CN107760886A - A kind of equipment for preparing high purity titanium - Google Patents
A kind of equipment for preparing high purity titanium Download PDFInfo
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- CN107760886A CN107760886A CN201711071575.2A CN201711071575A CN107760886A CN 107760886 A CN107760886 A CN 107760886A CN 201711071575 A CN201711071575 A CN 201711071575A CN 107760886 A CN107760886 A CN 107760886A
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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
This application discloses a kind of equipment for preparing high purity titanium, reaction unit (1) including halogenation occurs for raw material titanium, the decomposer (2) that halide for titanium decomposes, EGR (3), vacuum generating device (4), the reaction unit (1) is connected with the decomposer (2), the decomposer (2) is provided with sensing heating part (201), and the precipitation part (202) separated out for titanium, the EGR (3) and the reaction unit (1), decomposer (2) is respectively communicated with, the EGR (3), which is used to collect the halogen decomposited in decomposer (2), to be sent into reaction unit (1), the vacuum generating device (4) connects with the decomposer (2), for providing the vacuum environment in equipment.The equipment for preparing high purity titanium that the application provides, the halogenation of accurate control titanium and the temperature of decomposition reaction.
Description
Technical field
The application is related to high purity titanium technical field, more particularly to a kind of equipment for preparing high purity titanium.
Background technology
Usually using the titanium-silicon compound (TiSi of form of film in integrated circuitx), titanium nitride (TiN), tungsten titanium (W-Ti)
Etc. being used as the materials such as coordination electrode, diffusion impervious layer, distribution.Compound film is mainly prepared by sputtering method, and high purity titanium
Available for Strapping Material made in sputtering target material, and biomaterial etc..
As sputtering target material or the high purity titanium of biomaterial, it is necessary to fully remove the radiation of the alkalinous metals, U, Th etc. such as Na, K
The property heavy metal element such as element, Fe, Cr, Ni.In addition, with the miniaturization of semiconductor, the various parts in sputtering equipment cavity
Also begin to the high purity titanium using material same with sputtering target.
The production of high purity titanium mainly has the techniques such as Kroll process, fused salt electrolysis process and titanium iodide thermal decomposition method.Kroll process
Prepare purity and can reach 4N~5N up to 3N~4N, fused salt electrolysis process preparation purity, titanium iodide thermal decomposition method can reach more than 5N.
Existing titanium iodide thermal decomposition method is to be filled in the titanium material of low-purity in closed container together with iodine iodination reaction occurs,
Synthesize titanium iodide, the titanium filament of high temperature be provided with container, titanium iodide is thermally decomposed, separate out high purity titanium, free iodine again with
Iodination reaction occurs for the titanium material of low-purity, repeats said process, and the continuous thickening of titanium filament is into high-purity stud.
Existing titanium iodide thermal decomposition method, iodination reaction occur with pyrolysis in same device, the height of thermal decomposition
Temperature has an impact to the iodination reaction of low temperature so that iodate temperature is difficult to accurately control with heat decomposition temperature, the temperature of iodination reaction
Degree exceeds suitable temperature range, influences the speed of separating out and purity of high purity titanium.
The content of the invention
In order to solve the above technical problems, the purpose of the present invention is a kind of equipment for preparing high purity titanium of offer.The present invention provides
The equipment for preparing high purity titanium, the temperature of the accurate halogenation and decomposition reaction for controlling titanium, and realize the circulation of halogen
Utilize, accelerate the precipitation of high purity titanium, while improve the purity of titanium.
Technical scheme provided by the invention is as follows：
A kind of equipment for preparing high purity titanium, including reaction unit, the halogen for titanium for raw material titanium generation halogenation
Decomposer, EGR, the vacuum generating device of compound decomposition, the reaction unit are connected with the decomposer, institute
State decomposer and be provided with sensing heating part, and the precipitation part separated out for titanium, the EGR fills with the reaction
Put, decomposer is respectively communicated with, the EGR, which is used to collect the halogen that decomposite in decomposer, is sent into reaction
In device, the vacuum generating device connects with the decomposer, for providing the vacuum environment in equipment.
Preferably, the housing of the decomposer is prepared by cermet, and the precipitation part is arranged on decomposer
In housing, the sensing heating part is arranged on outside the housing of the decomposer.
Preferably, the precipitation part that the titanium separates out is specially hollow titanium tube.
Preferably, the decomposer is additionally provided with decomposition temperature detection part, and described decomposition temperature detection part one end is set
Put inside the hollow titanium tube.
Preferably, the supplementary device for providing halogen is additionally provided with, the supplementary device connects with the reaction unit
It is logical.
Preferably, on the path that the vacuum generating device connects with the decomposer, and the EGR with
Cooling device is respectively equipped with the path of the reaction unit connection.
Preferably, the reaction unit is provided with reaction temperature detection part.
Preferably, the reaction unit is provided with material grid, and the material grid is arranged on inside the reaction unit, instead
Material is answered to be arranged between the material grid and the housing of the reaction unit.
Preferably, it is provided with heat-insulation layer outside the reaction unit.
Preferably, control device is additionally provided with, the control device obtains the reaction temperature detection part, decomposition temperature inspection
The signal of part is surveyed, for controlling reaction unit, decomposer, EGR, vacuum generating device, supplementary device, cooling dress
The operation put.
The titanium iodide thermal decomposition method that prior art uses is that the titanium material of low-purity is filled in closed appearance together with iodine
In device, 300~600 DEG C are heated to using resistance furnace, iodination reaction occurs, synthesized titanium tetra iodide, titanium is additionally provided with container
Filament, titanium filament electrified regulation are thermally decomposed to titanium tetra iodide to 1300 DEG C~1500 DEG C, separated out on the titanium filament of energization
With the titanium material of low-purity iodination reaction occurs for high purity titanium, free iodine again, repeats said process, and the continuous thickening of titanium filament is into height
Pure titanium rod.Its iodination reaction occurs with pyrolysis in same device, and the high temperature of thermal decomposition produces to the iodination reaction of low temperature
It is raw to influence so that the temperature of iodination reaction exceeds suitable temperature range, causes the impurity element in the titanium material of low-purity
React, cause the purification efficiency of titanium to decline.
In addition, titanium is separated out on the filament of electrified regulation, initial precipitation area is small, and resistance is big, increases over time, carefully
The gradual thickening of silk, separates out area increase, and resistance is gradually reduced.Whole process resistance variations have as many as tens times, are initially high electricity
Pressure, low current, low-voltage, high current are progressively converted to, power supply is difficult in adapt to whole change procedure, and temperature control is difficult, it is impossible to
Ensure the constant of heat decomposition temperature, influence the precipitation of high purity titanium.
To solve above technical problem, the present invention provides a kind of equipment for preparing high purity titanium, is provided for the generation of raw material titanium
The reaction unit of halogenation, for titanium halide decompose decomposer, make the raw material titanium of low-purity halogenation, with
And the decomposition reaction of the halide of titanium occurs in different devices, mutual reaction temperature will not interfere with each other.
With halogen (such as iodine) halogenation, the halide (such as four of the titanium of generation occur in reaction unit for raw material titanium
Titanium iodide) entered by the pipeline connected between reaction unit and decomposer in decomposer.Decomposer is provided with sensing and added
Thermal part, to separate out part carry out sensing heating, make precipitation part temperature reach titanium halide decomposition temperature, then enter
The halide of the titanium of decomposer decomposes on the precipitation part of decomposer, obtains simple substance titanium and simple substance halogen, and titanium sinks
Product is on part is separated out.Obtained simple substance halogen is decomposed, in the circulation being respectively communicated with the reaction unit, decomposer
In the presence of device, it is collected and returns in reaction unit, is reacted with the titanium material of low-purity in reaction unit, realize halogen
Recycle.Meanwhile the halogenation in reaction unit, the high-temperature decomposition reaction in decomposer can be kept independently to enter
OK so that halogenation is carried out under preference temperature respectively with decomposition reaction, will not produce interference, the raw material titanium of low-purity each other
In impurity titanium carry out halogenation when, will not react, then into decomposer be titanium halide, decompose
Obtained is high purity titanium, and dust removal rate is high.EGR, which could be arranged to circulating pump or other, can provide halogen cycle
The structure of power.And the synthesis of the halide (such as titanium tetra iodide) of titanium and decomposition reaction are reversible, in the high temperature of decomposer
Under, the halide of titanium is decomposed into simple substance halogen and simple substance titanium.Equally, the reaction temperature of halogen and titanium in reaction unit
The lower halide that will synthesize titanium, by setting path and EGR so that dissociate in decomposer caused by thermal decomposition
Halogen (such as elementary iodine vapor) pumps rapidly, into reaction unit, i.e., is produced by reducing the decomposition reaction in decomposer
Thing, promote the positive precipitation process for carrying out, accelerating titanium of the pyrolysis in decomposer.
Further, in the equipment provided by the invention for preparing high purity titanium, decomposer uses sensing heating part,
Heated to separating out part.Using the principle of sensing heating, make the electric whirlpool of precipitation part autonomous induction in electromagnetic field of high frequency
Stream heating produces high temperature, can accurately control the temperature of pyrolysis.
Brief description of the drawings
, below will be to embodiment or existing in order to illustrate more clearly of the embodiment of the present application or technical scheme of the prior art
There is the required accompanying drawing used in technology description to be briefly described, it should be apparent that, drawings in the following description are only this
Some embodiments described in application, for those of ordinary skill in the art, on the premise of not paying creative work,
Other accompanying drawings can also be obtained according to these accompanying drawings.
Fig. 1 is the structural representation for the equipment that high purity titanium is prepared in the embodiment of the present invention；
Fig. 2 is the connection diagram of control device 7 in the embodiment of the present invention；
Reference：1- reaction units；101- reaction temperature detection parts；102- material grids；2- decomposers；201-
Sensing heating part；202- separates out part；203- decomposition temperature detection parts；3- EGRs；4- vacuum generating devices；5- is mended
Fill and put；6- cooling devices；7- control devices；The titanium material of a- low-purity；B- reaction unit heater blocks.
Embodiment
In order that those skilled in the art more fully understand the technical scheme in the application, it is real below in conjunction with the application
The accompanying drawing in example is applied, the technical scheme in the embodiment of the present application is clearly and completely described, it is clear that described implementation
Example only some embodiments of the present application, rather than whole embodiments.It is common based on the embodiment in the application, this area
The every other embodiment that technical staff is obtained under the premise of creative work is not made, it should all belong to the application protection
Scope.
Please as shown in Figure 1 to Figure 2, the embodiment of the present invention provides a kind of equipment for preparing high purity titanium, including for raw material titanium
Decomposer 2, EGR 3, the vacuum generating device that the reaction unit 1 of generation halogenation, the halide for titanium decompose
4, the reaction unit 1 is connected with the decomposer 2, and the decomposer 2 is provided with sensing heating part 201, Yi Jiyong
In the precipitation part 202 that titanium separates out, the EGR 3 is respectively communicated with the reaction unit 1, decomposer 2, the circulation
Device 3, which is used to collect the halogen that decomposite in decomposer 2, to be sent into reaction unit 1, the vacuum generating device 4 with
The decomposer 2 connects, for providing the vacuum environment in equipment.
The titanium iodide thermal decomposition method that prior art uses is that the titanium material of low-purity is filled in closed appearance together with iodine
In device, 300~600 DEG C are heated to using resistance furnace, iodination reaction occurs, synthesized titanium tetra iodide, titanium is additionally provided with container
Filament, titanium filament electrified regulation are thermally decomposed to titanium tetra iodide to 1300 DEG C~1500 DEG C, separated out on the titanium filament of energization
With the titanium material of low-purity iodination reaction occurs for high purity titanium, free iodine again, repeats said process, and the continuous thickening of titanium filament is into height
Pure titanium rod.Its iodination reaction occurs with pyrolysis in same device, and the high temperature of thermal decomposition produces to the iodination reaction of low temperature
It is raw to influence so that the temperature of iodination reaction exceeds suitable temperature range, causes the impurity element in the titanium material of low-purity
React, cause the purification efficiency of titanium to decline.
In addition, titanium is separated out on the filament of electrified regulation, initial precipitation area is small, and resistance is big, increases over time, carefully
The gradual thickening of silk, separates out area increase, and resistance is gradually reduced.Whole process resistance variations have as many as tens times, are initially high electricity
Pressure, low current, low-voltage, high current are progressively converted to, power supply is difficult in adapt to whole change procedure, and temperature control is difficult, it is impossible to
Ensure the constant of heat decomposition temperature, influence the precipitation of high purity titanium.
To solve above technical problem, the present invention provides a kind of equipment for preparing high purity titanium, is provided for the generation of raw material titanium
The reaction unit 1 of halogenation, for titanium halide decompose decomposer 2, make the raw material titanium of low-purity halogenation,
And the decomposition reaction of the halide of titanium occurs in different devices, mutual reaction temperature will not interfere with each other.
With halogen (such as iodine) halogenation, the halide (such as four of the titanium of generation occur in reaction unit 1 for raw material titanium
Titanium iodide) entered by the pipeline connected between reaction unit 1 and decomposer 2 in decomposer 2.Decomposer 2 is provided with sense
Answer heater block 201, to separate out part 202 carry out sensing heating, make precipitation part 202 temperature reach titanium halide point
Solve temperature, then decomposed into the halide of the titanium of decomposer 2 on the precipitation part 202 of decomposer 2, obtain simple substance titanium with
Simple substance halogen, titanium, which is deposited on, to be separated out on part 202.Decompose obtained simple substance halogen, with the reaction unit 1,
In the presence of the EGR 3 that decomposer 2 is respectively communicated with, it is collected and returns in reaction unit 1, it is and low pure in reaction unit 1
The titanium material reaction of degree, realizes recycling for halogen.Meanwhile halogenation in reaction unit 1 can be kept, decomposed
High-temperature decomposition reaction in device 2 is independently carried out so that halogenation is carried out under preference temperature respectively with decomposition reaction, each other
Interference will not be produced, the impurity in the raw material titanium of low-purity will not react when titanium carries out halogenation, then enter and decompose
In device 2 is the halide of titanium, is high purity titanium made from decomposition, and dust removal rate is high.EGR 3 could be arranged to circulate
Pump or other the structure of halogen cycle power can be provided.And the synthesis of the halide (such as titanium tetra iodide) of titanium is anti-with decomposing
Should be reversible, at a high temperature of decomposer 2, the halide of titanium is decomposed into simple substance halogen and simple substance titanium.Equally, halogen family
Element will synthesize the halide of titanium with titanium under the reaction temperature of reaction unit 1, by setting path and EGR 3,
So that the halogen (such as elementary iodine vapor) that dissociates in decomposer 2 caused by thermal decomposition pumps rapidly, into reaction unit 1,
I.e. by reducing the cleavage reaction product in decomposer 2, promote the pyrolysis in decomposer 2 is positive to carry out, accelerate
The precipitation process of titanium.
Further, in the equipment provided by the invention for preparing high purity titanium, decomposer 2 uses sensing heating part
201, heated to separating out part 202.Using the principle of sensing heating, make precipitation part 202 in electromagnetic field of high frequency itself
The current vortex heating of sensing produces high temperature, can accurately control the temperature of pyrolysis.Specifically：
METAL HEATING PROCESS power consumption is mainly made up of two parts：P0=P1+P2。
Wherein, P0：For general power；P1：METAL HEATING PROCESS temperature rise power；P2METAL HEATING PROCESS surface emissivity power attenuation；
METAL HEATING PROCESS temperature rise power P1
Wherein, m：Metal quality (units/kg)；c：Specific heat, the specific heat of titanium is 0.125；T：Heating-up temperature；t：Heat time
(unit s)；
Example：20Kg titaniums are heated to power needed for 1400 DEG C in 1 hour
METAL HEATING PROCESS surface emissivity power attenuation P2 P2=SW=S × δ × T4(W/cm2)
Wherein, S：Metal width penetrates area；W：Radiant flux per unit area；T：Width reflective surface temperature K；δ：Boltzmann is normal
Number, δ=5.67 × 10-12(W/cm2·K4)；
Titanium is heated to 1400 DEG C, radiant flux per unit area：
W=5.67 × 10-12×(1400+273)4=44.4W/cm2
Example：Φ 80mm titanium tubes 500mm grows, and original width penetrates area S0=1256cm2, width penetrates power attenuation P20=S0W=
55.3KW。
Titanium decomposes thickening to Φ 120mm, and it is S that width, which penetrates effective area increase,1=1885cm2, area increased
Times, separate out increment 20Kg.
Width penetrates power attenuation P21=S1W=83.7KW.
The analysis more than is as can be seen that because metal material heats temperature rise power, relative to width to penetrate power smaller, in material
When amount of precipitation increment is not very big, the size for depending mainly on the size of incremental area of induction heating power, and with the electricity of material
It is little to hinder variation relation.It is 1.5 times that material, which separates out increased area, and heating general power changing value is less than 2 times, therefore, is used
Sensing heating can more be precisely controlled heat decomposition temperature by thermometric closed-loop control.
The equipment provided by the invention for preparing high purity titanium, in addition to vacuum generating device 4, vacuum generating device 4 is to whole
Equipment vacuumizes, and especially for the oxygen removed in equipment, avoids titanium and oxygen reaction and generates titanium oxide.
In the embodiment of the present invention, the housing of the decomposer 2 is prepared by cermet, and the precipitation part 202 is set
In the housing of decomposer 2, the sensing heating part 201 is arranged on outside the housing of the decomposer 2.
Preferably, the housing of decomposer 2 is prepared by cermet, and decomposer 2 is arranged on by part 202 is separated out
Housing in, sensing heating part 201 is arranged on outside the housing of the decomposer 2.Cermet is by least one metal phase
With the agglomerated material of at least one nonmetallic phase composition for being usually ceramic property, have concurrently metal and it is ceramic the advantages of, density is small,
Hardness is high, thermal conductivity is good, will not be because of quenching or shock heating and embrittlement.The housing of decomposer 2 is prepared with cermet, then is separated out
When sensing heating produces high temperature in the presence of the sensing heating part 201 of part 202, the housing of decomposer 2 will not embrittlement, keep
The long-term normal use of device.And cermet will not generate heat in induced field and produce high temperature, then the decomposition in decomposer 2 is anti-
It should concentrate on to separate out and occur at part 202, high purity titanium caused by decomposition is separated out on part 202 is separated out, and will not be separated out and decomposed
On the housing of device 2.And be arranged on sensing heating part 201 outside the housing of decomposer 2, on the one hand can be to separating out part
202 carry out sensing heating, on the other hand, sensing heating part 201 can be avoided to produce pollution to high purity titanium material, pure to obtain
Spend high titanium material.
In the embodiment of the present invention, it is specially hollow titanium tube that what the titanium separated out, which separates out part 202,.
Preferably, separating out part 202 is specifically configured to hollow titanium tube.Titanium tube possesses certain size and thickness, compared with
The titanium filament that uses of prior art, the initial area of titanium tube is big, and resistance is small compared with titanium filament, is separated out beneficial to titanium caused by decomposition,
And when high purity titanium gradually separates out, the area change of titanium tube is small compared with titanium filament, then the change of resistor current is smaller, filled beneficial to decomposing
Put the control of decomposition temperature in 2.
In the embodiment of the present invention, the decomposer 2 is additionally provided with decomposition temperature detection part 203, the decomposition temperature inspection
The one end of part 203 is surveyed to be arranged on inside the hollow titanium tube.
Preferably, be additionally provided with decomposition temperature detection part 203 in decomposer 2, and by decomposition temperature detection part 203
One end is arranged on inside the hollow titanium tube.Because the halide of titanium is decomposed in titanium tube, by decomposition temperature detection part
203 one end, which are arranged on inside the hollow titanium tube, can more accurately detect decomposition temperature, be easy to decomposition reaction process
Control.Decomposition temperature detection part 203 includes the thermometric prod of decomposer 2, is preferably also provided with infrared temperature probe simultaneously, enters
One step is accurately detected to the temperature of whole decomposer 2.
Preferably, peep hole can be set on decomposer 2, preferably by peep hole and decomposition temperature detection part
203 are equipped with.Peep hole is used to observe course of reaction in decomposer 2, and separates out the high purity titanium separated out on part 202
Situation.
In the embodiment of the present invention, be additionally provided with the supplementary device 5 for providing halogen, the supplementary device 5 with it is described
Reaction unit 1 connects.
Preferably, the equipment provided by the invention for preparing high purity titanium, is additionally provided with the supplementary device 5 of halogen, supplements
Device 5 connects with the reaction unit 1.The halogen of initial action can start to react preceding and low-purity in reaction unit 1
Titanium material adds together, can also be after the titanium material reaction unit 1 of low-purity, as needed for supplementary device 5 supplies halogenation
Halogen.
Supplementary device 5 is typically provided with the valve that control supplementary device 5 is opened and closed, and according to needed for equipment, selects Open valve, mends
Fill and put 5 and supply halogen into reaction unit 1, or close valve, supplementary device 5 stops supplying halogen into reaction unit 1
Race's element.Preferably, supplementary device 5 can be connected with the EGR 3 with the path that the reaction unit 1 connects
Logical, i.e. EGR 3 and reaction unit 1 is by pipeline communication, by supplementary device 5 and the pipeline communication.
In the embodiment of the present invention, on the path that the vacuum generating device 4 connects with the decomposer 2, and it is described
Cooling device 6 is respectively equipped with the path that EGR 3 connects with the reaction unit 1.
Preferably, cooling device 6 is set on the path that vacuum generating device 4 connects with decomposer 2.Such as by vacuum
Generating means 4 and decomposer 2 set chuck by pipeline communication on the pipeline, driving air or water etc. gas, liquid
Circulated in chuck, decline the hot-gas temperature comprising halogen in decomposer 2 out, to maintain vacuum
The normal working temperature of device 4, avoid temperature too high and harmful effect is produced to vacuum generating device 4.
Preferably, cooling device 6 is set on the path that EGR 3 connects with reaction unit 1.Such as by EGR
3 with reaction unit 1 by pipeline communication, and chuck is set on the pipeline, driving air or water etc. gas, liquid are in chuck
Circulation, decline the hot-gas temperature comprising halogen in decomposer 2 out, to maintain the normal of EGR 3
Operating temperature, avoid temperature too high and harmful effect is produced to EGR 3.The cooling device 6 that the present invention uses can also be it
He provides the structure of cooling effect.
In the embodiment of the present invention, the reaction unit 1 is provided with reaction temperature detection part 101.
Preferably, reaction temperature detection part 101 is set in reaction unit 1, for detecting titanium material and halogen family member
The temperature of element reaction, enables a device to more preferably control the course of reaction of reaction unit 1.
In the embodiment of the present invention, the reaction unit 1 is provided with material grid 102, and the material grid 102 is arranged on described
Inside reaction unit 1, reaction mass is arranged between the housing of the material grid 102 and the reaction unit 1.
The equipment provided by the invention for preparing high purity titanium, material grid 102 can be set in reaction unit 1, and will be low
The titanium material of purity is stored between the housing of material grid 102 and reaction unit 1.Accumulated compared to by the titanium material of low-purity
In the bottom of reaction unit 1, by material grid 102, inner walls of the titanium material of low-purity along reaction unit 1 are made uniformly to divide
Dissipate, increase contact area, be more beneficial for the progress of the halogenation of titanium.
In the embodiment of the present invention, the outside of reaction unit 1 is provided with heat-insulation layer.
Preferably, heat-insulation layer is set outside reaction unit 1.More preferably reaction heater block (such as heating furnace silk) is set
Put between the outer wall of reaction unit 1 and heat-insulation layer.The heat that setting heat-insulation layer can be reduced in reaction unit 1 scatters and disappears, and makes reaction
Reaction temperature in device 1 maintains titanium and the preference temperature of halogen reaction, so as to save the energy.
In the embodiment of the present invention, control device 7 is additionally provided with, the control device 7 obtains the reaction temperature detection part
101st, the signal of decomposition temperature detection part 203, for controlling reaction unit 1, decomposer 2, EGR 3, vacuum to occur
The operation of device 4, supplementary device 5, cooling device 6.
Preferably, being additionally provided with control device 7, control device 7 obtains the reaction temperature detection part 101, decomposes temperature
The signal of detection part 203 is spent, for controlling reaction unit 1, decomposer 2, EGR 3, vacuum generating device 4, supplement
The operation of device 5, cooling device 6.
The equipment provided by the invention for preparing high purity titanium, by setting control 7, high purity titanium preparation process can be monitored, and
Automatically working can be realized.The equipment provided by the invention for preparing high purity titanium, can work according to the following procedure：
1) titanium material of low-purity, and iodine are put into reaction unit 1, the control of control device 7 is opened vacuum and filled
4 are put, vacuum in whole equipment is reached 1.33*10-2Pa stops the operating of vacuum generating device 4.
2) heater block that the control of control device 7 is opened in reaction unit 1 (such as sets heating furnace in reaction unit 1
Silk), reaction unit 1 is heated, makes titanium that iodination reaction occur with iodine, generates titanium tetra iodide.Due to the fusing point of titanium tetra iodide
For 150 DEG C, boiling point is 377.2 DEG C, then it is 400 DEG C -600 DEG C, preferably 450 DEG C to control the temperature in reaction unit 1.Cross herein
Cheng Zhong, reaction temperature detection part 101 persistently detects the temperature in reaction unit 1, and sends information to control device 7, control
Device 7 processed is according to the temperature information in the reaction unit 1 received, power or opening and closing to the heater block in reaction unit 1
It is adjusted, with the temperature stabilization in maintenance reaction device 1.The titanium tetra iodide of generation enters decomposer 2 in reaction unit 1
In.
Meanwhile the sensing heating part 201 in decomposer 2 is opened in the control of control device 7, to the analysis in decomposer 2
Go out part 202 and carry out sensing heating, make to enter titanium tetra iodide in decomposer 2 and decomposed on part 202 is separated out, separated out high-purity
Calcium.Because titanium tetra iodide heat decomposition temperature is more than 1000 DEG C, then it is 1300-1500 DEG C to control and separate out temperature on part 202, preferably
For 1400 DEG C.In the process, decomposition temperature detection part 203, the temperature in decomposer 2 is persistently detected, and information is sent out
Control device 7 is delivered to, according to the temperature information in the decomposer 2 received, the sensing to decomposer 2 adds control device 7
The power of thermal part 201 or opening and closing are adjusted, to maintain the temperature stabilization in decomposer 2.
Control device 7 controls EGR 3 to operate, and the iodine that decomposition obtains in decomposer 2 is collected, and is sent into again anti-
Answer the titanium material in device 1 with low-purity to react, realize recycling for iodine.Control device 7 according to the response situation in equipment,
The vacuum being turned on and off in the adjusting device of vacuum generating device 4 can be selected, is turned on and off the control device of supplementary device 5
The content of interior iodine, cooling device 6 is turned on and off, the gas for also having iodine for entering pipeline is cooled down.
The equipment provided by the invention for preparing high purity titanium, compared with prior art, there is advantages below：
1st, the halogenation of titanium and decomposition reaction are separately carried out, and different reaction temperatures will not produce interference each other, can be with
It is precisely controlled the thermal decomposition temperature of the reaction temperature of reaction unit 1 in ± 2 DEG C of design temperature, such as 450 ± 2 DEG C, decomposer 2
Spend ± 10 DEG C in design temperature, such as 1400 ± 10 DEG C.Meanwhile by being precisely controlled the temperature of reaction unit 1, decomposer 2,
Titanium is set to be reacted with halogen, while impurity is not involved in reacting, the purity of obtained titanium is up to more than 5N.
2nd, simple substance halogen caused by being thermally decomposed in decomposer 2 is collected to be sent into reaction unit 1 and recycled, and promotees
Enter pyrolysis in decomposer 2 to carry out, and it is titanium tube to set precipitation part 202, accelerates the speed of separating out of titanium, and increase titanium
Amount of precipitation, 3, the amount of precipitation of titanium can improve more than 100 times, 50% can be reduced by separating out the time.
3rd, sensing heating part 201 is set in decomposer 2, coordinates the cermet housing of decomposer 2, utilize sensing
The principle of heating, the current vortex of the autonomous induction in electromagnetic field of high frequency of precipitation part 202 is generated heat and produce high temperature, can accurately control
The temperature of pyrolysis.
The foregoing description of the disclosed embodiments, professional and technical personnel in the field are enable to realize or using the present invention.
A variety of modifications to these embodiments will be apparent for those skilled in the art, as defined herein
General Principle can be realized in other embodiments without departing from the spirit or scope of the present invention.Therefore, it is of the invention
The embodiments shown herein is not intended to be limited to, and is to fit to and principles disclosed herein and features of novelty phase one
The most wide scope caused.
Claims (10)
- A kind of 1. equipment for preparing high purity titanium, it is characterised in that the reaction unit including halogenation occurs for raw material titanium (1), decomposer (2), EGR (3), the vacuum generating device (4) decomposed for the halide of titanium, the reaction unit (1) it is connected with the decomposer (2), the decomposer (2) is provided with sensing heating part (201), and is analysed for titanium The precipitation part (202) gone out, the EGR (3) is respectively communicated with the reaction unit (1), decomposer (2), described to follow Loop device (3), which is used to collect the halogen decomposited in decomposer (2), to be sent into reaction unit (1), the vacuum hair Generating apparatus (4) connects with the decomposer (2), for providing the vacuum environment in equipment.
- 2. equipment according to claim 1, it is characterised in that the housing of the decomposer (2) is prepared by cermet, The precipitation part (202) is arranged in the housing of decomposer (2), and the sensing heating part (201) is arranged on described point Outside the housing for solving device (2).
- 3. equipment according to claim 2, it is characterised in that the precipitation part (202) that the titanium separates out is specially hollow Titanium tube.
- 4. equipment according to claim 3, it is characterised in that the decomposer (2) is additionally provided with decomposition temperature test section Part (203), described decomposition temperature detection part (203) one end are arranged on inside the hollow titanium tube.
- 5. according to the equipment any one of claim 1-4, it is characterised in that be additionally provided with the benefit for providing halogen Fill and put (5), the supplementary device (5) connects with the reaction unit (1).
- 6. equipment according to claim 5, it is characterised in that the vacuum generating device (4) and the decomposer (2) On the path of connection, and cooling device is respectively equipped with the path that is connected with the reaction unit (1) of the EGR (3) (6)。
- 7. equipment according to claim 6, it is characterised in that the reaction unit (1) is provided with reaction temperature detection part (101)。
- 8. equipment according to claim 7, it is characterised in that the reaction unit (1) is provided with material grid (102), institute State material grid (102) and be arranged on the reaction unit (1) inside, reaction mass is arranged on the material grid (102) and institute Between the housing for stating reaction unit (1).
- 9. equipment according to claim 8, it is characterised in that be provided with heat-insulation layer outside the reaction unit (1).
- 10. equipment according to claim 9, it is characterised in that be additionally provided with control device (7), the control device (7) is obtained Take the reaction temperature detection part (101), the signal of decomposition temperature detection part (203), for control reaction unit (1), The operation of decomposer (2), EGR (3), vacuum generating device (4), supplementary device (5), cooling device (6).
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| CN201711071575.2A CN107760886A (en) | 2017-11-03 | 2017-11-03 | A kind of equipment for preparing high purity titanium |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201711071575.2A CN107760886A (en) | 2017-11-03 | 2017-11-03 | A kind of equipment for preparing high purity titanium |
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| CN107760886A true CN107760886A (en) | 2018-03-06 |
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| CN201711071575.2A Pending CN107760886A (en) | 2017-11-03 | 2017-11-03 | A kind of equipment for preparing high purity titanium |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109097602A (en) * | 2018-09-25 | 2018-12-28 | 陆世强 | A kind of method of thermal dissociation reactor and its thick beryllium powder ingot of purifying and the mode for preparing ultra-high purity metal beryllium |
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| CN109097602B (en) * | 2018-09-25 | 2021-03-26 | 陆世强 | Thermal dissociation reactor, method for purifying coarse beryllium powder into ingot and method for preparing ultra-high-purity metal beryllium |
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Application publication date: 20180306 |