CN102912379A - Method for preparing metal titanium - Google Patents
Method for preparing metal titanium Download PDFInfo
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- CN102912379A CN102912379A CN2012104121006A CN201210412100A CN102912379A CN 102912379 A CN102912379 A CN 102912379A CN 2012104121006 A CN2012104121006 A CN 2012104121006A CN 201210412100 A CN201210412100 A CN 201210412100A CN 102912379 A CN102912379 A CN 102912379A
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- titanium
- preparing metal
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Abstract
The invention provides a method for preparing metal titanium. The method comprises the steps of: mixing, pressing and drying titanium oxide and a carbon reducing agent to obtain an anode material; and connecting the anode material with the electric conductive part to form an anode, taking metal or alloy as a cathode, taking alkali metal chloride fused metal and/or alkaline earth chloride fused salt as an electrolyte for electrolysis under an inert atmosphere to obtain the metal titanium powder. The electrolyte further contains TiCl2 (titanium dichloride) and TiCl3 (titanium trichloride). The method provided by the invention has the advantage of low energy consumption.
Description
Technical field
The present invention relates to fused salt electrolysis and prepare the metal titanium technical field, more particularly, relate to a kind of take the method for titanyl compound as raw material direct production metallic titanium powder.
Background technology
Metal titanium is as a kind of new metal, have low density, good solidity to corrosion and a series of advantageous properties such as plasticity-, high specific strength, be widely used in the fields such as aerospace, man-made satellite, military project, chemical industry, oil, metallurgy, light industry, electric power, sea water desaltination, naval vessels, weaving and medical treatment, so it is described as the metal of 21 century.
At present, the industrial process of titanium sponge still is magnesium reduction process, and this technique comprises: titanium mineral is produced TiCl through enrichment-chlorination-rectifying
4, then in argon or helium inert atmosphere, use magnesium reduction TiCl
4Behind titanium sponge, carry out the vacuum distilling separation and remove magnesium and MgCl
2, be the finished product titanium sponge finally by product finishing processing.The method production capacity is large, easily realizes commercialization, so up to the present also there is not other technique to substitute.Yet a series of shortcomings such as the existing long flow path of this technique, the cycle is long, reduction ratio is low, the reductive agent price is higher, the difficult realization serialization of process cause cost of sponge Titanium too high.
The research of preparation metal titanium method is had a variety of, more representative as: the PRP technique that the OS method that the FFC method that univ cambridge uk proposes, Kyoto Univ Japan propose, the Okabe of Japan etc. proposes, fluotitanate reduction etc.Yet these methods all exist at present still unvanquishable technical problem, so all do not realize industrialization.
The method that a kind of sosoloid anode TiOmTiC Direct Electrolysis with metallic conductivity prepares pure titanium that the invention provides is disclosed in the Chinese invention patent application of publication number CN1712571A, sosoloid anode TiOmTiC in the method is with carbon and titanium dioxide or take titanium carbide and titanium dioxide as raw material, be mixed into powder by the chemical reaction metering, then compression moulding, vacuum reaction is made in 600 ℃～1600 ℃ temperature range.The method has the advantages such as technique is simple, electrolytic process carries out continuously, but the method need to prepare sosoloid TiOmTiC under the condition of high-temperature vacuum, and therefore, energy consumption is higher.
Publication number is that the american documentation literature of US7410562B2 discloses a kind of TiO of using
2-C composite anode prepares the method for metal titanium, and the method is the method that the thermal and electrochemical process combines, and its main points are to heat-treat with carbon and titanyl compound, forms TiC
xO
yComposite anode is then with this TiC
xO
yComposite anode carries out fused salt electrolysis as soluble anode, obtains metal titanium at negative electrode.The method has similar relative merits with above-mentioned Chinese invention patent application, that is, the method need to be carried out thermal reduction equally and be prepared composite anode under high-temperature vacuum, so the energy consumption of the method is still higher.
Summary of the invention
For the high deficiency of energy consumption that above-mentioned prior art exists, one of purpose of the present invention is to provide a kind of method by fused salt electrolysis process less energy-consumption ground production metallic titanium powder.
An aspect of of the present present invention provides a kind of method for preparing metal titanium, said method comprising the steps of: with titanyl compound and carbonaceous reducing agent mix, suppress, dry to obtain the anode material; The anode material is connected to consist of anode with electric-conductor, with metal or alloy as negative electrode, take alkali metal chloride fused salt and/or alkaline earth metal chloride fused salt as ionogen, under inert atmosphere, carry out electrolysis, to make metallic titanium powder, wherein, described ionogen also contains TiCl
2And TiCl
3
In one exemplary embodiment of the present invention, what described titanyl compound can be in titanium dioxide, five oxidation Tritanium/Trititaniums, titanium sesquioxide and the titanium monoxide is at least a.
In one exemplary embodiment of the present invention, described titanyl compound and carbonaceous reducing agent can have can be by the granularity of 200 mesh sieves.
In one exemplary embodiment of the present invention, what described carbonaceous reducing agent can be in graphite, carbon black and the refinery coke is at least a.
In one exemplary embodiment of the present invention, in the described titanyl compound in Sauerstoffatom and the carbonaceous reducing agent number ratio of carbon atom can be 2:1 ~ 1:1.
In one exemplary embodiment of the present invention, described negative electrode can be carbon steel rod, molybdenum bar or titanium rod.
In one exemplary embodiment of the present invention, described method can also comprise anodic current density is controlled to be 0.025A/cm
2~ 0.75A/cm
2, cathode current density is controlled to be 0.1A/cm
2~ 2A/cm
2
In one exemplary embodiment of the present invention, described TiCl
2And TiCl
3Accounting for described electrolytical massfraction can be 0.4% ~ 3%, and wherein the atom number ratio of divalence titanium and titanous can be 1:5 ~ 1:0.5.
Compared with prior art, method of the present invention can be with the mixture of titanyl compound and carbonaceous reducing agent in the situation that carry out fused salt electrolysis without the high-temperature vacuum thermal reduction as anode, thereby made metallic titanium powder, have advantages of that energy consumption is low.
Embodiment
Hereinafter, describe the method for preparing metal titanium of the present invention in detail in connection with exemplary embodiment.
In one exemplary embodiment of the present invention, the method for preparing metal titanium may further comprise the steps:
With titanyl compound and carbonaceous reducing agent mix, suppress, dry to obtain the anode material;
The anode material is connected to consist of anode with electric-conductor, with metal or alloy as negative electrode, take alkali metal chloride fused salt and/or alkaline earth metal chloride fused salt as ionogen, under inert atmosphere, carry out electrolysis, to make metallic titanium powder, wherein, described ionogen also contains TiCl
2And TiCl
3Here, electric-conductor is the device that the anode material can be electrically connected with power supply, for example, can be conducting rod or conductive filament etc.
In another exemplary embodiment of the present invention, what titanyl compound can be in titanium dioxide, five oxidation Tritanium/Trititaniums, titanium sesquioxide and the titanium monoxide is at least a.Yet, the invention is not restricted to this, other titanium oxide also can.What in addition, carbonaceous reducing agent can be in graphite, carbon black and the refinery coke is at least a.Yet, the invention is not restricted to this, other also can be used as carbonaceous reducing agent such as coal dust etc.In addition, preferably, titanyl compound and carbonaceous reducing agent can have can be by the granularity of 200 mesh sieves, further preferably, titanyl compound and carbonaceous reducing agent can have can be by the granularity of 300 mesh sieves, this metallurgical power that is conducive to improve method of the present invention is learned condition, can improve the efficient of solid phase-solid state reaction.Yet, the invention is not restricted to this, that is to say, granularity also can be used as raw material of the present invention greater than titanyl compound and the carbonaceous reducing agent of above-mentioned granularity.
In another exemplary embodiment of the present invention, preferably, the number of carbon atom is than being 2:1 ~ 1:1 in Sauerstoffatom and the carbonaceous reducing agent in the titanyl compound, and it is complete that such batching scope can form titanyl compound and the carbonaceous reducing agent primitive reaction of anode.Yet, the invention is not restricted to this, that is to say, exceed above-mentioned batching scope and the anode material that forms for employing, still go for method of the present invention.
In another exemplary embodiment of the present invention, preferably, described negative electrode is carbon steel rod or molybdenum bar or titanium rod.In the method for the invention, along with the carrying out of electrolytic reaction, the titanium valve of generation can be attached to negative electrode place (for example, sometimes being equivalent to apply one deck titanium valve at cathode surface), therefore, method of the present invention can also adopt other material that is different from above-mentioned negative electrode material.
In another exemplary embodiment of the present invention, preferably, described method can also comprise anodic current density is controlled to be 0.025A/cm
2~ 0.75A/cm
2, cathode current density is controlled to be 0.1A/cm
2~ 2A/cm
2, to obtain better electrolytic efficiency.Further preferably, the control anodic current density is 0.05A/cm
2~ 0.25A/cm
2,, the control cathode current density is 0.2A/cm
2~ 1.5A/cm
2Yet, the invention is not restricted to this, those of ordinary skills can determine cathode current density and anodic current density according to concrete electrolytic reaction condition.
In another exemplary embodiment of the present invention, preferably, described TiCl
2And TiCl
3Accounting for described electrolytical massfraction can be 0.4% ~ 3%, and wherein the atom number ratio of divalence titanium and titanous can be 1:5 ~ 1:0.5, to obtain better electrolytic efficiency.Yet, the invention is not restricted to this, in the method for the invention, as long as have a small amount of Ti in the molten salt electrolyte
3+And Ti
2+, just can promote the carrying out of electrolytic reaction, and improve electrolytic efficiency, therefore, even TiCl
2And TiCl
3Content in ionogen and the atom number ratio between them be not in above-mentioned scope, and method of the present invention still can be carried out.
In addition, fused salt of the present invention can be in alkali metal chlorides such as LiCl, CaCl, KCl, NaCl or the alkaline earth metal chloride one or more.
Come brief description reaction process of the present invention below in conjunction with a preferred exemplary.
The number of at first titanyl compound and carbonaceous reducing agent being pressed Sauerstoffatom and carbon atom is pressed into the shape of suitable electrolysis than being 2:1 ~ 1:1 batching after mixing in ball mill, stand-by after dry.
Utilize titanium sponge (for example, wherein Ti 〉=99.6wt%) and smart titanium tetrachloride (TiCl
4〉=99.95wt%) in being the sodium-chlor of 1:1 and Repone K mixing salt, mol ratio prepares TiCl
2With TiCl
3, the content of titanium ion is 0.4% ~ 3% in the control fused salt, the atom number of divalence titanium and titanous is than being 1:5 ~ 1:0.5.
Upper dried material piece with after electric installation is connected, is carried out electrolysis as anode in above-mentioned ionogen, the negative electrode material adopts carbon steel, molybdenum or titanium.Following electrochemical reaction occurs at anode in this anode material:
TiO
2+C→Ti
3++Ti
2++CO+CO
2
Ti
3O
5+C→Ti
3++Ti
2++CO+CO
2
Ti
2O
3+C→Ti
3++Ti
2++CO+CO
2
TiO+C→Ti
3++Ti
2++CO+CO
2
In electrolytic process, when anodic current density is higher, separate out Ti on the anode
3+And CO
2Large percentage, when anodic current density is low, separate out Ti on the anode
2+Large percentage with CO.
Finally, form titanium valve at negative electrode.
In sum, the present invention has obtained metallic titanium powder by titanyl compound and carbonaceous reducing agent are mixed, suppress also and directly carry out fused salt electrolysis as anode after the drying, has advantages of that energy consumption is low.
Further specify the method for preparing metal titanium of the present invention below in conjunction with the example 1-6 that comprises design parameter.
Example 1
Take by weighing titanium dioxide 80g, Graphite Powder 99 24 grams mix in planetary ball mill, and with the pressure compression moulding of 500kg/cm2, as anode, carbon steel rod is negative electrode.Take the NaCl-KCl-TiCl2-TiCl3 fused salt as ionogen, electrolyzer is with argon shield, 700 ℃ of electrolysis.Anodic current density is 0.025A/cm
2, cathode current density is 0.1A/cm
2Carry out electrolysis.After electrolysis is finished, take out negative electrode with the residual ionogen of 0.5% dilute hydrochloric acid flush away, clean chlorion with deionized water again, oven dry.The product result who obtains is as follows: Ti:99.55%, C:0.05%, O:0.20%, Fe:0.04%, Si:0.02%, Mn:0.01%, Cl:0.03%; And the anode scrap material the analysis showed that still be TiO
2Mixture with C.
Example 2
Take by weighing titanium dioxide 80g, Graphite Powder 99 12 grams mix in planetary ball mill, with 500kg/cm
2Pressure compression moulding, as anode, carbon steel rod is negative electrode.With NaCl-KCl-TiCl
2-TiCl
3Fused salt is ionogen, and electrolyzer is with argon shield, 700 ℃ of electrolysis.Anodic current density is 0.25A/cm
2, cathode current density is 0.2A/cm
2Carry out electrolysis.After electrolysis is finished, take out negative electrode with the residual ionogen of 0.5% dilute hydrochloric acid flush away, clean chlorion with deionized water again, oven dry.The product result who obtains is as follows: Ti:99.24%, C:0.05%, O:0.20%, Fe:0.04%, Si:0.02%, Mn:0.01%, Cl:0.03%; And the anode scrap material the analysis showed that still be TiO
2Mixture with C.
Example 3
Take by weighing titanium dioxide 80g, Graphite Powder 99 18 grams mix in planetary ball mill, with 500kg/cm
2Pressure compression moulding, as anode, carbon steel rod is negative electrode.With NaCl-KCl-TiCl
2-TiCl
3Fused salt is ionogen, and electrolyzer is with argon shield, 700 ℃ of electrolysis.Anodic current density is 0.5A/cm
2, cathode current density is 0.5A/cm
2Carry out electrolysis.After electrolysis is finished, take out negative electrode with the residual ionogen of 0.5% dilute hydrochloric acid flush away, clean chlorion with deionized water again, oven dry.The product result who obtains is as follows: Ti:99.36%, C:0.05%, O:0.20%, Fe:0.04%, Si:0.02%, Mn:0.01%, Cl:0.03%; And the anode scrap material the analysis showed that still be TiO
2Mixture with C.
Example 4
Take by weighing five oxidation Tritanium/Trititanium 224g, Graphite Powder 99 30 grams mix in planetary ball mill, with 500kg/cm
2Pressure compression moulding, as anode, molybdenum bar is negative electrode.With NaCl-KCl-TiCl
2-TiCl
3Fused salt is ionogen, and electrolyzer is with argon shield, 800 ℃ of electrolysis.Anodic current density is 0.75A/cm
2, cathode current density is 1.0A/cm
2Carry out electrolysis.After electrolysis is finished, take out negative electrode with the residual ionogen of 0.5% dilute hydrochloric acid flush away, clean chlorion with deionized water again, oven dry, the product result who obtains is as follows: Ti:99.67%, C:0.05%, O:0.20%, Fe:0.03%, Si:0.02%, Mn:0.01%, Cl:0.03%; And the anode scrap material the analysis showed that still be Ti
3O
5Mixture with C.
Example 5
Take by weighing titanium sesquioxide 144g, Graphite Powder 99 27 grams mix in planetary ball mill, with 500kg/cm
2Pressure compression moulding, as anode, molybdenum bar is negative electrode.With NaCl-KCl-TiCl
2-TiCl
3Fused salt is ionogen, and electrolyzer is with argon shield, 750 ℃ of electrolysis.Anodic current density is 0.050A/cm
2, cathode current density is 2.0A/cm
2Carry out electrolysis.After electrolysis is finished, take out negative electrode with the residual ionogen of 0.5% dilute hydrochloric acid flush away, clean chlorion with deionized water again, oven dry, the product result who obtains is as follows: Ti:99.70%, C:0.05%, O:0.20%, Fe:0.03%, Si:0.02%, Mn:0.01%, Cl:0.03%; And the anode scrap material the analysis showed that still be Ti
2O
3Mixture with C.
Example 6
Take by weighing titanium monoxide 64g, Graphite Powder 99 12 grams mix in planetary ball mill, with 500kg/cm
2Pressure compression moulding, as anode, molybdenum bar is negative electrode.With NaCl-KCl-TiCl
2-TiCl
3Fused salt is ionogen, and electrolyzer is with argon shield, 750 ℃ of electrolysis.Anodic current density is 0.050A/cm
2, cathode current density is 2.0A/cm
2Carry out electrolysis.After electrolysis is finished, take out negative electrode with the residual ionogen of 0.5% dilute hydrochloric acid flush away, clean chlorion with deionized water again, oven dry, the product result who obtains is as follows: Ti:99.70%, C:0.05%, O:0.20%, Fe:0.03%, Si:0.02%, Mn:0.01%, Cl:0.03%; And the anode scrap material the analysis showed that still be the mixture of TiO and C.
Although the above has described the present invention in conjunction with exemplary embodiment, those of ordinary skills should be clear, in the situation of the spirit and scope that do not break away from claim, can carry out various modifications to above-described embodiment.
Claims (8)
1. a method for preparing metal titanium is characterized in that, said method comprising the steps of:
With titanyl compound and carbonaceous reducing agent mix, suppress, dry to obtain the anode material;
The anode material is connected to consist of anode with electric-conductor, with metal or alloy as negative electrode, take alkali metal chloride fused salt and/or alkaline earth metal chloride fused salt as ionogen, under inert atmosphere, carry out electrolysis, to make metallic titanium powder, wherein, described ionogen also contains TiCl
2And TiCl
3
2. the method for preparing metal titanium according to claim 1 is characterized in that, described titanyl compound is at least a in titanium dioxide, five oxidation Tritanium/Trititaniums, titanium sesquioxide and the titanium monoxide.
3. the method for preparing metal titanium according to claim 1 is characterized in that, described titanyl compound and carbonaceous reducing agent have can be by the granularity of 200 mesh sieves.
4. the method for preparing metal titanium according to claim 1 is characterized in that, described carbonaceous reducing agent is at least a in graphite, carbon black and the refinery coke.
5. the method for preparing metal titanium according to claim 1 is characterized in that, in the described titanyl compound in Sauerstoffatom and the carbonaceous reducing agent number of carbon atom than being 2:1 ~ 1:1.
6. the method for preparing metal titanium according to claim 1 is characterized in that, described negative electrode is carbon steel rod, molybdenum bar or titanium rod.
7. the method for preparing metal titanium according to claim 1 is characterized in that, described method also comprises anodic current density is controlled to be 0.025A/cm
2~ 0.75A/cm
2, cathode current density is controlled to be 0.1A/cm
2~ 2A/cm
2
8. the method for preparing metal titanium as claimed in claim 1 is characterized in that, described TiCl
2And TiCl
3Accounting for described electrolytical massfraction is 0.4% ~ 3%, and wherein the atom number of divalence titanium and titanous than being 1:5 ~ 1:0.5.
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Cited By (4)
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| CN103882477A (en) * | 2012-12-21 | 2014-06-25 | 攀钢集团攀枝花钢铁研究院有限公司 | Electrolyte and molten salt for preparing metal titanium, and metal titanium preparation method |
| CN106591888A (en) * | 2016-12-26 | 2017-04-26 | 宝纳资源控股(集团)有限公司 | Preparation method and device of low-valence titanium ion molten salt electrolyte |
| CN111364065A (en) * | 2020-03-05 | 2020-07-03 | 中国原子能科学研究院 | Method for preparing uranium by utilizing uranium oxide |
| CN113699560A (en) * | 2021-07-17 | 2021-11-26 | 广西大学 | Method for preparing metal titanium by soluble anode electrolysis of fluorine-chlorine mixed molten salt system |
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| CN103882477A (en) * | 2012-12-21 | 2014-06-25 | 攀钢集团攀枝花钢铁研究院有限公司 | Electrolyte and molten salt for preparing metal titanium, and metal titanium preparation method |
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| CN106591888A (en) * | 2016-12-26 | 2017-04-26 | 宝纳资源控股(集团)有限公司 | Preparation method and device of low-valence titanium ion molten salt electrolyte |
| CN111364065A (en) * | 2020-03-05 | 2020-07-03 | 中国原子能科学研究院 | Method for preparing uranium by utilizing uranium oxide |
| CN113699560A (en) * | 2021-07-17 | 2021-11-26 | 广西大学 | Method for preparing metal titanium by soluble anode electrolysis of fluorine-chlorine mixed molten salt system |
| CN113699560B (en) * | 2021-07-17 | 2023-12-29 | 广西大学 | Method for preparing metallic titanium by soluble anode electrolysis of fluorine-chlorine mixed molten salt system |
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Application publication date: 20130206 |