CN105838907B - Titanium purifying plant and application method - Google Patents
Titanium purifying plant and application method Download PDFInfo
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- CN105838907B CN105838907B CN201610342840.5A CN201610342840A CN105838907B CN 105838907 B CN105838907 B CN 105838907B CN 201610342840 A CN201610342840 A CN 201610342840A CN 105838907 B CN105838907 B CN 105838907B
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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
- C22B34/1295—Refining, melting, remelting, working up of titanium
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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
- C22B9/00—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
- C22B9/04—Refining by applying a vacuum
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Abstract
The invention discloses a kind of titanium purifying plant, including purification bag, high pressure-temperature inert gas installation, heater and discharge duct, it is closed tank structure that purification, which is wrapped, is provided with crucible in it, insulation material is filled between crucible and purification bag, cooling device is embedded with the insulation material；The outlet of high pressure-temperature inert gas installation wears purification bag bottom, insulation material connects with crucible bottom, and crucible bottom is provided with the drain pipe for stretching out purification bag；Heater includes middle part heater, and middle part heater upper end is fixed on purification bag top, and lower end is located in the cavity of crucible；Discharge duct is located on purification bag top.The inert gas that the present invention blows preheating by bottom has stirring action to titanium liquid, constantly allows surface titanium liquid and internal titanium liquid that mass exchange occurs, the impurity in liquid titanium is risen on liquid level, remove volatile impurity.
Description
Technical field
The present invention relates to metal to propose equipment technical field, especially a kind of titanium purifying plant, and its application method.
Background technology
Titanium refines due to being difficult to, and preparation process is extremely difficult, the general high temperature all more than 800 DEG C of its smelting process
Lower progress, and chemical combination is very competent at high temperature for titanium, can be with oxygen, carbon, nitrogen and other many element compounds, it is therefore necessary to
Operated in vacuum or under inert atmosphere protection.Ilmenite is become titanium tetrachloride in laboratory, then is put into the stainless steel of sealing
In tank, argon gas is filled with, makes they and metal reactive magnesium, is just obtained " titanium sponge ".This porous " titanium sponge " is can not be direct
Use, it is necessary to they are fused into liquid in electric furnace, casts titanium ingot.But this electric furnace of manufacture is again easier said than done！Except electricity
The air of stove must be drained outside net, more nerve-racking to be, the crucible for containing liquid titanium is can not find simply, because general refractory material
Containing oxide, and oxygen therein will be seized by liquid titanium.
The method of industrial conventional sulfuric acid decomposition ilmenite produces titanium dioxide, then produces Titanium by titanium dioxide.Sea
Continuous titanium is eventually fabricated various titaniums by crushing, being put into melting in vacuum arc furnace ignition.Metallothermic processes is produced spongy
Titanium, purity % (quality) are generally 99.1~99.7.Impurity element % (quality) total amount is 0.3~0.9, impurity element oxygen %
(quality) is 0.06~0.20, and hardness (HB) is 100~157, is divided into WHTi according to the difference of purity0To MHTi4Five grades,
To produce the primary raw material of industrial titanium alloy.
Also reaction can be passed through：Ti+2I2=TiI4
Obtain TiI4By high temperature（1250 DEG C or so）In the case of decompose：
TiI4=Ti+2I2
Thus pure titanium rod is obtained.
Presently mainly using the electric furnace of a kind of " water jacketed copper crucible ".Industrially use titanium casting melting casting equipment at present
There are three kinds：Vacuum consumable electric arc skull crucible, vacuum non-consumable skull crucible and electron beam skull stove, its common feature are all to use
" scull crucible ", i.e., using the copper crucible or graphite crucible of Forced water cooling.During melting titanium formed on sidewall of crucible one it is very thin
Solidifying shell, protect titanium not contaminated in the molten state, so as to obtain " pure " liquid titanium of enough cast.It is this
The electric furnace only a part of region in center is awfully hot, and remainder is all cold, after titanium melts in electric furnace, flows to the copper being water-cooled
On sidewall of crucible, titanium ingot is congealed at once.Have been able to produce several tons heavy of titanium block in this way, but its cost is too high, the cycle
It is long, low production efficiency, high energy consumption.
The content of the invention
The present invention in view of the shortcomings of the prior art, proposes a kind of titanium purifying plant, and clever structure is easy to use.
In order to realize foregoing invention purpose, the present invention provides following technical scheme：A kind of titanium purifying plant, including purification
Bag, high pressure-temperature inert gas installation, heater and discharge duct, purification bag is closed tank structure, is provided with crucible in it,
Insulation material is filled between crucible and purification bag, cooling device is embedded with the insulation material；High pressure-temperature inert gas fills
Put outlet and wear purification bag bottom, insulation material and connect with crucible bottom, crucible bottom, which is provided with, stretches out the drain pipe that purification is wrapped；Add
Thermal includes middle part heater, and middle part heater upper end is fixed on purification bag top, and lower end is located in the cavity of crucible；Row
Feed channel is located on purification bag top.
Further, middle part heater is made up of heater and protective cover, and heater is located in protective cover, protective cover upper end
Purification bag top is fixed on, lower end is located in the cavity of crucible.
Further, heater also includes top heater, and the top heater is fixed on the middle and upper part of protective cover.
Further, high pressure-temperature inert gas installation is made up of high-pressure inert gas tank, pipeline heater and heat-insulation layer,
High-pressure inert gas tank is connected through pipeline with crucible, and pipeline heater is located at pipeline periphery, and heat-insulation layer is coated on pipeline.
Further, crucible is tungsten crucible, molybdenum crucible or graphite crucible.
Further, protective cover is graphite material, and outer surface is titanium carbide layer.
Further, heater is Si-Mo rod heater or graphite heater.
Further, pipeline heater is silicon molybdenum heater, iron wire heater or graphite heater.
Further, crucible is graphite crucible, and its interior surface layers is titanium carbide layer or titanium carbonitride layer.
A kind of application method of titanium purifying plant as described above, comprises the following steps：
(1), application of vacuum purification bag：Purification bag is carried out vacuumizing a below 10Pa, while is passed through inert gas so that
It is in purification bag in inert gas atmosphere；
(2), the liquid titanium of melting is imported in the case where completely cutting off air in the crucible of purification bag；
(3), 1000 DEG C ~ 1600 DEG C of inert gas is continually fed into purification bag bottom, flow is 0.5 ~ 5 l/min, gas
Pressure is 0.5 ~ 1MPa, while starts top heater and middle part heater, controls the upper epidermis liquid titanium temperature in crucible to be
1750 ~ 1900 DEG C, internal layer liquid titanium temperature is 1700 ~ 1900 DEG C；Continue 1 ~ 8h；
(4), control middle part heater, slow cooling liquid titanium start cooling device to 1700 DEG C so that liquid titanium
Solidified by four circumferential center oriented of crucible；The high liquid titanium that do not solidify of partial impurities content is discharged through drain pipe.
Compared with prior art, the present invention has advantages below：
1) inert gas that preheating is blown by bottom has stirring action to titanium liquid, constantly allows surface titanium liquid and internal titanium liquid
Generation mass exchange, the impurity in liquid titanium is risen on liquid level, remove volatile impurity.
2) present invention purification titanium technique is simple, and cost is low；Whole purification process excludes without acid-base reaction, no waste gas, ring
Protect.
3）Overcome and low pure and mild high-purity difficult separate condition is realized in industrial production, low-purity titanium of the present invention is real in liquid
Now separated with high-purity solid-state titanium, solve high low-purity and be not easy problem of separation.
4）In purification process, impurity content highest on solid-liquid face, bottom blown inert gas, make impurity on solid-liquid face quick
It is diffused into liquid, reduces diffusion of the impurity to high-purity solid-state titanium.
5）To 99% titanium refining effect, purified rear purity can reach 99.9~99.997%.
6）Graphite and titanium contact place have carried out titanium carbide processing, solve the problems, such as to select crucible difficulty.
7）Realize and the inert gas for being blown into purification bag bottom is preheated, avoid because gas reduces the temperature of liquid titanium.
8）Realize in whole purification schemes and carried out under vacuum or inert gas atmosphere, prevent from aoxidizing with air contact
And nitridation, it is that reduction oxygen and nitrogen lay the first stone in purification process.
9）Realize liquid titanium and carry out directional solidification in the dynamic case.
10）Traditional handicraft simply heats on liquid titanium surface, and the present invention realizes carries out heating inside liquid titanium.
Brief description of the drawings
Fig. 1 is the structural representation of titanium purifying plant of the present invention；
Fig. 2 is the use state figure of titanium purifying plant of the present invention.
Embodiment
The present invention will be described in detail below in conjunction with the accompanying drawings, and the description of this part is only exemplary and explanatory, should not
There is any restriction effect to protection scope of the present invention.
As illustrated in fig. 1 and 2, a kind of titanium purifying plant, including purification bag 6, high pressure-temperature inert gas installation, heater
With discharge duct 1, purification bag 6 be closed tank structure, is provided with crucible 4 in it, crucible 4 and purification are filled between wrapping 6 and be incubated
Material 3, cooling device 2 is embedded with the insulation material 3；The outlet of high pressure-temperature inert gas installation wears 6 bottoms of purification bag, protected
Adiabator 3 connects with the bottom of crucible 4, and the bottom of crucible 4 is provided with the drain pipe 7 for stretching out purification bag；Heater heats including middle part
Device, middle part heater upper end are fixed on the top of purification bag 6, and lower end is located in the cavity of crucible 4；Discharge duct 1 is located at purification
On the top of bag 6.
Discharge duct 1 leads to outside through top high temperature resistant top cover, and being filled with pipeline 10 by argon gas is blown into argon gas, and argon gas carries
Volatile impurity and gas are discharged to purification bag outside, play purification effect.
The position of cooling device 2 is among insulation material 3, by water cooling, the heat taken away according to water-carrying capacity size, to control
Liquid titanium setting rate processed, from four circumferential center oriented solidifications.
Insulation material 3 is close to the outer surface of crucible 4, is combined by alundum (Al2O3) insulation material, graphite felt and high temperature cotton etc.
Into preventing that the heat losses of top heater and middle part heater are too fast, control the temperature of liquid titanium.
Crucible 4 is dystectic tungsten crucible, molybdenum crucible or graphite crucible, and for holding liquid titanium 5, this crucible is circle
Or square, this patent is by taking circle as an example, it is illustrated that with circle.
Molten titanium or liquid titanium 5, are placed in crucible 4, through vacuum intermediate-frequency stove, vacuum electrophoresis stove or other vacuum stove heats
The liquid titanium 5 being fused into.
Purification bag 6 is circular or square, and this patent is by taking circle as an example, it is illustrated that with circle.
The high liquid titanium of remaining impure amount after surrounding and bottom directional solidification reach purification effect of drain pipe 7 is managed through this
Pour out.
Exotic material 8 is made up of the material such as alundum (Al2O3) and soft carbon felt, prevents high temperature argon thermal loss.
Pipeline heater 9 heats argon gas pipeline, and heat up argon gas indirectly, and its temperature control is at 1000 DEG C~1600 DEG C.
Argon gas is blown into pipeline 10, and this pipe wraps bottom by purifying, and by purifying bag inside thermal conservation material 3, reaches crucible bottom,
Crucible bottom is blown into liquid titanium 5 through spongy exotic material.Argon gas is blown into through this pipeline, stirring is played to liquid titanium 5
Effect, while carry volatile impurity and gas and be discharged to purification bag outside, purification effect is played, equipment for purifying is completely lazy in addition
Property gas shield under, prevent and air contact, insulation material and titanium is oxidized and nitridation.
High pressure argon gas tank 11 controls the flow and pressure of argon gas.
Top heater 12 is fixed on the high temperature resistant top cover of top, is remained that top is in high-temperature liquid state titanium, is ensured argon
Gas can be discharged from bottom by liquid titanium from top.
It is fixed on the high temperature resistant top cover of top, the heating of middle part heater, ensures that middle part is in liquid condition all the time, argon gas leads to
Road is completely smooth, while controls liquid titanium temperature, and cooling system coordinates, and controls its four circumferential center oriented setting rate,
Reach refining effect.
Protective cover 14, because middle part heater 13 can not directly contact with liquid titanium, to its protective effect of heater.
High-purity solidification solid-state titanium 15, it is circumferential four according to segregation coefficient of the different impurities in liquid titanium and fractional condensation principle
In center oriented process of setting, partial impurities are rejected in the liquid titanium at center, and obtained solid-state titanium purity is of a relatively high.
Low pure liquid titanium 16, after directional solidification, the higher molten titanium of residual impurity content.
The raw material of titanium purifying plant of the present invention, melted through vacuum intermediate-frequency stove, vacuum electrophoresis stove or other vacuum stove heats
Change Powdered Titanium, titanium sponge or the other forms solid titanium that purity is 99%；In fusion process is heated can in vacuum state or
Carried out under inert gas shielding, fusion temperature is controlled at 1700~1900 DEG C.
Crucible 4 is using dystectic tungsten crucible, molybdenum crucible or graphite crucible etc. in stove.Carried out first using graphite crucible
Titanium directly melts in graphite crucible, and sidewall of crucible pours out liquid after forming titanium carbide protective layer, it is necessary to be kept for 1~4 hour after melting
State titanium.In the titanium carbide that sidewall of crucible is formed, fusing point is 3150 DEG C, the g/cm of density 4.913.TiC have good heat transfer property and
Electric conductivity, as temperature raises the reduction of its electric conductivity, this explanation TiC has metalline.Although having carbon and titanium solid solution phenomenon,
It is only possible to that crucible surrounding and crucible bottom thickness can be increased.Graphite guide heating rate is high, and the surface that titanium liquid surface flows through can quickly form
The titanium shell of one solidification, prevents the phenomenon of dissolving each other between graphite and titanium.
Or titanium valve is sprayed in graphite crucible inwall, 1~4 hour in a nitrogen environment, form titanium nitride.Density is at 25 DEG C
5.21 g/cm3.Its hardness is very high, Mohs' hardness 9, and microhardness is 2.12 GPa, and fusing point is 2930 DEG C.TiN has very
Good electric conductivity, electrical conductivity is 8.7 μ s/m at 20 DEG C.With the rise of temperature, its electric conductivity reduces, and shows as metal
Property.The nitride of titanium is a lot, such as TiN, TiN2、Ti2N、Ti3N、Ti4N、Ti3N4、Ti3N5、Ti5N6Deng, but it is wherein important
For TiN.TiN forms solid solution in Ti-N systems, and it is in TiN0.37~TiN1.2It is stable in compositing range.Their phase mutual energy
Form a series of continuous solid solutions.Reacted with C, the stable Ti of easy forming properties（C,N）Compound, layer protecting film is formed, is subtracted
C content in few titanium.
Molten condition titanium must reach 10 below Pa before being transferred to purification bag 6 to purifying bag 6 and vacuumize in intermediate frequency furnace
When, then pass to argon gas and vacuumize again, so clean repeatedly, make entirely to purify packet system and be in clean state, reduce to liquid
The pollution of titanium.Before liquid titanium is transferred to purification bag 6, purification 6 systems of bag are in inert gas positive atmosphere.
Inert gas can be argon gas, helium and neon etc.；Middle part heater 13 can be Si-Mo rod heater and graphite heating
Device；Argon gas pipeline heater 9 can use silicon molybdenum heater, iron wire heater and graphite heater.
Exemplified by inert gas of the present invention uses argon gas, middle part heater 13 uses Si-Mo rod heater, argon gas pipeline heating
Device 9 is using progress purifying technique explanation exemplified by graphite heater.Top heater 12 uses graphite heater, control 1750~
In the range of 1900 DEG C, ensure that the surface of liquid titanium 5 is liquid situation, the inert gas being blown into from bottom can be in liquid titanium upper surface
Overflow, smoothly discharged through argon gas escape pipe 1.Middle part Si-Mo rod heater 13 prevents from touching liquid titanium, needs graphite protective cover 14
Protected.The surface of graphite protective cover 14 needs also exist for carrying out titanium carbide processing.Middle part Si-Mo rod heater 13 is controlled 1700
In the range of~1900 DEG C, ensure to be in the state of liquid titanium 5, argon gas 5 upper surface passage from bottom to liquid titanium all the time in the middle part of crucible
Smoothly.
To ensure high-temperature solid titanium, liquid titanium and air insulated, argon gas atmosphere is needed to protect in whole titanium purification process.It is whole
Individual process mainly includes：Liquid titanium, intermediate frequency furnace are transferred to purification bag, purifying technique and finally remained in the fusing of intermediate frequency furnace titanium, crucible
Remaining liquid titanium is poured out, and is all completed in argon gas atmosphere.Purity of argon is>99.99 (4N), are fused into argon in liquid titanium in stove
The l/min of throughput 5~30, pressure are 0.3~0.5 MPa.Purification bag is transferred in intermediate frequency furnace and last remaining liquid titanium is poured out
During argon flow amount be 30~100 l/min, pressure is 0.3~0.5 MPa.Crucible bottom is blown into purification bag purification process
Portion, argon gas pipeline heater 9 heat temperature of argon gas scope：1000 DEG C~1600 DEG C, the l/min of argon flow amount 0.5~5, gas pressure
Power is 0.5~1 MPa.
In purification process, the temperature of control middle part heater 13, progressively cool from 1900 DEG C, final temperature drops to 1700
℃.It is stepped up purifying the water pressure of bag cooling device 2 and flow, range hydraulic pressure is 0.2~0.6 MPa, water-carrying capacity scope 30~
75 m3/h.It is final liquid titanium is solidified from surrounding toward center oriented, as shown in Figure 2.Due to directional solidification reason, impurity element
It is rejected in liquid titanium 16, high-purity solidification solid-state titanium purity is significantly larger than liquid titanium 16.Because of remainder after the completion of purifying technique
Divide liquid titanium 16, its impurity content is high, to prevent it is frozen into solid-state from having influence on the high-purity solid-state 15 solidified, makes high purity titanium
15 and the high low pure titanium 16 of impure amount easily separate, it is necessary to which the high low pure liquid titanium 16 of impure amount is fallen before curing
Go out purification bag.To prevent it from combustion phenomena occurring during pouring out, low pure liquid titanium 16 is transferred to argon gas through effuser 17 and protected
In atmosphere chamber, the separation of high purity titanium and low pure titanium is realized.
Because the outer surface of solid high purity titanium 15 has the materials such as titanium carbide, inner surface impurity content is of a relatively high, needs simultaneously
Remove end to end.Because solid-state titanium plasticity is good and low intensity, purification bag is that also have symmetry with symmetry, output solid-state titanium 15,
Outer surface and inner surface are directly cut on lathe, the solid-state titanium reserved.Or along vertical centerline by whole solid-state titanium
15 are sawn into two parts, and two symmetry solid-state titaniums are squeezed into square, cutting removal is carried out to surface.
Described above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, under the premise without departing from the principles of the invention, some improvements and modifications can also be made, these improvements and modifications also should
It is considered as protection scope of the present invention.
Claims (10)
- A kind of 1. titanium purifying plant, it is characterised in that：Including purification bag, high pressure-temperature inert gas installation, heater and row Feed channel, purification bag be closed tank structure, is provided with crucible in it, and crucible and purifying is filled with insulation material, the guarantor between wrapping Cooling device is embedded with adiabator；The outlet of high pressure-temperature inert gas installation wears purification bag bottom, insulation material and crucible Bottom connects, and crucible bottom is provided with the drain pipe for stretching out purification bag；Heater includes middle part heater, middle part heater upper end It is fixed on purification bag top, lower end is located in the cavity of crucible；Discharge duct is located on purification bag top.
- 2. titanium purifying plant as claimed in claim 1, it is characterised in that：Middle part heater is made up of heater and protective cover, is added Hot device is located in protective cover, and protective cover upper end is fixed on purification bag top, and lower end is located in the cavity of crucible.
- 3. titanium purifying plant as claimed in claim 2, it is characterised in that：Heater also includes top heater, and the top adds Hot device is fixed on the middle and upper part of protective cover.
- 4. titanium purifying plant as claimed in claim 1, it is characterised in that：High pressure-temperature inert gas installation is by high-pressure inert gas Tank, pipeline heater and heat-insulation layer are formed, and high-pressure inert gas tank is connected through pipeline with crucible, and pipeline heater is located at outside pipeline Week, heat-insulation layer are coated on pipeline.
- 5. titanium purifying plant as claimed in claim 1, it is characterised in that：Crucible is tungsten crucible, molybdenum crucible or graphite crucible.
- 6. titanium purifying plant as claimed in claim 2, it is characterised in that：Protective cover is graphite material, and outer surface is titanium carbide layer.
- 7. titanium purifying plant as claimed in claim 2, it is characterised in that：Heater is Si-Mo rod heater or graphite heater.
- 8. titanium purifying plant as claimed in claim 4, it is characterised in that：Pipeline heater is silicon molybdenum heater, iron wire heater Or graphite heater.
- 9. titanium purifying plant as claimed in claim 5, it is characterised in that：Crucible is graphite crucible, and its interior surface layers is titanium carbide Layer or titanium carbonitride layer.
- 10. a kind of application method of titanium purifying plant as claimed in claim 1, comprises the following steps：(1), application of vacuum purification bag：Purification bag is carried out vacuumizing a below 10Pa, while is passed through inert gas so that purification It is in bag in inert gas atmosphere；(2), the liquid titanium of melting is imported in the case where completely cutting off air in the crucible of purification bag；(3), 1000 DEG C ~ 1600 DEG C of inert gas is continually fed into purification bag bottom, flow is 0.5 ~ 5 l/min, gas pressure For 0.5 ~ 1MPa, while start top heater and middle part heater, control in crucible upper epidermis liquid titanium temperature be 1750 ~ 1900 DEG C, internal layer liquid titanium temperature is 1700 ~ 1900 DEG C；Continue 1 ~ 8h；(4), control middle part heater, slow cooling liquid titanium start cooling device to 1700 DEG C so that liquid titanium is by earthenware Four circumferential center oriented of crucible solidifies；The high liquid titanium that do not solidify of partial impurities content is discharged through drain pipe.
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| CN116443867A (en) * | 2023-04-21 | 2023-07-18 | 厦门凯纳石墨烯技术股份有限公司 | Heating and purifying equipment and method for graphene powder |
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| CN101850975A (en) * | 2009-04-01 | 2010-10-06 | 高文秀 | Method for purifying silicon by removing phosphorus and metal impurities |
| CN101850976A (en) * | 2009-04-01 | 2010-10-06 | 高文秀 | Method for removing boron in silicon metal in transfer ladle |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101850975A (en) * | 2009-04-01 | 2010-10-06 | 高文秀 | Method for purifying silicon by removing phosphorus and metal impurities |
| CN101850976A (en) * | 2009-04-01 | 2010-10-06 | 高文秀 | Method for removing boron in silicon metal in transfer ladle |
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