CN106350687B - The device and method of separating-purifying titanium sponge - Google Patents
The device and method of separating-purifying titanium sponge Download PDFInfo
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- CN106350687B CN106350687B CN201610802555.7A CN201610802555A CN106350687B CN 106350687 B CN106350687 B CN 106350687B CN 201610802555 A CN201610802555 A CN 201610802555A CN 106350687 B CN106350687 B CN 106350687B
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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
- C22B9/02—Refining by liquating, filtering, centrifuging, distilling, or supersonic wave action including acoustic waves
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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
- C22B9/05—Refining by treating with gases, e.g. gas flushing also refining by means of a material generating gas in situ
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Abstract
The invention discloses a kind of device and method of separating-purifying titanium sponge, especially a kind of device and method applied to non-ferrous metal metallurgy technical field separating-purifying titanium sponge.The present invention provides one kind, low energy consumption, efficient, with short production cycle, the device of the separating-purifying titanium sponge of good product quality, the present invention also provides one kind, low energy consumption, efficient, with short production cycle, the method for the separating-purifying titanium sponge of good product quality, including following steps：A, vacuumize process is carried out to condenser；B, it is sticked together and is purged to titanium sponge using high temperature argon, and continuous air extraction is carried out to separating-purifying device.The application carries out vacuum purging using high temperature argon to titanium sponge, improves Mg, MgCl in titanium sponge pore2Dynamic conditions is evaporated, distillation equipment vacuum level requirements are low, vapo(u)rizing temperature is low, separating-purifying is efficient；Forced condensation is carried out to condenser using shower water, condenser cooling efficiency is high, and condenses Mg, MgCl2Recycling is convenient.
Description
Technical field
The present invention relates to a kind of device and method of separating-purifying titanium sponge, especially a kind of to be applied to non-ferrous metal metallurgy
The device and method of technical field separating-purifying titanium sponge.
Background technology
Currently, magnesiothermy is unique method prepared by industrial titanium sponge, after magnesium-reduced the product of gained substantially by
55%~60%Ti, 30%~35%Mg, 5%~15%MgCl2, a small amount of titanium lower chloride composition, for sea will be remained in
MgCl in continuous titanium2, Mg, the chloride for the Low-valent Titanium not restored fully and titanium sponge be effectively separated, industrially generally adopt
Separating-purifying is carried out with the method for vacuum distillation.Titanium sponge vacuum distillation production in, for by the Mg of titanium sponge pore,
MgCl2It is detached with higher rate, alembic temperature need to be increased to 1000~1020 DEG C, and by alembic vacuum degree control
It makes in higher level, therefore high to the vacuum suction performance requirement of vacuum pump set, while titanium sponge will also be become by high-temperature heating
It is fine and close.In addition, the conductivity of heat of titanium sponge is poor in alembic, distilling rate Mg, MgCl in by titanium sponge pore2It sticks together table to titanium
Face diffusion rate influences seriously, therefore the vacuum distillation period of titanium sponge is longer, and vacuum distillation is less efficient, and energy consumption is higher.
Existing titanium sponge process for separation and purification and device disclose such as application No. is 201210583541.2 patent
Magnesium chloride containing titanium sponge is washed in a kind of method of magnesium chloride in removal titanium sponge, the proposition of this patent, then to carry out room temperature true
Sky, which distills, removes water process, and magnesium chloride inferior separating effect in the method titanium sponge, titanium sponge water-washing process is oxidizable, magnesium chloride cycle
Using of high cost；Such as application No. is 201310731580.7 patent, the processing that chlorinity is exceeded in a kind of titanium sponge is disclosed
Method, this patent proposes that carrying out heating stage by stage to the exceeded titanium sponge of chlorine is evaporated in vacuo, but the distillation period is long, and sponge titanyl nitrogen contains
Amount is easily exceeded；Such as application No. is the patents of 201310191177.X, disclose a kind of 15 tons of joints of falling U for producing titanium sponge
Device and production technology, this patent carry out separating-purifying using vacuum distillation method titanium sponge, and 750~1000 DEG C of vapo(u)rizing temperature is steamed
The period is evaporated up to 100~150h, therefore it is fine and close to distill high energy consumption, low production efficiency, Sponge Titanium.Therefore in the prior art also
Without one kind, low energy consumption, efficient, with short production cycle, the device and method of the separating-purifying titanium sponge of good product quality.
Invention content
Technical problem to be solved by the invention is to provide one kind, low energy consumption, efficient, with short production cycle, good product quality
Separating-purifying titanium sponge device.
The present invention solve above-mentioned technical problem used by separating-purifying titanium sponge device, including alembic, condenser,
Heating device, argon gas injection apparatus, vacuum pump set are distilled, the condenser is located above alembic, the alembic and condensation
Device is connected to, and the vacuum pump set is connected to condenser, and the distillation heating device is arranged outside alembic, the argon gas injection
The argon gas exit wound of bullet of device is located at distillation pot bottom.
Further, the distillation heating device is hot plate, the alembic is located in hot plate.
Further, the hot plate is anti-heating in vacuum electric furnace.
Further, being provided with heat screen between the alembic and condenser.
Further, there are three the argon nozzles for being mutually 180 degree for setting on the argon gas injection apparatus.
Further, the condenser overhead is provided with spray sprinkler head.
Further, further including purification for argon processing unit, outlet and the argon gas of the purification for argon processing unit spray
The import of injection device is connected, and the import of the argon gas purifying unit is connected with vacuum pump set.
Another technical problem to be solved by this invention is to provide one kind, and low energy consumption, efficient, with short production cycle, product
The method of high-quality separating-purifying titanium sponge.
The method that the present invention solves separating-purifying titanium sponge used by above-mentioned technical problem, including following steps：
A, vacuumize process is carried out to condenser, condenser vacuum is made to be higher than 10Pa；
B, using high temperature argon to remaining Mg and MgCl under vacuum state2Titanium sponge stick together and purged, simultaneously respectively
Alembic, condenser are heated and forced to cool down, and continuous air extraction, wherein high temperature argon are carried out to separating-purifying device
Temperature range is 1000 DEG C~1020 DEG C.
Further, be more than 3000L/s to the speed of exhaust of condenser, the control of alembic outside wall temperature 850 DEG C~
900 DEG C, condenser outer walls temperature is less than 45 DEG C, argon pressure, 0.10MPa~0.12MPa, argon flow amount 2000L/S；Argon gas passes through
It is used continuously after purified treatment.
Further, being recycled after the purified processing of argon gas.
The beneficial effects of the invention are as follows：The application carries out vacuum purging using high temperature argon to titanium sponge, improves sponge
Mg, MgCl in titanium pore2Dynamic conditions is evaporated, distillation equipment vacuum level requirements are low, vapo(u)rizing temperature is low, separating-purifying efficiency
Height, titanium sponge are loose；Forced condensation is carried out to condenser using shower water, condenser cooling efficiency is high, and condense Mg,
MgCl2Recycling is convenient；Argon gas used in the method can be recycled by purified treatment, and argon gas consumption is small.
Description of the drawings
Fig. 1 is the structural schematic diagram of apparatus of the present invention；
Parts, position and number in figure：Alembic 1, condenser 2, hot plate 3, vacuum pump set 4, purification for argon dress
Set 5, argon nozzle 6, heat screen 7, spray sprinkler head 8.
Specific implementation mode
The invention will be further described below in conjunction with the accompanying drawings.
As shown in Figure 1, the device of the separating-purifying titanium sponge of the present invention, including alembic 1, condenser 2, distillation heating dress
It sets, argon gas injection apparatus, vacuum pump set 4, the condenser 2 is located at 1 top of alembic, and the alembic 1 connects with condenser 2
Logical, the vacuum pump set 4 is connected to condenser 2, and the distillation heating device is arranged outside alembic 1, the argon gas injection
The argon gas exit wound of bullet of device is located at 1 bottom of alembic.Wherein condenser 2 is identical as 1 model of alembic, and drainer is located at alembic
Right over 1, and pass through flanged joint.The present apparatus is 1000 DEG C~1020 DEG C using argon gas injection apparatus injection temperation, and air pressure is
0.10MPa~0.12MPa, throughput are the high temperature argon of 2000L/S to remaining Mg and MgCl under vacuum state2Titanium sponge
It sticks together and is purged, while respectively to being heated using distillation heating device alembic 1, carrying out pressure cooling to condenser 2, and
And continuous air extraction is carried out to separating-purifying device using vacuum pump, so as to improve Mg, MgCl in titanium sponge pore2Evaporate dynamics
Condition, reduce to distillation equipment vacuum level requirements, make vapo(u)rizing temperature reduce it is low, improve separating-purifying efficiency, make titanium sponge
It is more loose.
The distillation heating device is hot plate 3, and the alembic 1 is located in hot plate 3.In order to ensure titanium sponge
Evaporation rate, alembic 1 is positioned in hot plate 3, and carries out accurate temperature controlling.
The hot plate 3 is anti-heating in vacuum electric furnace 3.To protect alembic 1 not damaged by atmospheric pressure, hot plate 3
For the anti-heating in vacuum electric furnace 3 with anti-vacuum function.
Heat screen 7 is provided between the alembic 1 and condenser 2.In order to ensure between alembic 1 and condenser 2
Temperature gradient installs heat screen 7 between alembic 1 and condenser 2.
There are three the argon nozzles 6 for being mutually 180 degree for setting on the argon gas injection apparatus.In order to ensure high temperature argon to sea
Effective purging of continuous titanium, argon nozzle 6 are designed at 1 bottom of alembic, and high temperature argon is equal by 3 argon nozzles 6 for being mutually 180 °
Even injection.
2 top of the condenser is provided with spray sprinkler head 8.Specifically, in order to ensure Mg, MgCl2Volatilization steam and condensation
2 inner wall of device collides, and is effectively condensed, and carries out continuous air extraction to condenser 2 using vacuum pump set 4, and set on 2 top of condenser
Meter spray sprinkler head 8.
Further include purification for argon processing unit, the import of the outlet and argon gas injection apparatus of the purification for argon processing unit
It is connected, the import of the argon gas purifying unit 5 is connected with vacuum pump set 4.Purification for argon may be used in purification for argon processing unit
Stove.In order to reduce the consumption of high temperature argon, argon gas is discharged to vacuum pump set 4 by purification for argon stove and carries out purified treatment.
The method of the separating-purifying titanium sponge of the present invention, including following steps：
A, vacuumize process is carried out to condenser 2,2 vacuum degree of condenser is made to be higher than 10Pa；
B, using high temperature argon to remaining Mg and MgCl under vacuum state2Titanium sponge stick together and purged, simultaneously respectively
Alembic 1, condenser 2 are heated and forced to cool down, and separating-purifying device is continuously taken out using vacuum pump set 4
Gas, wherein high temperature argon temperature range are 1000 DEG C~1020 DEG C.Vacuum purging is carried out to titanium sponge using high temperature argon, it can be with
Significantly improve Mg, MgCl in titanium sponge pore2Dynamic conditions is evaporated, is reduced to the vacuum level requirements of distillation equipment, pair will be set
Standby vacuum level requirements are reduced to the order of magnitude of 10Pa from the order of magnitude of 1Pa, while reducing vapo(u)rizing temperature, and can significantly carry
High score is high from purification efficiency, titanium sponge is loose；Using vacuum pump set 4 to condenser 2 carry out continuous air extraction can ensure Mg,
MgCl2The steam that volatilizees is collided with 2 inner wall of condenser, and is effectively condensed.
Prototype group is more than 3000L/s to the speed of exhaust of condenser 2, and 1 outside wall temperature of alembic is controlled 850 DEG C~900
DEG C, 2 outside wall temperature of condenser is less than 45 DEG C, argon pressure, 0.10MPa~0.12MPa, argon flow amount 2000L/S；Argon gas is through net
It is used continuously after change processing.
It is recycled after the purified processing of argon gas.Argon gas is discharged to vacuum pump set 4 by purification for argon stove to carry out at purification
Reason, by treated, argon gas is passed through in alembic 1 repeatedly use again, greatly reduces the consumption of high temperature argon.
Claims (3)
1. using the device of separating-purifying titanium sponge come the method for separating-purifying titanium sponge, the wherein device of separating-purifying titanium sponge
Including alembic (1), condenser (2), distillation heating device, argon gas injection apparatus, vacuum pump set (4), condenser (2) position
Above alembic (1), the alembic (1) is connected to condenser (2), and the vacuum pump set (4) is connected to condenser (2),
The distillation heating device setting is external in alembic (1), and the argon gas exit wound of bullet of the argon gas injection apparatus is located at alembic (1)
Bottom, it is characterised in that：Including following steps：
A, vacuumize process is carried out to condenser (2), condenser (2) vacuum degree is made to be higher than 10Pa；
B, using high temperature argon to remaining Mg and MgCl under vacuum state2Titanium sponge stick together and purged, while respectively to distillation
Tank (1), condenser (2) are heated and are forced to cool down, and carry out continuous air extraction, wherein high temperature argon to separating-purifying device
Temperature range is 1000 DEG C~1020 DEG C.
2. the method for separating-purifying titanium sponge as described in claim 1, it is characterised in that：To the speed of exhaust of condenser (2)
More than 3000L/s, the control of alembic (1) outside wall temperature is at 850 DEG C~900 DEG C, and condenser (2) outside wall temperature is less than 45 DEG C, argon
Atmospheric pressure 0.10MPa~0.12MPa, argon flow amount 2000L/S；It is used continuously after the purified processing of argon gas.
3. the method for separating-purifying titanium sponge as described in claim 1, it is characterised in that：Being recycled after the purified processing of argon gas makes
With.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610802555.7A CN106350687B (en) | 2016-09-05 | 2016-09-05 | The device and method of separating-purifying titanium sponge |
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| CN201610802555.7A CN106350687B (en) | 2016-09-05 | 2016-09-05 | The device and method of separating-purifying titanium sponge |
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Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107287449A (en) * | 2017-08-17 | 2017-10-24 | 东方弗瑞德（北京）科技有限公司 | A kind of argon gas introducing device and introducing method produced for magnesium method titanium sponge |
| CN107674999B (en) * | 2017-10-10 | 2019-10-01 | 攀钢集团研究院有限公司 | The method of titanium sponge vacuum distillation |
| CN108690916A (en) * | 2018-08-02 | 2018-10-23 | 绵阳力洋英伦科技有限公司 | High temperature distillation separation equipment and separation method applied to titanium sponge fused salt |
| CN109825854A (en) * | 2019-03-26 | 2019-05-31 | 北京科技大学 | A kind of molten-salt electrolysis-high temperature distillation prepares the device and method of high-purity titanium |
| CN112030009B (en) * | 2020-08-31 | 2022-07-19 | 攀钢集团攀枝花钢铁研究院有限公司 | Device and method for producing titanium sponge with low nitrogen and oxygen impurity content and low Brinell hardness |
| CN112029996B (en) * | 2020-08-31 | 2022-07-19 | 攀钢集团攀枝花钢铁研究院有限公司 | Production method of high-quality sponge titanium with low oxygen impurity content |
| CN114703380A (en) * | 2022-03-24 | 2022-07-05 | 朝阳金达钛业股份有限公司 | Production method of titanium sponge with ultralow chlorine content |
| CN115821069B (en) * | 2022-12-07 | 2023-06-16 | 云南国钛金属股份有限公司 | Temperature control method for rotor-grade titanium sponge inverted U-shaped distillation process |
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| JP4185832B2 (en) * | 2003-08-19 | 2008-11-26 | 孝 前島 | Negative pressure combustion incinerator |
| WO2006010223A1 (en) * | 2004-07-30 | 2006-02-02 | Commonwealth Scientific And Industrial Research Organisation | Industrial process |
| CN2801807Y (en) * | 2005-05-26 | 2006-08-02 | 唐山市天赫钛业有限公司 | Direct cooling type condensation device of reductive distilling furnace |
| CN203569169U (en) * | 2013-10-31 | 2014-04-30 | 攀钢集团钛业有限责任公司 | Cooling device for distillates in titanium sponge condensing tank |
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Effective date of registration: 20180720 Address after: 610306 Chengdu City, Chengdu, Sichuan, China (Sichuan) free trade test zone, Chengdu City, Qingbaijiang District, xiangdao Boulevard, Chengxiang Town, No. 1509 (room 13, A District, railway port mansion), room 1319 Applicant after: Chengdu advanced metal material industry technology Research Institute Co., Ltd. Address before: 617000 Taoyuan street, East District, Panzhihua, Sichuan Province, No. 90 Applicant before: Pangang Group Panzhihua Iron & Steel Research Institute Co., Ltd. |
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Address after: 610306 Chengdu City, Chengdu, Sichuan, China (Sichuan) free trade test zone, Chengdu City, Qingbaijiang District, xiangdao Boulevard, Chengxiang Town, No. 1509 (room 13, A District, railway port mansion), room 1319 Patentee after: Chengdu advanced metal material industry technology Research Institute Co.,Ltd. Address before: 610306 Chengdu City, Chengdu, Sichuan, China (Sichuan) free trade test zone, Chengdu City, Qingbaijiang District, xiangdao Boulevard, Chengxiang Town, No. 1509 (room 13, A District, railway port mansion), room 1319 Patentee before: CHENGDU ADVANCED METAL MATERIALS INDUSTRY TECHNOLOGY RESEARCH INSTITUTE Co.,Ltd. |