CN108441893A - A kind of molten-salt electrolysis TiO2The method for preparing Titanium - Google Patents

A kind of molten-salt electrolysis TiO2The method for preparing Titanium Download PDF

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Publication number
CN108441893A
CN108441893A CN201810607896.8A CN201810607896A CN108441893A CN 108441893 A CN108441893 A CN 108441893A CN 201810607896 A CN201810607896 A CN 201810607896A CN 108441893 A CN108441893 A CN 108441893A
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cathode
molten
anode
tio
preparing titanium
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Inventor
扈玫珑
屈正峰
胡蒙均
李朝东
赖平生
马通祥
高雷章
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Chongqing Jing Tai Business Management Consulting Co Ltd
Chongqing University
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Chongqing Jing Tai Business Management Consulting Co Ltd
Chongqing University
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Priority to CN201810607896.8A priority Critical patent/CN108441893A/en
Publication of CN108441893A publication Critical patent/CN108441893A/en
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    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
    • C25C3/00—Electrolytic production, recovery or refining of metals by electrolysis of melts
    • C25C3/26—Electrolytic production, recovery or refining of metals by electrolysis of melts of titanium, zirconium, hafnium, tantalum or vanadium
    • C25C3/28—Electrolytic production, recovery or refining of metals by electrolysis of melts of titanium, zirconium, hafnium, tantalum or vanadium of titanium
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
    • C25C7/00—Constructional parts, or assemblies thereof, of cells; Servicing or operating of cells
    • C25C7/005—Constructional parts, or assemblies thereof, of cells; Servicing or operating of cells of cells for the electrolysis of melts
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
    • C25C7/00—Constructional parts, or assemblies thereof, of cells; Servicing or operating of cells
    • C25C7/04—Diaphragms; Spacing elements

Abstract

The invention discloses a kind of molten-salt electrolysis TiO2The method for preparing Titanium, this method are carried out in anode and cathode or crucible structure using alumina material and improve to carry out the anode and cathode fused salts of insulation surfaces and be directly connected with anode and cathode so as to avoid the black conductive floating material on fused salt surface the floating material for wasting and achieving the purpose that improve current efficiency and control black of electric current is caused to pollute fused salt and sample.The method of the present invention is simple but actual significant effect, improves FFC method molten-salt electrolysis and prepares Titanium and the current efficiency of other metal materials.

Description

A kind of molten-salt electrolysis TiO2The method for preparing Titanium
Technical field
The present invention relates to molten-salt electrolysis to prepare technical field of metal material more particularly to a kind of molten-salt electrolysis TiO2Prepare gold Belong to the method for titanium.
Background technology
For titanium or titanium alloy due to having the advantages that a series of protrusions such as specific strength height, the good, high temperature resistant of corrosion resistance, being originally can With should widespread adoption superior metal, but its use in civil field is limited because of at high price.
Industrially use Kroll methods from TiO at present2Set out for raw material finally obtain Titanium powder will be after a series of unrestrained Long step.It is TiO first2Carburizing chlorination TiCl is prepared4, then sponge is prepared as reducing agent using metal Mg Titanium, titanium sponge produce titanium ingot using subsequent melting and carry out subsequent processing again, and whole process energy consumption is huge.
Fused salt CaCl2It is considered as potential replacement tradition that middle electrolysis titanium dioxide, which prepares Titanium technique (Cambridge FFC), One of the abbreviated system of Kroll techniques (magnesiothermy).But the CO that anode generates during electrolysis2Gas is easy to dissolve In CaCl2In fused salt, and O2-With stablizing CO in fused salt2Effect, i.e. O in fused salt2-It can be with CO2Reaction formed carbonate from Son (CO3 2-).Currently, during the process electrolyte, since anode generates CO2Gas, and cathode removes O2-, therefore, in molten salt body Unavoidably there is CO in system3 2-.Under current electrolytic condition, CO3 2-Cell reaction can occur, carbon, anode O are obtained in cathode2- Electric discharge.In addition, oversaturated CaO and CO2Effect can form CaCO3.Since the continuous deoxidation of cathode so that part carbanion is electric The carbon dust that solution cathode obtains sheds into fused salt.Anode graphite also has a small amount of carbon dust to fall off and calls in fused salt due to constantly reacting In.Fused salt surface can form the floating material of one layer of black in electrolytic process, due to the presence of carbon dust, cause cathode, carbon dust and Anode forms short circuit and the current efficiency of the technique is reduced.
Invention content
For deficiencies of the prior art, the present invention provides a kind of molten-salt electrolysis TiO that current efficiency is high2It prepares The method of Titanium.
To achieve the goals above, the technical solution adopted by the present invention is as follows：
A kind of molten-salt electrolysis TiO2Fused salt is isolated using the electrode district isolator of corundum material for the method for preparing Titanium Cheng Yangqu and cathodic region, make TiO2It is placed in cathodic region and is electrolysed.
Specifically comprise the following steps：
1) by TiO2Powder is simultaneously unidirectionally cold-pressed compression moulding, and bulk sample is made.
2) bulk sample made from step 1) is placed in 3~5h of sintering in Muffle furnace in air atmosphere；The Muffle furnace Temperature control at 900~1200 DEG C.This can make TiO in sample2Occur crystal transfer and intensity increase it is non-breakable to Conducive to subsequent operation.
3) sintered bulk sample in the step 2) is fixed on steel electrode bar, obtains assembly cathode, it is spare. Fixing means can select as needed, compare with wire binding etc..Most handy electric conductivity is good and fusing point it is relatively high (>= 1300 DEG C) wire ensure that sample will not fall off in electrolytic process and fall down.
4) the electrode district isolator is placed in the corundum crucible equipped with anhydrous calcium chloride, the electrode district isolator Bottom be provided with the through-hole people so that anhydrous calcium chloride penetrate the electrode district isolator, make corundum crucible formed two electrode districts, Respectively as anode region and cathodic region；Electrolytic furnace is led into ar purging and Continuous aeration atmosphere again, to ensure argon gas atmosphere, increases temperature It spends and controls at 800~1050 DEG C, obtain molten salt body；Then it is inserted into anode region using graphite electrode as anode, with metal electrode Stick is inserted into cathodic region as cathode, and applies DC voltage and carry out preelectrolysis between anode and cathode.It is to remove to carry out preelectrolysis Remove CaCl2Impurity in fused salt, such as the moisture that is dissolved in fused salt.
Above-mentioned electrolytic process carries out in tubular type electrolytic furnace, and ensures the atmosphere of argon gas in stove.Electrolysis before with argon gas into Row prepurging 3 times then passes to argon gas first the electrolysis stove evacuation of sealing, recycles 2 times again, is continually fed into argon for the last time After gas and venthole is opened, ensures good argon atmosphere in stove.It heats up to electrolytic furnace, control heating rate is in 5K/min Left and right, and reaching heat preservation 30min or so after 800~1050 DEG C of assigned temperature again makes system reach stable state.
5) metal electrode bar is taken out, the assembly cathode that step 3) obtains is placed in cathodic region, applies DC voltage in the moon It is electrolysed between anode；Until Faradaic current reduces and stablizes to 0.2A, stop being electrolysed and take out assembly cathode, it is placed in argon gas With electrolytic furnace cooled to room temperature in atmosphere, the assembly cathode after being electrolysed.
6) bulk sample is removed from the assembly cathode after electrolysis, after washing away the attachment of residual on it with clear water, It is placed in baking oven and dries, obtain Titanium.
Wherein, the pressure that compacting is unidirectionally cold-pressed in step 1) is 2.5~5MPa, and the dwell time is 1~10s.The TiO2 Purity >=99.8% of powder.In order to ensure the easily molded and good reactivity of the sample prepared, the TiO in raw material2Powder it is pure Degree is preferably >=99.8%, TiO2The sieve of most well 140 mesh of powder, powder size it is smaller so as to ensure sample compacting when be easier Molding.With steel die by mixed material cold moudling obtained, unidirectional to suppress, pressing pressure is 2.5~5MPa, dwell time For 1~10s.Here pressure is not easy excessive, it is ensured that sample has certain porosity to be conducive to electrolysis deoxidation.
The electrode district isolator is the pipe sleeve of upper end opening or the corundum adaptable with the corundum crucible interior shape Plate.The purity of argon is not less than 99.99%.
In step 5), temperature when electrolysis is controlled at 900~1050 DEG C.Since the fusing point of calcium chloride is close to 800 DEG C, electricity Solution temperature has to be higher than this temperature, electrolysis temperature is controlled at 900-1050 DEG C, one can reinforce fused salt in electrolytic process The transmitting effect of intermediate ion, temperature is higher, and Ion transfer can be faster；Second is that due to CaCl2Fused salt has certain volatilization, Temperature is excessively high to make fused salt volatilization be led out excessively by protective gas in stove, and considers from energy consumption angle, select 900- 1050 DEG C relatively reasonable.
In step 4), the DC voltage of the application is 2.8V, electrolysis time 2h.Voltage 2.8V is more in an experiment Verification can remove CaCl in fused salt after secondary trial2One voltage of middle major part impurity, so this voltage is selected to carry out pre- electricity Solution.The electric current of general preelectrolysis can be reduced to a range that is relatively small and stablizing after 2h, show that preelectrolysis has been compared More abundant, the impurity in fused salt has been removed to a very small range.
In step 5), the DC voltage of application is 3.1V.The CaCl at 900 DEG C2Theoretical decomposition voltage be 3.2V, electricity Solution will carry out under the theoretical decomposition voltage of electrolyte, therefore be arranged in 3.1V.
In step 6), oven temperature is 105 DEG C, soaking time 10h.
It is directed to and uses the direct molten-salt electrolysis TiO of FFC methods at present2Prepare fused salt surface during Titanium can be formed one layer it is black The floating material of color, due to the presence of carbon dust, causing cathode, carbon dust and anode to form short circuit and the current efficiency of the technique is made to drop Fused salt isolation in negative and positive polar region surface is made cathode, anode and fused salt surface by the problems such as low, the present invention using insulating oxide aluminum material The circuit that conductor is formed is switched off, to effectively improve the current efficiency of technique.
Compared with prior art, the present invention has the advantages that：
1, the present invention directly addition alumina material is used to be isolated the fused salt region of anode and cathode, and method is simple, easy to operation.
2, the conductive floating material for avoiding fused salt upper black is directly connected to anode and cathode and causes wasting for electric current, to improve Current efficiency.
3, the range for controlling the flowing of black floating material has efficiently controlled its dirt to fused salt with being electrolysed sample Dye.
Description of the drawings
Fig. 1 is the crucible sectional view after comparative example experiment；
Fig. 2 is the electrolytic cell schematic diagram of corundum casing；
Fig. 3-a are the crucible figure after embodiment one is tested；
Fig. 3-b are the crucible figure after embodiment two is tested；
Fig. 3-c are the crucible figure after embodiment two is tested；
Fig. 4 is the time current curve comparison figure of different electrolytic cells；
Fig. 5 is the XRD diagram for the sample that electrolysis obtains.
Specific implementation mode
With reference to specific embodiment, invention is further described in detail.
Comparative example
This comparative example selects purity to be >=99.8% and cross the TiO of 140 mesh sieve2Powder does not use electrode district isolator, step It is rapid as follows：
1) by TiO2Powder steel die is by material cold moudling, and unidirectional to suppress, pressing pressure is 2.5~5MPa, is protected The pressure time is 1~10s, demoulds bulk sample is made later.
2) bulk sample made from step 1) is placed in 3~5h of sintering in Muffle furnace in air atmosphere；The Muffle furnace Temperature control at 900~1200 DEG C.
3) sintered bulk sample in the step 2) is tied up with wire in steel electrode bar, obtains assembly cathode, It is spare.
4) electrolytic furnace is led into ar purging and Continuous aeration atmosphere, to ensure argon gas atmosphere, increase temperature and control 800~ 1050 DEG C, obtain molten salt body；Then it is inserted into anode region using graphite electrode as anode, is inserted into using metal electrode bar as cathode cloudy Polar region, and the DC voltage for applying 2.8V carries out preelectrolysis 2h between anode and cathode.
5) take out metal electrode bar, the assembly cathode that step 3) is obtained is inserted into molten salt body, apply 3.1V DC voltages in It is electrolysed between anode and cathode；Up to Faradaic current reduces and stablizes to the background current stage of 0.2A or so and there is no reductions Trend can stop being electrolysed, stop be electrolysed simultaneously take out assembly cathode, be placed in argon gas atmosphere and naturally cool to room with electrolytic furnace Temperature, the assembly cathode after being electrolysed.
6) bulk sample is removed from the assembly cathode after electrolysis, after washing away the attachment of residual on it with clear water, It is placed in 105 DEG C of baking ovens and dries 10h, obtain Titanium.
Crucible after experiment is as shown in Figure 1.
Embodiment one：
The present embodiment selects purity to be >=99.8% and cross the TiO of 140 mesh sieve2Powder, by the way of corundum casing come Anode and cathode fused salt is isolated, the structure of electrolytic cell is as shown in Fig. 2, steps are as follows：
1) by TiO2Powder steel die is by material cold moudling, and unidirectional to suppress, pressing pressure is 2.5~5MPa, is protected The pressure time is 1~10s, demoulds bulk sample is made later.
2) bulk sample made from step 1) is placed in 3~5h of sintering in Muffle furnace in air atmosphere；The Muffle furnace Temperature control at 900~1200 DEG C.
3) sintered bulk sample in the step 2) is tied up with wire in steel electrode bar, obtains assembly cathode, It is spare.
4) corundum casing is placed in the corundum crucible equipped with anhydrous calcium chloride, the bottom of the corundum casing is provided with logical Hole makes corundum crucible form two electrode districts, respectively as sun so that anhydrous calcium chloride enters the corundum casing through through-hole Polar region and cathodic region；Electrolytic furnace is led into ar purging and Continuous aeration atmosphere again, to ensure argon gas atmosphere, temperature is increased and controls 800~1050 DEG C, obtain molten salt body；Then it is inserted into anode region using graphite electrode as anode, using metal electrode bar as cathode It is inserted into cathodic region, and the DC voltage for applying 2.8V carries out preelectrolysis 2h between anode and cathode.
5) metal electrode bar is taken out, the assembly cathode that step 3) obtains is placed in cathodic region, applies 3.1V DC voltages It is electrolysed between anode and cathode；Up to Faradaic current reduces and stablizes to the background current stage of 0.2A or so and there is no drops Low trend can stop being electrolysed, and stop being electrolysed and take out assembly cathode, be placed in argon gas atmosphere and naturally cooled to electrolytic furnace Room temperature, the assembly cathode after being electrolysed.
6) bulk sample is removed from the assembly cathode after electrolysis, after washing away the attachment of residual on it with clear water, It is placed in 105 DEG C of baking ovens and dries 10h, obtain Titanium.
Crucible after experiment is as shown in Fig. 3-a.
Embodiment two：
The present embodiment selects purity to be >=99.8% and cross the TiO of 140 mesh sieve2Powder, by the way of corundum casing come Anode and cathode fused salt is isolated, the structure of electrolytic cell is as shown in Fig. 2, steps are as follows：
1) by TiO2Powder steel die is by material cold moudling, and unidirectional to suppress, pressing pressure is 2.5~5MPa, is protected The pressure time is 1~10s, demoulds bulk sample is made later.
2) bulk sample made from step 1) is placed in 3~5h of sintering in Muffle furnace in air atmosphere；The Muffle furnace Temperature control at 900~1200 DEG C.
3) sintered bulk sample in the step 2) is tied up with wire in steel electrode bar, obtains assembly cathode, It is spare.
4) corundum casing is placed in the corundum crucible equipped with anhydrous calcium chloride, the bottom of the corundum casing is provided with logical Hole makes corundum crucible form two electrode districts, respectively as sun so that anhydrous calcium chloride enters the corundum casing through through-hole Polar region and cathodic region；Electrolytic furnace is led into ar purging and Continuous aeration atmosphere again, to ensure argon gas atmosphere, temperature is increased and controls 800~1050 DEG C, obtain molten salt body；Then it is inserted into anode region using graphite electrode as anode, using metal electrode bar as cathode It is inserted into cathodic region, and the DC voltage for applying 2.8V carries out preelectrolysis 2h between anode and cathode.
5) metal electrode bar is taken out, the assembly cathode that step 3) obtains is placed in cathodic region, applies 3.1V DC voltages It is electrolysed between anode and cathode；Up to Faradaic current reduces and stablizes to the background current stage of 0.2A or so and there is no drops Low trend can stop being electrolysed, and stop being electrolysed and take out assembly cathode, be placed in argon gas atmosphere and naturally cooled to electrolytic furnace Room temperature, the assembly cathode after being electrolysed.
6) bulk sample is removed from the assembly cathode after electrolysis, after washing away the attachment of residual on it with clear water, It is placed in 105 DEG C of baking ovens and dries 10h, obtain Titanium.
Crucible after experiment is as shown in Fig. 3-b.
Embodiment three：
The present embodiment selects purity to be >=99.8% and cross the TiO of 140 mesh sieve2Powder, by the way of corundum casing come Anode and cathode fused salt is isolated, the structure of electrolytic cell is as shown in Fig. 2, steps are as follows：
1) by TiO2Powder steel die is by material cold moudling, and unidirectional to suppress, pressing pressure is 2.5~5MPa, is protected The pressure time is 1~10s, demoulds bulk sample is made later.
2) bulk sample made from step 1) is placed in 3~5h of sintering in Muffle furnace in air atmosphere；The Muffle furnace Temperature control at 900~1200 DEG C.
3) sintered bulk sample in the step 2) is tied up with wire in steel electrode bar, obtains assembly cathode, It is spare.
4) corundum casing is placed in the corundum crucible equipped with anhydrous calcium chloride, the bottom of the corundum casing is provided with logical Hole makes corundum crucible form two electrode districts, respectively as sun so that anhydrous calcium chloride enters the corundum casing through through-hole Polar region and cathodic region；Electrolytic furnace is led into ar purging and Continuous aeration atmosphere again, to ensure argon gas atmosphere, temperature is increased and controls 800~1050 DEG C, obtain molten salt body；Then it is inserted into anode region using graphite electrode as anode, using metal electrode bar as cathode It is inserted into cathodic region, and the DC voltage for applying 2.8V carries out preelectrolysis 2h between anode and cathode.
5) metal electrode bar is taken out, the assembly cathode that step 3) obtains is placed in cathodic region, applies 3.1V DC voltages It is electrolysed between anode and cathode；Up to Faradaic current reduces and stablizes to the background current stage of 0.2A or so and there is no drops Low trend can stop being electrolysed, and stop being electrolysed and take out assembly cathode, be placed in argon gas atmosphere and naturally cooled to electrolytic furnace Room temperature, the assembly cathode after being electrolysed.
6) bulk sample is removed from the assembly cathode after electrolysis, after washing away the attachment of residual on it with clear water, It is placed in 105 DEG C of baking ovens and dries 10h, obtain Titanium.
Crucible after experiment is as shown in Fig. 3-a.
Obtained sample progress XRD objects are mutually detected and sem analysis, the information such as form, the structure of Titanium can be measured. Fig. 5 is the XRD diagram of the Titanium obtained of the present embodiment.
Fig. 1 is the crucible sectional view after plain electrolysers electrolysis, is electrolysed TiO2After it can be found that after cooling CaCl2On have one layer of black carbon black color substance, electrolysis when, the material floats of this layer of carbon black color above fused salt, If being directly connected to anode and cathode, it will cause the short circuits between anode and cathode, and certain electric current is caused to waste.And such carbon The presence of black substance can make the fused salt after electrolysis contaminated, it is difficult to reuse.Fig. 2 is by the way of corundum casing The fused salt region of anode and cathode is separated, blocks the black floating material above fused salt by the direct short circuit of anode and cathode with this.
Fig. 3-a to Fig. 3-c are respectively using the crucible figure after corundum casing.Using can be effectively isolated really after casing Open the floating material generated on fused salt surface when electrolysis.Atrament after corundum casing is just swum within casing, other areas Domain relative clean.Atrament after anode casing does not swim in anode region, is effectively protected the molten of anode region Salt.
Fig. 4 is the time current curve comparison figure implemented electrolysis using comparative example and be electrolysed using the present invention. In order to carry out the comparison of current efficiency, following formula is introduced below：
η is current efficiency in formula
QTFor theoretical consumption electricity
QAFor actual consumption electricity, practical electricity is calculated by the integral to time current curve
Assuming that the sample obtained after electrolysis does not have difference, i.e., the theory that theoretically sample of electrolysis to same degree is consumed Electricity QAIt is identical.And in the electricity of actual consumption, the integral area of electric current and time graph is smaller, and the electricity consumed is got over Small, current efficiency η is bigger.It is analyzed according to the current-time curvel in Fig. 4, whether corundum casing or anode casing, the time The integral area of current curve can all be less than the area of not casing, so under the structure of casing, current efficiency improves. According to the experimental phenomena of front, casing is followed every can play the role of separating anode and cathode fused salt really, to a certain extent to cathode Certain restriction effect is played in side reaction, and the carbon dust that side reaction may generate is blocked only in cathode zone, reduces fused salt In electronic conduction, to reduce wasting for electric current in fused salt.
In conclusion the present invention have it is following prominent a little：First, alumina material is directly added for anode and cathode to be isolated Fused salt region, method is simple；Second, the conductive floating material for avoiding fused salt upper black is directly connected to anode and cathode and causes electric current Waste, to improve current efficiency.Third controls the range of the flowing of black floating material, it is right to have efficiently controlled it Pollution of the fused salt with being electrolysed sample.
It can be seen that the present invention has method simple, the features such as significant effect, prepares Titanium for FFC methods and improve certain electricity Stream efficiency and the diffusion for controlling black pollution object, are effectively prevented from its pollution to fused salt and sample.
In addition, the electrode district isolator of the present invention also can be replaced corundum plate, in the corundum plate, lower part be provided with it is logical Hole.
The above embodiment of the present invention is only example to illustrate the invention, and is not the implementation to the present invention The restriction of mode.For those of ordinary skill in the art, other can also be made not on the basis of the above description With the variation and variation of form.Here all embodiments can not be exhaustive.It is every to belong to technical scheme of the present invention Row of the changes and variations that derived from still in protection scope of the present invention.

Claims (10)

1. a kind of molten-salt electrolysis TiO2The method for preparing Titanium, which is characterized in that use the electrode district isolator of corundum material will Fused salt is isolated into Yang Qu and cathodic region, makes TiO2It is placed in cathodic region and is electrolysed.
2. molten-salt electrolysis TiO according to claim 12The method for preparing Titanium, which is characterized in that include the following steps：
1) by TiO2Powder is simultaneously unidirectionally cold-pressed compression moulding, and bulk sample is made；
2) bulk sample made from step 1) is placed in 3~5h of sintering in Muffle furnace in air atmosphere；The temperature of the Muffle furnace Degree control is at 900~1200 DEG C；
3) sintered bulk sample in the step 2) is fixed on steel electrode bar, obtains assembly cathode, it is spare；
4) the electrode district isolator is placed in the corundum crucible equipped with anhydrous calcium chloride, the bottom of the electrode district isolator Portion is provided with the through-hole people, so that anhydrous calcium chloride penetrates the electrode district isolator, so that corundum crucible is formed two electrode districts, respectively As anode region and cathodic region；Electrolytic furnace is led into ar purging and Continuous aeration atmosphere again, to ensure argon gas atmosphere, increases temperature simultaneously Control obtains molten salt body at 800~1050 DEG C；Then it is inserted into anode region using graphite electrode as anode, is made with metal electrode bar It is inserted into cathodic region for cathode, and applies DC voltage and carries out preelectrolysis between anode and cathode；
5) metal electrode bar is taken out, the assembly cathode that step 3) obtains is placed in cathodic region, applies DC voltage in anode and cathode Between be electrolysed；Until Faradaic current reduces and stablizes to 0.2A, stop being electrolysed and take out assembly cathode, it is placed in argon gas atmosphere In with electrolytic furnace cooled to room temperature, the assembly cathode after being electrolysed；
6) bulk sample is removed from the assembly cathode after electrolysis, after washing away the attachment of residual on it with clear water, is placed in It is dried in baking oven, obtains Titanium.
3. molten-salt electrolysis TiO according to claim 22The method for preparing Titanium, which is characterized in that unidirectional in step 1) The pressure of cold pressing compacting is 2.5~5MPa, and the dwell time is 1~10s.
4. molten-salt electrolysis TiO according to claim 22The method for preparing Titanium, which is characterized in that described in step 1) TiO2Purity >=99.8% of powder.
5. according to the molten-salt electrolysis TiO described in claim 22The method for preparing Titanium, which is characterized in that the electrode district Isolator is the pipe sleeve of upper end opening or the corundum plate adaptable with the corundum crucible interior shape.
6. according to the molten-salt electrolysis TiO described in claim 22The method for preparing Titanium, which is characterized in that the argon gas Purity is not less than 99.99%.
7. according to the molten-salt electrolysis TiO described in claim 22The method for preparing Titanium, which is characterized in that in step 5), Temperature when electrolysis is controlled at 900~1050 DEG C.
8. according to the molten-salt electrolysis TiO described in claim 22The method for preparing Titanium, which is characterized in that in step 4), institute The DC voltage for stating application is 2.8V, electrolysis time 2h.
9. according to the molten-salt electrolysis TiO described in claim 22The method for preparing Titanium, which is characterized in that it is characterized in that, The DC voltage applied in step 5) is 3.1V.
10. according to the molten-salt electrolysis TiO described in claim 22The method for preparing Titanium, which is characterized in that dried in step 6) Box temperature degree is 105 DEG C, soaking time 10h.
CN201810607896.8A 2018-06-13 2018-06-13 A kind of molten-salt electrolysis TiO2The method for preparing Titanium Pending CN108441893A (en)

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