Cathode is liquid metal bismuth, and anode is sponge Ti plate.It is electrolysed after carrying out fritting at 800 DEG C, after anode material is completely dissolved
Stop electrolysis, electrolysis cathode product is Bi-Ti alloy.Cathode product is transferred in distillation equipment, in 1580 DEG C of cucurbit
In be evaporated in vacuo.Product of distillation obtains high-purity titanium by processing such as drying, encapsulation.
Embodiment 2
By TiCl2And CaCl2- NaF (molar ratio 3:2) according to mass ratio 1:30 mixing it is uniform after, be fitted into electrolytic cell,
Cathode is liquid metal tin, and anode is titanium carbon oxygen solid solution.It is electrolysed after carrying out fritting at 900 DEG C, electrolysis cathode product is Sn-
Ti alloy.Cathode product is transferred in distillation equipment, is evaporated in vacuo at 2280 DEG C.Product of distillation is by drying, encapsulation
Equal processing obtain high-purity titanium, and gained tin further recycles.
Embodiment 3
By TiCl3With KCl-NaF (molar ratio 2:3) according to mass ratio 1:27 mixing it is uniform after, be fitted into electrolytic cell, yin
Extremely liquid metal lead, anode are sponge Ti plate.It is electrolysed after carrying out fritting at 700 DEG C, electrolysis cathode product is Pb-Ti conjunction
Gold.Cathode product is transferred in distillation equipment, is evaporated in vacuo in 1780 DEG C.Product of distillation is by processing such as drying, encapsulation
Obtain high-purity titanium.
Certainly, there are also various embodiments to be familiar with this field without departing substantially from the technology of the present invention essence by the present invention
Technical staff can disclosure according to the present invention make various corresponding changes and modification, but these corresponding adjustment all should belong to this
The protection scope of invention appended claims.
Claims (7)
1. the device that a kind of molten-salt electrolysis-high temperature distillation prepares high-purity titanium, it is characterised in that including fused salt electrolysis apparatus and
Distiller；
Fused salt electrolysis apparatus includes anode electrode bar (1), electrolytic furnace (2), heating element (3), electrolysis crucible (4), anode titanium plate
(5), electrolyte (6), cathode electrode bar (7), cathode liquid metal (8)；Anode electrode bar is connect with anode, so that anode is led
Electricity；Heating element is located at electrolysis furnace sidewall and bottom, for heating and keeping the temperature to furnace body；Electrolysis crucible is located in electrolytic furnace, uses
In holding electrolyte；Anode titanium plate by electrolysis bell electrode hole be inserted into electrolytic furnace in, and with electrolysis crucible in electrolyte
Contact；Electrolyte is used for electrolysis reaction solution, is placed in electrolysis crucible；Cathode electrode bar is connect with cathode, so that catholyte
State metallic conduction；Liquid metal cathode is placed in electrolysis crucible bottom, or is placed in particular cathode crucible, and final all immerse melts
In electrolyte；Distiller includes: alembic (9), raw material tank (10), heating device (11), condenser (12), cycle argon gas import
(13), high temperature argon outlet (14), vacuum plant (15), argon gas recyclable device (16), heat-insulating material (17), argon gas separator
(18), it sprays water tube head (19), clarifier (20), bismuth metal, tin, lead collecting chamber (21)；Alembic is the main equipment of distillation, is set
In the centre of distillation workshop；Raw material tank is located at the top of alembic, for adding titanium alloy raw material into alembic；Heating device
Positioned at distillation pot bottom and side bottom, for heating and keeping the temperature；Condenser is located at the top of alembic, for collecting distillation gained
Impurity element；Circulation argon gas import is located at the top of distiller, for providing the argon atmosphere in distiller；High temperature argon
Outlet is located at alembic top, is listed in circulation argon gas entrance location, for realizing the circulation discharge of argon gas in alembic；Vacuum
Device is located at alembic side, for realizing the vacuum in alembic；Argon gas recyclable device is located at vacuum plant lower part, main to use
Tonifying Qi is vacuumized in realization vacuum plant；Insulating materials is located at alembic in-between, for realizing heating device and cold
It is heat-insulated between condenser；Argon gas separator is connected with circulation argon gas import, for realizing the circulation of high-purity argon gas；Water pipeline position
In distillation pot bottom, and with raw material tank, circulation argon gas import, outlet laid out in parallel, for realizing condenser fast cooling and
Heat preservation；Clarifier is located at alembic upper right, for removing the gaseous impurity of distillage carrying；Metal collector chamber, which is located at, to be steamed
The right for evaporating tank, for collecting final high-purity titanium products.
2. a kind of method for preparing high-purity titanium using device molten-salt electrolysis-high temperature distillation as described in claim 1, feature
Be the following steps are included:
1) according to chemical reaction metering than will contain titanium halide and supporting electrolyte mixing it is uniform after, more than electrolyte fusing point
50-200 DEG C of progress fritting, anode are that titanium sponge, titanium carbon oxygen solid solution or titanium carbon nitrogen oxygen solid solution, cathode are liquid metal；
2) anode wait immerse in fused salt is completely dissolved or cathode liquid Metal Phase Transition is stops electrolysis when solid alloy, and cathode obtains
Obtain titanium alloy product；
3) cathode titanium alloy product is fitted into distiller, is distilled using the temperature for being higher than liquid cathode metal boiling point, temperature
Degree control removes liquid cathode metal impurities between 1200~2500 DEG C, and gained liquid metal can be recycled further；
4) distillation resultant product is collected, high-purity titanium is finally obtained；
3. the method that molten-salt electrolysis-high temperature distillation as claimed in claim 2 prepares high-purity titanium, it is characterised in that step 3) institute
Stating the heating device in distiller is anti-vacuum heater, and works as impurity element in titanium alloy and be lower than 0.00001-0.001%
When stop distillation, be then cooled to 50 DEG C hereinafter, open rewinding room, Vacuum Package or high-purity argon gas protection under encapsulate high purity titanium
Product.
4. the method that molten-salt electrolysis-high temperature distillation as claimed in claim 2 prepares high-purity titanium, it is characterised in that the anode
For titanium sponge purity 90% or more, titanium sponge, titanium carbon oxygen solid solution or titanium carbon nitrogen oxygen solid solution are processed as block, rodlike, or are in
Graininess is placed in stainless steel or copper anode material frame as anode, and block, rodlike use metal fixture or threaded connection are conductive,
Anode reaction is as follows: Ti-xe=Tix+(wherein x=2 or 3).
5. a kind of method that molten-salt electrolysis-high temperature distillation prepares high-purity titanium as claimed in claim 2, it is characterised in that titaniferous
Halide is the TiCl that purity is higher than 90%3、TiCl2Or K2TiF6One or both of, in the electrolyte containing titanium halide
Content is 0.1-30%.
6. a kind of method that molten-salt electrolysis-high temperature distillation prepares high-purity titanium as claimed in claim 2, it is characterised in that support
Electrolyte is NaCl, KCl, LiCl, MgCl that purity is higher than 95%2、CaCl2、BaCl2、NaF、KF、LiF、MgF2、CaF2、BaF2
In two or more fused salt mixture.
7. the method that molten-salt electrolysis-high temperature distillation as claimed in claim 2 prepares high-purity titanium, it is characterised in that cathode liquid
Metal is the mixture of bismuth of the purity higher than 90%, tin, lead, aluminum metal or two or more in them, cathode reaction
It is as follows: Tix++ xe=Ti (titanium alloy) (wherein x=2 or 3).
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| CN110983378A (en) * | 2019-11-15 | 2020-04-10 | 北京理工大学 | Device and method for preparing metal aluminum and titanium tetrachloride in molten salt by soluble anode |
| CN112281190A (en) * | 2020-10-12 | 2021-01-29 | 郑州大学 | Electrochemical method for preparing molybdenum metal by utilizing molybdenum disulfide |
| CN112853113A (en) * | 2021-01-08 | 2021-05-28 | 宁波长振铜业有限公司 | Method and device for removing lead impurities in scrap copper alloy |
| CN113445080A (en) * | 2021-06-09 | 2021-09-28 | 北京科技大学 | Method for preparing titanium alloy based on direct electrolysis of liquid cathode-soluble titanium-containing anode |
| CN114410975A (en) * | 2022-01-25 | 2022-04-29 | 东北大学 | Method for recovering waste aluminum/waste aluminum alloy |
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Application publication date: 20190531 |
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| RJ01 | Rejection of invention patent application after publication |