CN110042433A - A kind of industrialized preparing process of titaniferous solubility solid solution anode - Google Patents
A kind of industrialized preparing process of titaniferous solubility solid solution anode Download PDFInfo
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- CN110042433A CN110042433A CN201910380166.3A CN201910380166A CN110042433A CN 110042433 A CN110042433 A CN 110042433A CN 201910380166 A CN201910380166 A CN 201910380166A CN 110042433 A CN110042433 A CN 110042433A
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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
Abstract
The present invention relates to a kind of industrialized preparing process of titaniferous solubility solid solution anode, belong to titanium technical field of smelting.The present invention includes fusing whipping step, cast molding step, cooling step and shaping step.Use titaniferous solubility solid solution for raw material in the present invention; liquid is fused under conditions of being higher than the temperature of raw material fusing point and having inert atmosphere protection and is sufficiently stirred; then melt is poured into cast molding in the mold for be preheating in advance 1000 DEG C or more; and it is cooling with certain cooling rate under inert atmosphere protection; anode after cooling can be directly used for molten-salt electrolysis production Titanium after integer is handled.Titaniferous solubility solid solution anode industrialized preparing process of the invention, it is simple process, high-efficient, at low cost, and the anode produced has many advantages, such as big density, good conductivity, internal zero defect.Molten-salt electrolysis is carried out using the anode of this industrialized production and prepares Titanium, it can be achieved that anode long-time stable dissolves out, and electrolytic process Anodic is not scaling-off, anodic electrochemical dissolution efficiency is 90% or more.
Description
Technical field
The present invention relates to titanium technical field of smelting, in particular to a kind of industrialized production of titaniferous solubility solid solution anode
Method.
Background technique
Titanium has excellent physical chemistry and mechanical performance.Its density is about the 60% of steel, but specific strength height compares
Steel double it is above, and the fusing point of Titanium it is high, it is corrosion-resistant and have good bio-compatibility, be widely used in military project, boat
The fields such as empty space flight, chemical industry, medical implantation, electronic information, are known as " the following metal ".Titanium elements reserves in the earth's crust are extremely rich
Rich (0.44%, the is arranged in all elements 9), but the yield of titanium and sales volume are very limited (producing per year less than 200,000 tons in the whole world).Mesh
The mainstream production technology of preceding Titanium is Kroll method, i.e. magnesium reduction.It is reducing agent that its core, which is with magnesium metal, 800~
Gaseous titanium tetrachloride is restored at 900 DEG C, obtains the titanium sponge that purity is 99.7% or so.The flow process is cumbersome, complicated and energy
Consumption is big, so as to cause Titanium high production cost, expensive, limits the extensive use of Titanium.
To reduce titanium sponge price, in past nearly 70 years, the metallurgists of countries in the world are multi-faceted seek it is new
Inexpensive Titanium smelting process.In all multi-methods having already appeared, Chinese invention patent ZL200510011684.6 and
ZL201310421132.7 discloses a kind of method that titaniferous solubility solid solution anode electrolysis produces pure titanium.With traditional metal
Titanium production method (Kroll method) is compared, and this method has many advantages, such as that simple process, process are short, at low cost, pollution is small, is recognized
For be hopeful very much realize industrially scalable extract Titanium a kind of new process.The core of process industryization application is closed
Key, be how high efficiency, low cost ground industrialized production large size titaniferous solubility solid solution anode.To solve this problem, above-mentioned two
Compression molding-high temperature sintering anode moulding process is proposed in a patent, and obtains success in bench scale.However into
It is found during the scale-up of one step, compression molding-high-sintering process is difficult to produce large scale anode, and sintering process
Temperature schedule is required very stringent, it is necessary to which slow heating-cooling, production cycle are longer.
After the method for learning the pure titanium of electrolysis production of above-mentioned Chinese invention patent proposition, the meaning of DuPont Corporation's acumen
Knowing industrialized production solubility solid solution anode is the key that entire technique success or failure, and in United States Patent (USP) US7628937B2
Propose the soluble solid solution anode preparation method of kneading-extrusion forming-high temperature sintering.This method is with TiO2It is restored with carbonaceous
Agent is raw material, using cellulose or pitch as additive, first prepares TiO by kneading-extrusion forming method2- C green compact, so
It is reduced to titaniferous solubility solid solution at 1800 DEG C afterwards and sinters anode into turn.This method the biggest problems are that: (1)
After cellulose or asphalt additive are carbonized at high temperature, additional carbon can be brought, causes the ingredient of titaniferous solubility solid solution difficult
Accurately to control；(2)TiO2With carbonaceous reducing agent in reaction, bulk gas can be released, this will lead to after sintering in anode
Portion is there are many stomatas, and the anode density prepared is lower, and resistivity is also larger.This anode is when being electrolysed, not only
Tank voltage is higher, and while being electrolysed is easy scaling-off, and anodic electrochemical dissolution efficiency is relatively low, and only 80% or so.In addition, this method
Still unresolved strict demand of the sintering process to slow heating-cooling, the production cycle is equally longer, generally in 3~5 days/heat.
Also the electrolytic method that a kind of titanium soluble anode was once referred in Chinese invention patent ZL201510408576.6, uses
Anode be particle of the granularity less than 74 μm and to be simply stacked in a porous insulation basketry.Although this anode construction is easy,
But maximum problem be in addition to metal titanium or titanium alloy is the anode of raw material, cannot be real by the anode of raw material of soluble solid solution
Existing long-time stable dissolution can not continue to protect between soluble solid solution pellet because constantly dissolving as electrolysis carries out anode
Good electrical contact is demonstrate,proved, so that tank voltage increases rapidly simultaneously final open circuit after electrolysis 1~3 hour, causes electrolytic process can not
Continue.
Summary of the invention
Set forth above to solve the problems, such as, the present invention provides a kind of industrialized production side of titaniferous solubility solid solution anode
Method.It is an object of the present invention to which providing one kind for the technique that soluble solid solution anode electrolysis produces pure titanium is easy to extensive work
Industry metaplasia produces the approach of anode, fills up the blank of technology.Using method provided by the invention, can not only it is simple, efficient, low at
Native industry metaplasia produces large scale solubility solid solution anode, and the anode produced has density big, good conductivity, interior
The advantages that portion's zero defect.Molten-salt electrolysis is carried out using the anode of this industrialized production and prepares Titanium, it can be achieved that when anode is long
Between stablize dissolution, and electrolytic process Anodic is not scaling-off, and anodic electrochemical dissolution efficiency is 90% or more.
The present invention is achieved through the following technical solutions:
A kind of industrialized preparing process of titaniferous solubility solid solution anode, comprising the following steps:
(1) it melts whipping step: using titaniferous solubility solid solution for raw material, be higher than 50~500 DEG C of raw material fusing point
Temperature and has and be fused into liquid under conditions of inert atmosphere protection and 5~60min is sufficiently stirred；
(2) melt after being sufficiently stirred cast molding step: is poured into the prior mold for being preheating to 1000 DEG C or more
Mold is carried out the pre-heat treatment here by middle cast molding, be rapid heat cycle when casting in order to prevent cause anode crack or
Person's crack of die；
(3) temperature control cooling step: by the good anode of cast molding with mold, with certain under inert atmosphere protection
Cooling rate is cooled down；
(4) shaping step: after being cooled to room temperature, anode is demoulded and takes out and carries out integer, here, to anode through row
Integer is to remove the sanding burr of anode surface, or be processed into required shape with mach mode.
Further, titaniferous solubility solid solution described in the step (1) includes titanium monoxide (TiO), titanium carbide
(TiC), oxidation of coal titanium (TiCxOy, x+y=1), titanium carbonitride (TiCxNz, x+z=1), carbon titanium oxynitrides (TiCxOyNz, x+y
+ z=1), titanium oxynitrides (TiOyNz, y+z=1), one or more of titanium nitride (TiNz, 0 < z≤1).
Further, inert atmosphere described in the step (1) and step (3) includes vacuum atmosphere, nitrogen atmosphere, argon gas
One or more of atmosphere, helium atmosphere.
Further, agitating mode described in the step (1) includes Gas Stirring, magnetic agitation, mechanical stirring, centrifugation
One of stirring or various ways are mixed.
Further, the material selection metal of mold described in the step (2), preferably stainless steel, carbon steel, Titanium and
Its alloy, metallic nickel and its alloy particularly cannot select sand mo(u)ld and graphite material mold.
Further, the control of cooling rate described in the step (3) is at 10~500 DEG C/h.
Compared with prior art, technical effect beneficial brought by the present invention is shown:
1, the industrialized preparing process of a kind of titaniferous solubility solid solution anode of the invention, for soluble solid solution anode
The technique of the pure titanium of electrolysis production provides a kind of approach for being easy to large-scale industrial production anode, fills up the blank of technology.Together
When, it, can not only simple, industrialized production large scale solubility solid solution efficiently at low cost using method provided by the invention
Body anode, and the anode produced has many advantages, such as big density, good conductivity, internal zero defect.Using this industrialization
The anode of production carries out molten-salt electrolysis and prepares Titanium, it can be achieved that anode long-time stable dissolves out, and electrolytic process Anodic is not
Scaling-off, anodic electrochemical dissolution efficiency is 90% or more.
2, the present invention will be stirred after titaniferous solubility solid solution melting sources, be advantageous in that in fusing whipping step:
One is omitted green compact molding link, and simplified technique avoids the use of binder, additive etc. while reducing cost, thus
Ensure the accuracy of anode components；Second is that relaxing the requirement to temperature schedule, it can be rapidly heated, thus greatly
Shortening the production cycle, (compared with high temperature sintering methods, 80%) every heat time at least shortens, and greatly improves production effect
Rate；Third is that while non-uniform components, the solid inclusions in raw material is also allowed to float or sink and divide with raw material by stirring
From to improve anode purity.
It 3,, not only can be with the production large scale of simple and effective using cast molding combination temperature control cooling step in the present invention
Anode, and the defects of ensure that anode interior pore-free.The anode density produced in this way is big, good conductivity, is using
Can accomplish in the process long-time stable dissolution and it is not scaling-off, to improve the electrochemical dissolution efficiency of anode.
4, the present invention is specific to select metal material mold without selecting sand mo(u)ld and graphite mo(u)ld in cast molding step
Tool, is based on the considerations of anode purity and overall cost.Under cast temperature, do not sent out between selected metal material mold and anode material
Raw reaction；And graphite jig can then be reacted with anode material, cause anode components uncontrollable, and mold can then occur as sand mo(u)ld
Grain (gravel) falls off the phenomenon being mixed into anode, and the two can pollute anode.In terms of cost, although metal material mold
Processing charges is higher, but there is no abrasion condition and mould strength it is sufficiently high, it is basic not have to maintenance and finishing, therefore service life
Much higher than sand mo(u)ld and graphite jig, overall cost is lower instead.
Specific embodiment
The specific embodiment of form by the following examples makees further specifically above content of the invention
It is bright.Embodiment illustrates but does not limit the present invention.
Embodiment 1:
50kg oxidation of coal titanium (TiCxOy, x+y=1,1950~2050 DEG C of fusing point) is weighed, in half an hour under vacuum atmosphere
It is inside warming up to 2400 DEG C and is fused into liquid and magnetic agitation 10min to uniform state, heat preservation stands 20min, then falls melt
Enter the cylindrical electrode that 200 × 350mm of Φ is cast into the stainless steel mould for have been preheated with 1000 DEG C, and under vacuum conditions
Room temperature is cooled to 240 DEG C/h of cooling velocity.Total production cycle is 11 hours time-consuming, wherein heating and cooling time-consuming 11 are small
When.Anode demoulding after cooling removes flash removed through surface polishing, Archimedes method is used to measure the density of this anode as 4.9g/
cm3, four probe method is used to measure the room temperature resistivity of this anode as 1.84 μ Ω m.
Using this anode as electrode, stainless steel plate makees cathode, in KCl-NaCl fused salt mixt, using China at 750 DEG C
The method progress pure titanium of electrolysis production of patent ZL200510011684.6, electrolysis time 48 hours.After electrolysis, anode is taken out
Anode scrap, discovery anode scrap profile keep initial rules shape, illustrate that the anode can realize that long-time stable dissolves out；It is washed with deionized water
Then net anode residue pole surface bur dries, weighs, be computed and find that the electrochemical dissolution efficiency of the anode is 94%.
Embodiment 2:
Weigh 25kg titanium carbide (TiC, 3015 DEG C of fusing point) and 25kg titanium monoxide (TiO, 1750 DEG C of fusing point), mechanical mixture
40min is stirred to being uniformly mixed in being warming up to 2400 DEG C in half an hour and be fused into liquid and argon gas under an argon atmosphere afterwards, heat preservation
20min is stood, then melt is poured into the circle for being cast into 200 × 350mm of Φ in the stainless steel mould for have been preheated with 1000 DEG C
Cylindrical electrode, and room temperature is cooled to 240 DEG C/h of cooling velocity under the protection of argon gas.Total production cycle is time-consuming
11.5 hours, wherein heating and cooling are 11.5 hours time-consuming.Anode demoulding after cooling is removed flash removed through surface polishing, is used
The density that Archimedes method measures this anode is 4.7g/cm3, four probe method is used to measure the room temperature resistivity of this anode as 1.96
μΩ·m。
Using this anode as electrode, stainless steel plate makees cathode, in KCl-NaCl fused salt mixt, uses at 750 DEG C
The method progress pure titanium of electrolysis production of state patent ZL200510011684.6, electrolysis time 48 hours.After electrolysis, sun is taken out
Pole anode scrap, discovery anode scrap profile keep initial rules shape, illustrate that the anode can realize that long-time stable dissolves out；Use deionized water
Anode residue pole surface bur is cleaned, then dries, weigh, is computed and finds that the electrochemical dissolution efficiency of the anode is 93%.
Comparative example 1:
50kg oxidation of coal titanium (TiCxOy, x+y=1,1950~2050 DEG C of fusing point) is weighed, with the polyethylene glycol of 1% concentration
It (PEG) is binder, referring to the step of being announced in United States Patent (USP) US7628937B2, using kneading-extrusion forming-high temperature sintering
Method prepares anode, specific steps are as follows: by oxidation of coal titanium and binder in kneader kneading 120min, be then squeezed into Φ
The cylindrical green body of 200 × 350mm；Green compact are dried 72 hours at 120 DEG C, sufficiently to remove the moisture in green compact, then
After being warming up to 1800 DEG C, heat preservation 1 hour under argon atmosphere protection with the heating rate of 30 DEG C/min, then with 240 DEG C/h
Cooling velocity is cooled to room temperature.Total production cycle is 142.5 hours time-consuming, wherein heating and cooling are 68.5 hours time-consuming.After cooling
Anode use Archimedes method to measure density as 3.8g/cm3, four probe method is used to measure room temperature resistivity as 3.06 μ Ω
m。
Using this anode as electrode, stainless steel plate makees cathode, in KCl-NaCl fused salt mixt, uses at 750 DEG C
The method progress pure titanium of electrolysis production of state patent ZL200510011684.6, electrolysis time 48 hours.After electrolysis, sun is taken out
Pole anode scrap, discovery anode scrap profile keep initial rules shape substantially, illustrate that the anode can realize that long-time stable dissolves out；Spend from
Sub- water cleans anode residue pole surface bur, and discovery anode scrap has a small amount of scaling-off in cleaning process；Drying, weighing after anode scrap is cleaned,
It is computed and finds that the electrochemical dissolution efficiency of the anode is 87%.
Comparative example 2:
Weigh 65.6kg TiO2, 17.7kg high purity graphite, using cellulose as additive, with the polyethylene glycol of 1% concentration
(PEG) solution is binder, prepares anode, specific steps fully according to the method announced in United States Patent (USP) US7628937B2 are as follows:
By TiO2, high purity graphite and 2.5kg cellulose mixed in three-dimensional material mixer 2 hours, then mixture and binder are being pinched
Kneading 120min in conjunction machine, is then squeezed into the cylindrical green body of 200 × 350mm of Φ；It is small that green compact are dried to 72 at 120 DEG C
When, sufficiently to remove the moisture in green compact, 1800 then are warming up to the heating rate of 30 DEG C/min under argon atmosphere protection
DEG C, after heat preservation 1 hour, then room temperature is cooled to 240 DEG C/h of cooling velocity.Total production cycle is 144.5 hours time-consuming,
Middle heating and cooling are 68.5 hours time-consuming.There are many holes in anode surface after cooling, measures density using Archimedes method
For 2.3g/cm3, four probe method is used to measure room temperature resistivity as 4.98 μ Ω m.
Using this anode as electrode, stainless steel plate makees cathode, in KCl-NaCl fused salt mixt, uses at 750 DEG C
The method progress pure titanium of electrolysis production of state patent ZL200510011684.6, electrolysis time 48 hours.After electrolysis, sun is taken out
Pole anode scrap, the profile that discovery anode scrap immerses salt face or less part locally have defect, but the whole basic holding original shape of anode scrap, say
The bright anode can still be realized and be dissolved out for a long time；It is washed with deionized water anode residue pole surface bur, is found in cleaning process residual
Pole has a certain amount of scaling-off；Drying, weighing after anode scrap is cleaned are computed and find that the electrochemical dissolution efficiency of the anode is 81%.
The result of above-described embodiment and comparative example explanation can be simple, high using industrialized preparing process of the invention
Effect produces large scale solubility solid solution anode at low cost, and the anode density produced is bigger, electric conductivity is more preferable,
Internal zero defect.The anode produced using the method for the present invention is carried out molten-salt electrolysis and prepares Titanium, and anode can be with long-time stable
Dissolution, and it is not scaling-off in electrolytic process, anodic electrochemical dissolution is more efficient.
It should be noted that those skilled in the art are that this hair may be implemented completely according to the various embodiments described above of the present invention
Bright independent claims and the full scope of appurtenance, realize process and the same the various embodiments described above of method；And the present invention is not
It elaborates and partly belongs to techniques well known.
The above, part specific embodiment only of the present invention, but scope of protection of the present invention is not limited thereto, appoints
In the technical scope disclosed by the present invention, any changes or substitutions that can be easily thought of, should all cover by what those skilled in the art
Within protection scope of the present invention.
Claims (6)
1. a kind of industrialized preparing process of titaniferous solubility solid solution anode, which comprises the following steps:
(1) fusing stirring: using titaniferous solubility solid solution for raw material, in the temperature higher than 50~500 DEG C of raw material fusing point and has
It is fused into liquid under conditions of inert atmosphere protection and 5~60min is sufficiently stirred；
(2) cast molding: the melt after being sufficiently stirred is poured into the mold for be preheating in advance 1000 DEG C or more and is cast into
Mold is carried out the pre-heat treatment here by type, is that rapid heat cycle when casting in order to prevent causes anode crack or mold to be opened
It splits；
(3) temperature control is cooling: by the good anode of cast molding with mold, with certain cooling rate under inert atmosphere protection
It is cooled down；
(4) integer: after being cooled to room temperature, anode is demoulded and takes out and carries out integer, here, to anode through row integer, is
The sanding burr of anode surface is removed, or be processed into required shape with mach mode.
2. a kind of industrialized preparing process of titaniferous solubility solid solution anode as described in claim 1, which is characterized in that institute
State titaniferous solubility solid solution described in step (1) include titanium monoxide (TiO), titanium carbide (TiC), oxidation of coal titanium (TiCxOy,
X+y=1), titanium carbonitride (TiCxNz, x+z=1), carbon titanium oxynitrides (TiCxOyNz, x+y+z=1), titanium oxynitrides
One or more of (TiOyNz, y+z=1), titanium nitride (TiNz, 0 < z≤1).
3. a kind of industrialized preparing process of titaniferous solubility solid solution anode as described in claim 1, which is characterized in that institute
Stating inert atmosphere described in step (1) and step (3) includes vacuum atmosphere, nitrogen atmosphere, argon atmosphere, one in helium atmosphere
Kind is several.
4. a kind of industrialized preparing process of titaniferous solubility solid solution anode as described in claim 1, which is characterized in that institute
Stating agitating mode described in step (1) includes one of Gas Stirring, magnetic agitation, mechanical stirring, centrifugal mixer or a variety of
Mode is mixed.
5. a kind of industrialized preparing process of titaniferous solubility solid solution anode as described in claim 1, which is characterized in that institute
State the material selection metal of mold described in step (2), including stainless steel, carbon steel, Titanium and its alloy, metallic nickel and its conjunction
Gold cannot select sand mo(u)ld and graphite material mold.
6. a kind of industrialized preparing process of titaniferous solubility solid solution anode as described in claim 1, which is characterized in that institute
The control of cooling rate described in step (3) is stated at 10~500 DEG C/h.
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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 |
| CN114672849A (en) * | 2022-04-29 | 2022-06-28 | 中国原子能科学研究院 | Rapid casting method of molten salt electrolysis metal |
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