CN107475539B - A kind of method that gaseous state electrochemistry prepares Titanium - Google Patents
A kind of method that gaseous state electrochemistry prepares Titanium Download PDFInfo
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- CN107475539B CN107475539B CN201710713591.0A CN201710713591A CN107475539B CN 107475539 B CN107475539 B CN 107475539B CN 201710713591 A CN201710713591 A CN 201710713591A CN 107475539 B CN107475539 B CN 107475539B
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B34/00—Obtaining refractory metals
- C22B34/10—Obtaining titanium, zirconium or hafnium
- C22B34/12—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08
- C22B34/129—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08 obtaining metallic titanium from titanium compounds by dissociation, e.g. thermic dissociation of titanium tetraiodide, or by electrolysis or with the use of an electric arc
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Abstract
The invention discloses a kind of method that gaseous state electrochemistry prepares Titanium, this method is to prepare Titanium using high frequency plasma reactor using titanium halide as raw material；The high frequency plasma reactor is vertical reactor, and main body includes cavity, and cavity is from top to bottom divided into plasma reaction section, cell reaction section and collecting chamber；Titanium halide and carrier gas are added in high-frequency induction plasma reactor, are first heated to plasma in plasma reaction section, cell reaction section electrochemical reduction is entered back into and generates Titanium, Titanium is collected in collecting chamber；This method using plasma technology and electrolysis tech combine, halogenated titanium is obtained into high pure metal titanium simple substance by simple ion and reduction, this method is simple, condition is controllable, can be reduced environmental pollution with continuous production, low in cost, is expected to realize industrialized production.
Description
Technical field
The present invention relates to a kind of method for preparing Titanium, in particular to a kind of gaseous state electrochemistry prepares the side of Titanium
Method belongs to Titanium preparation technical field.
Background technique
Titanium is a kind of argenteous transition metal, is also considered as a kind of rare metal, its main feature is that density is small, it is mechanical strong
Degree is big, is easily worked, and plasticity is strong, strong, strong, nontoxic, nonmagnetic, high temperature resistant low temperature of resistance damping properties of corrosion resistance etc..Its matter
Gently, tough, the low temperature resistant feature of high temperature resistant becomes the ideal material of aviation and aerospace industry；And since its is excellent resistance to
Corrosive nature becomes the ideal material of chemical industry and shipping industry.But the greatest drawback of titanium is that refinement is very difficult, because
Lead to it to reduce the purity of Titanium with oxygen, nitrogen, carbon and other many element compounds for titanium is very easy at high temperature
The weakening of performance.
Most early in 1791, British scientist Gregor is had found for the first time with titanium elements existing for minerals, and straight
The metal that purity is up to 99.9% was just obtained with metal sodium reduction titanium tetrachloride by Americanized scholar Hunter for the first time by 1910
Titanium.1940, after pure titanium is made using magnesium reduction in Luxembourg scientist W.J.Kroll, the refinement of Titanium just formally entered
The industrialized epoch.But there is the shortcomings such as long flow path, complex procedures for the technique, so that the production cost of titanium occupies always
It is high not under, while a large amount of pollutions generated in production process cause the industrial production of titanium to be constantly subjected to limit.Titanium production cost is inclined
Height, the in addition environmental pollution in production process, constrains the extensive use of titanium significantly.Scientist is also exploring always new refinement
The method of titanium, such as Titanium is obtained with the method Direct Electrolysis of electrochemistry, but the mechanism of this restoring method is not at present
Have and opened completely, is unable to control to obtain high-purity product.
As structural material most important in aerospace industry, the production of Titanium indicates the high point industry of a country
The level of technology.Currently, the U.S., Britain, Japan, France, Germany etc. country Titanium refinement, the exploitation of titanium alloy and add
Work, precision forging of titanium alloy etc. is in world lead level, and the Ti industry in China is started late, at present also in chasing after
The stage caught up with.And China's titanium total resources is up to first of 9.65 hundred million worlds Dun Ju, accounting for titanium gross reserves is verified in the world 38.85%, it is main
The provinces such as Sichuan, Yunnan are distributed in, especially in Panxi Diqu, titanium resource total amount is provided up to 8.7 hundred million tons to develop Ti industry
Rich material base, but the 2%~3% of the world the titanium sponge production Jin Zhan existing production capacity in China, far can not expire
The demand of the sufficient national economic development.Therefore, accelerate China's titanium industry production and have become the task of top priority.
Summary of the invention
Complex process existing for preparation method for Titanium in the prior art and it is seriously polluted the problems such as, the present invention
Purpose be to provide it is a kind of combined using plasma technique and electrolysis tech, using titanium halide as raw material, pass through letter
The method that single ionization and reduction obtain high pure metal titanium simple substance, this method is simple, condition is controllable, can be with continuous production, cost
It is cheap, it is expected to realize industrialized production.
In order to achieve the above technical purposes, the present invention provides a kind of method that gaseous state electrochemistry prepares Titanium, the party
Method prepares Titanium using titanium halide as raw material, using high frequency plasma reactor；The high frequency plasma reactor is vertical
Reactor, the high frequency plasma reactor includes cavity, and the cavity is from top to bottom divided into plasma reaction section, electrolysis
Conversion zone and collecting chamber；Titanium halide and carrier gas are added in high-frequency induction plasma reactor, first added in plasma reaction section
Heat enters back into cell reaction section electrochemical reduction and generates Titanium, Titanium is collected in collecting chamber to plasma.
Preferred scheme, the plasma reaction section top is equipped with side gas entrance, central gas entrance and feeding inlet, described etc.
Ionic reaction section containment portion is equipped with induction coil.Side gas entrance and central gas entrance are mainly passed through auxiliary gas.It is lazy for assisting gas
Property gas, generally argon gas and/or helium.Feeding inlet is connect with external charging system.
Preferred scheme, the cell reaction section cavity inner wall are equipped with one group of high temperature resistant electrode, and cavity lateral wall is equipped with electricity
Magnet assemblies.Electromagnet assembly includes two groups of electromagnet, is evenly distributed on cell reaction section cavity lateral wall.
Preferred scheme, the cell reaction section cavity top are equipped with waste gas outlet.Discharge can be recycled from waste gas outlet
Halogen gas.To realize no pollution to the environment.
High temperature resistant electrode anode of the invention is arranged at waste gas outlet.
Preferred scheme, the collecting chamber are equipped with discharge port.Titanium under the effect of gravity natural subsidence from collecting chamber,
Pass through discharge port output high frequency plasma reactor again.
More preferably scheme is passed through the high-frequency current that frequency size is 20~50MHz, cavity during the plasma
Interior temperature is 1200~2500 DEG C.The frequency of high-frequency current is preferably sized to 30~40MHz.Temperature is preferably 1600~1800
℃。
More preferably scheme, the voltage of the high temperature resistant electrode are 1.0~4.0V.The voltage of the high temperature resistant electrode is preferred
For 2~2.5V.
More preferably scheme, the magnetic field that the electromagnet assembly generates: main field strength is 100~300A/cm, axial magnetic
Field variable gradient is 0.8~1.2A/cm2.Main field strength is preferably 180~220A/cm.Axial magnetic field variable gradient is 0.9
~1A/cm2。
More preferably scheme, the carrier gas are argon gas and/or helium.
More preferably scheme, the titanium halide are titanium tetrachloride and/or titanium tetrabromide.Titanium halide is not limited to tetrachloro
Change titanium and titanium tetrabromide, titanium tetra iodide and titanium tetrafluoride are also adapted to prepare metal titanium material as gaseous state electrochemistry.
The method that gaseous state electrochemistry of the invention prepares Titanium is first led to together with carrier gas using titanium halide as raw material
Enter in high-frequency induction plasma reactor, is first heated at high temperature to plasma in plasma reaction section, enters back into cell reaction
Section, under effect of contraction under high-intensity magnetic field, makes plasma form stable shape, has good electrical conductive properties using plasma
The characteristics of, directly restore gaseous titanium ion mixture on cathode plate by a pair of of high temperature resistant electrode to get high-purity titanium is arrived
Simple substance, purity can reach 99% or more.
Compared with the prior art, technical solution of the present invention bring advantageous effects:
1, technical solution of the present invention uses high frequency plasma reactor for the first time to prepare Titanium, high frequency of use etc. from
Sub- reactor has merged plasma technique and electrochemical techniques, can rapidly, continuously change the Titanium of preparation high-purity, solves existing
Have in technology chemical reduction method prepare Titanium long flow path, complex process, environmental pollution, can not continuous production the defects of,
Solve with electrochemistry can not Direct Electrolysis prepare the technological deficiency of high pure metal titanium, breach the limitation of traditional technology；
2, high frequency plasma reactor design principle of the invention is simple, is easy in existing plasma reactor, high temperature
It improves to obtain on the basis of electrolysis reactor etc..
3, technical solution of the present invention is using titanium chloride as raw material, inexpensive, and reacts by using high frequency plasma
One step of device realizes reduction, has the characteristics that step is simple, efficient high yield, Titanium purity obtained is up to 99%, using high frequency
Plasma reactor operating condition is controllable, can be continuously produced, and meets industrialized production.
Detailed description of the invention
[Fig. 1] is high frequency plasma structure of reactor schematic diagram；
[Fig. 2] is cell reaction section cavity cross-section figure；
1 is plasma reaction section, and 2 be cell reaction section, and 3 be collecting chamber, gas entrance centered on 4, and 5 be side gas entrance, and 6 are
Feeding inlet, 7 be induction coil, and 8 be high temperature resistant electrode, and 9 be electromagnet assembly, and 10 be waste gas outlet, and 11 be discharge port.
Specific embodiment
Following embodiment is in order to which the present invention is explained in greater detail, these embodiments do not form any restrictions to the present invention,
The present invention can be implemented by formula either described in summary of the invention.
High frequency plasma structure of reactor schematic diagram of the invention is as shown in Figure 1.High frequency plasma reactor is vertical anti-
Device is answered, high frequency plasma reactor includes cavity, and the cavity is from top to bottom divided into plasma reaction section, cell reaction section
And collecting chamber.Side gas entrance, central gas entrance and feeding inlet, feeding inlet and external charging system are equipped at the top of plasma reaction section
System connection, main offer reaction raw materials and carrier gas, side gas entrance and central gas entrance are mainly passed through auxiliary gas.Plasma reaction
Section containment portion is equipped with induction coil, is mainly used for being passed through high-frequency current heating.The cell reaction section cavity inner wall is equipped with one
Group high temperature resistant electrode, cavity lateral wall are equipped with electromagnet assembly, and electromagnet assembly includes two groups of electromagnet, are evenly distributed on electrolysis
Conversion zone cavity lateral wall stabilizes the titanium ion of plasma for providing magnetic field, and high temperature electrode is for plasma
The reduction of gaseous titanium ion mixture.The cell reaction section cavity top is equipped with waste gas outlet, is mainly used for the gas generated row
It puts.The collecting chamber is equipped with discharge port, and the Titanium collected in collecting chamber can be in time from discharge port output.
Embodiment 1
Titanium tetrachloride is added continuously in high frequency plasma reactor, the high-frequency current of 40MHz, temperature in reactor are passed through
Degree rises to 1800 DEG C, and setting main field strength is 200A/cm, axial magnetic field gradient 1A/cm2, titanium tetrachloride formation plasma
After state, stable plasma form is kept under the influence of a magnetic field, adds the decomposition voltage of 2.5V, chloride ion at electrode both ends
Chlorine is generated in anodic oxidation, is collected and is recycled by gas concentration unit, Titanium generates molten gold in cathodic reduction
Belong to simple substance, be collected under the effect of gravity into collecting chamber, realizes continuous Titanium production, member is surveyed by ICP-AES method
Cellulose content, the purity of gained Titanium are 99%.
Embodiment 2
Titanium tetrachloride is added continuously in high frequency plasma reactor, the high-frequency current of 50MHz, temperature in reactor are passed through
Degree rises to 2200 DEG C, and setting main field strength is 300A/cm, and axial magnetic field gradient is 1.2A/cm2, titanium tetrachloride formed
After ionic state, keep stable plasma form under the influence of a magnetic field, electrode both ends add 4V decomposition voltage, chlorine from
Son generates chlorine in anodic oxidation, is collected and is recycled by gas concentration unit, and Titanium generates molten in cathodic reduction
Metal simple-substance is collected into collecting chamber under the effect of gravity, is realized continuous Titanium production, is surveyed by ICP-AES method
Constituent content, the purity of gained Titanium are 90%.
Embodiment 3
Titanium tetrabromide is added continuously in high frequency plasma reactor, the high-frequency current of 40MHz, temperature in reactor are passed through
Degree rises to 1800 DEG C, and setting main field strength is 200A/cm, and axial magnetic field gradient is 1A/cm2, titanium tetrachloride formed etc. from
After sub- state, keep stable plasma form under the influence of a magnetic field, electrode both ends add 3.0V decomposition voltage, bromine from
Son generates gaseous state bromine simple substance in anodic oxidation, is collected and is recycled by gas concentration unit, and Titanium is in cathodic reduction, life
It at molten metal simple-substance, is collected under the effect of gravity into collecting chamber, continuous Titanium production is realized, by ICP-
AES method surveys constituent content, and the purity of gained Titanium is 95%.
Embodiment 4
Titanium tetrachloride is added continuously in high frequency plasma reactor, the high-frequency current of 20MHz, temperature in reactor are passed through
Degree rises to 1400 DEG C, and setting main field strength is 100A/cm, and axial magnetic field gradient is 1A/cm2, titanium tetrachloride formed etc. from
After sub- state, keep stable plasma form under the influence of a magnetic field, electrode both ends add 2.0V decomposition voltage, chlorine from
Son generates chlorine in anodic oxidation, is collected and is recycled by gas concentration unit, and Titanium generates molten in cathodic reduction
Metal simple-substance is collected into collecting chamber under the effect of gravity, is realized continuous Titanium production, is surveyed by ICP-AES method
Constituent content, the purity of gained Titanium are 80%.
Comparative example 1
Titanium tetrachloride is added continuously in high frequency plasma reactor, the high-frequency current of 15MHz, temperature in reactor are passed through
Degree rises to 900 DEG C, and setting main field strength is 200A/cm, axial magnetic field gradient 1A/cm2, titanium tetrachloride formation plasma state
Afterwards, stable plasma form is kept under the influence of a magnetic field, the decomposition voltage of 2.5V is added at electrode both ends, without metal
Titanium generates, the reason is that temperature is too low, can not form good plasma.
Comparative example 2
Titanium tetrachloride is added continuously in high frequency plasma reactor, the high-frequency current of 40MHz, temperature in reactor are passed through
Degree rises to 1800 DEG C, and setting main field strength is 50A/cm, axial magnetic field gradient 0.5A/cm2, titanium tetrachloride formation plasma
After state, stable plasma form is kept under the influence of a magnetic field, adds the decomposition voltage of 2.5V, chloride ion at electrode both ends
Chlorine is generated in anodic oxidation, is collected and is recycled by gas concentration unit, Titanium generates molten gold in cathodic reduction
Belong to simple substance, be collected under the effect of gravity into collecting chamber, realizes continuous Titanium production, member is surveyed by ICP-AES method
Cellulose content, the purity of gained Titanium are 20%.
Claims (9)
1. a kind of method that gaseous state electrochemistry prepares Titanium, it is characterised in that: using titanium halide as raw material, using high frequency etc. from
Sub- reactor prepares Titanium；
The high frequency plasma reactor be vertical reactor, the high frequency plasma reactor includes cavity, the cavity by
Plasma reaction section, cell reaction section and collecting chamber are divided under；The cell reaction section cavity inner wall is equipped with one group
High temperature resistant electrode, cavity lateral wall are equipped with electromagnet assembly；
Titanium halide and carrier gas are added in high-frequency induction plasma reactor, are first heated to plasma in plasma reaction section
Change, enters back into cell reaction section electrochemical reduction and generate Titanium, Titanium is collected in collecting chamber.
2. the method that a kind of gaseous state electrochemistry according to claim 1 prepares Titanium, it is characterised in that:
Side gas entrance, central gas entrance and feeding inlet, the plasma reaction section cavity are equipped at the top of the plasma reaction section
Outside is equipped with induction coil.
3. the method that a kind of gaseous state electrochemistry according to claim 1 prepares Titanium, it is characterised in that: the electrolysis is anti-
Section cavity top is answered to be equipped with waste gas outlet.
4. the method that a kind of gaseous state electrochemistry according to claim 1 prepares Titanium, it is characterised in that: the collecting chamber
Equipped with discharge port.
5. the method that a kind of gaseous state electrochemistry according to any one of claims 1 to 4 prepares Titanium, it is characterised in that:
The high-frequency current that frequency size is 20~50MHz is passed through during the plasma, cavity inner temperature is 1200~2500 DEG C.
6. the method that a kind of gaseous state electrochemistry according to any one of claims 1 to 4 prepares Titanium, it is characterised in that:
The voltage of the high temperature resistant electrode is 1.0~4.0V.
7. the method that a kind of gaseous state electrochemistry according to any one of claims 1 to 4 prepares Titanium, it is characterised in that:
The magnetic field that the electromagnet assembly generates: main field strength is 100~300A/cm, axial magnetic field variable gradient is 0.8~
1.2A/cm2。
8. the method that a kind of gaseous state electrochemistry according to any one of claims 1 to 4 prepares Titanium, it is characterised in that:
The carrier gas is argon gas and/or helium.
9. the method that a kind of gaseous state electrochemistry according to any one of claims 1 to 4 prepares Titanium, it is characterised in that:
The titanium halide is titanium tetrachloride and/or titanium tetrabromide.
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| US7381366B2 (en) * | 2003-12-31 | 2008-06-03 | General Electric Company | Apparatus for the production or refining of metals, and related processes |
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| CN101040064A (en) * | 2004-10-12 | 2007-09-19 | 东邦钛株式会社 | Method for producing metal by molten salt electrolysis and method for producing metal titanium |
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