CN106834747A - A kind of method for preparing titanium sponge - Google Patents
A kind of method for preparing titanium sponge Download PDFInfo
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- CN106834747A CN106834747A CN201710040045.5A CN201710040045A CN106834747A CN 106834747 A CN106834747 A CN 106834747A CN 201710040045 A CN201710040045 A CN 201710040045A CN 106834747 A CN106834747 A CN 106834747A
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- titanium
- titanium tetrachloride
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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
- C22B34/1263—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, e.g. by reduction
- C22B34/1268—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, e.g. by reduction using alkali or alkaline-earth metals or amalgams
- C22B34/1272—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, e.g. by reduction using alkali or alkaline-earth metals or amalgams reduction of titanium halides, e.g. Kroll process
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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
- C22B34/1204—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 preliminary treatment of ores or scrap to eliminate non- titanium constituents, e.g. iron, without attacking the titanium constituent
- C22B34/1209—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 preliminary treatment of ores or scrap to eliminate non- titanium constituents, e.g. iron, without attacking the titanium constituent by dry processes, e.g. with selective chlorination of iron or with formation of a titanium bearing slag
-
- 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
- C22B5/00—General methods of reducing to metals
- C22B5/02—Dry methods smelting of sulfides or formation of mattes
- C22B5/04—Dry methods smelting of sulfides or formation of mattes by aluminium, other metals or silicon
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- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention discloses a kind of method for preparing titanium sponge, ilmenite is taken, add anthracite to carry out reduction reaction, be made titanium slag, it is standby；After titanium slag and petroleum coke are mixed, it is suspended in sodium chloride fused salt, is passed through chlorine, obtains rough titanium tetrachloride；Rough titanium tetrachloride carries out rectifying in rectifying column, obtains titanium tetrachloride experimental liquid；To aluminium powder is added in titanium tetrachloride experimental liquid, reacted at 130 140 DEG C, be made refining titanic chloride；Reactor is soaked with hot acid, is then washed with water, after drying, after reactor wall smears titanium；To refining titanic chloride and magnesium is added in reactor, intensification is oozed titanium, is obtained final product.The inventive method reduces product impurity content, changes product appearance color, improves yield rate, improves product quality.
Description
Technical field
The present invention relates to a kind of production method of titanium sponge, the titanium sponge that particularly a kind of impurity content is low, energy consumption is low
Preparation method.
Background technology
Titanium sponge is the biscuit titanium that metallothermic processes is produced.Purity (quality) is generally 99.1%-
99.7%.Impurity element (quality) total amount is 0.3%-0.9%, and impurity element oxygen (quality) is 0.06%-0.20%, hardness
(HB) it is 100-157, the difference according to purity is divided into five grades of MHTiO to MHTi4.Titanium sponge is to produce industrial titanium alloy
Primary raw material.
Titanium sponge production is the basic link of Ti industry, and it is the raw material of titanium, titanium valve and other titanium components.Ilmenite
Become titanium tetrachloride, then be put into the stainless cylinder of steel of sealing, be filled with argon gas, make they and metal reactive magnesium, just obtain " sponge
Titanium ".This porous " titanium sponge " can not be used directly, it is necessary to which they are fused into liquid, Cai Nengzhu in electric furnace
Into titanium ingot.
Magnesium-reduced vacuum distillation method produces titanium sponge, be by raw material magnesium and refined titanic chloride under certain condition, in reaction
Reaction production titanium sponge in device.
The content of the invention
The purpose of the present invention, is to provide a kind of method for preparing titanium sponge.The inventive method reduces product impurity content,
Product quality is improve, and energy consumption is low.
What the present invention was realized in：
A kind of method for preparing titanium sponge, comprises the following steps：
(1) take at ilmenite, 1600-1900 DEG C, be 4-6 by ilmenite and anthracitic weight ratio:1 ratio adds nothing
Bituminous coal carries out reduction reaction, is made titanium slag, standby；
(2) by weight it is 6-8 by titanium slag and petroleum coke:After 1 mixing, it is suspended in sodium chloride fused salt, is passed through chlorine, obtains
Rough titanium tetrachloride；
(3) rough titanium tetrachloride carries out rectifying in rectifying column, controls each parameter of rectifying column to be：Charging rate 10-12t/
H, 65-75 DEG C of feeding temperature, reflux ratio 50-80,130-135 DEG C of tower top temperature, 80-90 DEG C of phegma temperature, tower top pressure -1-
3kPa, rate of withdrawal is that charging rate is 1-4%；Obtain titanium tetrachloride experimental liquid；
(4) it is 10-12 by the weight ratio of titanium tetrachloride experimental liquid and aluminium powder：1 ratio adds in titanium tetrachloride experimental liquid
Enter reaction at aluminium powder, 130-140 DEG C, be made refining titanic chloride；
(5) reactor is soaked 1-3 days with hot acid, is then washed with water, after drying, inner wall surface area 20- is pressed in reactor wall
30g/m2After smearing titanium；To refining titanic chloride and magnesium is added in reactor, it is warming up to 800-950 DEG C and oozes titanium, obtains final product.
The foregoing method for preparing titanium sponge, in the step (1), the ilmenite is 5 with anthracitic weight ratio:1.
The foregoing method for preparing titanium sponge, the step (3) is：Rough titanium tetrachloride carries out rectifying in rectifying column, control
Each parameter of rectifying column processed is：Charging rate 11t/h, 65-75 DEG C of feeding temperature, reflux ratio 65,130-135 DEG C of tower top temperature is returned
80-90 DEG C of flow liquid temperature, tower top pressure -1-3kPa, rate of withdrawal is that charging rate is 2%；Obtain titanium tetrachloride experimental liquid.
The foregoing method for preparing titanium sponge, in the step (4), titanium tetrachloride experimental liquid is 11 with the weight ratio of aluminium powder：
1。
The foregoing method for preparing titanium sponge, in the step (5), the temperature of hot acid is 50-60 DEG C.
The foregoing method for preparing titanium sponge, in the step (5), hot acid is that concentration is the sulfuric acid of 5-10%.
The foregoing method for preparing titanium sponge, in the step (5), the weight ratio of refining titanic chloride and magnesium is 5-15:23.
The weight ratio of the foregoing method for preparing titanium sponge, the refining titanic chloride and magnesium is 10:23.
Impurity is obtained in the titanium sponge for oozing the reactor production that titanium effect is preferable, after oozing titanium of titanizing method of the present invention
It is greatly reduced；Titanizing method temperature of the present invention is low, it is to avoid high temperature oozes titanium new reactor is constituted and damages, and improves after oozing titanium
The service life of reactor, while reducing energy consumption；Titanizing method of the present invention improves the temperature of acidleach, when can shorten acidleach
Between, improve acid leaching efficiency.Applicant has carried out long-term substantial amounts of experimental study to the production method of titanium sponge, and part test is such as
Under：
1 test material
1.1 contrast titanium sponges 1：It is commercially available；
1.2 contrast titanium sponges 2：Manufacture craft is：Petroleum coke and melting ilmenite obtain two in 1600 DEG C of -1800 DEG C of reduction
Titanium oxide, at 900 DEG C, is passed through chlorine and titanium dioxide reaction obtains titanium tetrachloride, standby；Simple metal is put into retort
Magnesium, full of argon gas, after heating melts magnesium, adds titanium tetrachloride at 800-900 DEG C, discharges magnesium chloride, obtains final product.
1.3 titanium sponges of the present invention：Produced by embodiment 1.
2 methods and result
Contrast titanium sponge and titanium sponge index of the present invention are contrasted, concrete outcome part table 1, table 2 and table 3.
Table 1 contrasts titanium sponge 1
Table 2 contrasts titanium sponge 2
The titanium sponge that table 3 is produced using embodiment 1
, it is apparent that the titanium sponge that is produced of the method for the embodiment of the present invention 1 is than original work from table 1, table 2 and table 3
The titanium sponge quality that skill is produced is significantly improved.After testing, molten titanium ingot of the titanium sponge of present invention production to Downstream processing titanium
Technique brings highly beneficial condition, reduces the segregation problems of melted ingot, and increased the service life of melted ingot crucible.
Compared with prior art, the inventive method reduces product impurity content, improves product quality, and energy consumption is low.
Specific embodiment
Embodiment 1.
A kind of method for preparing titanium sponge, comprises the following steps：
(1) take at ilmenite, 1600-1900 DEG C, be 5 by ilmenite and anthracitic weight ratio:1 ratio adds smokeless
Coal carries out reduction reaction, is made titanium slag, standby；
(2) by weight it is 7 by titanium slag and petroleum coke:After 1 mixing, it is suspended in sodium chloride fused salt, is passed through chlorine, obtains slightly
Titanium tetrachloride processed；
(3) rough titanium tetrachloride carries out rectifying in rectifying column, controls each parameter of rectifying column to be：Charging rate 11t/h, enters
65-75 DEG C of material temperature degree, reflux ratio 65,130-135 DEG C of tower top temperature, 80-90 DEG C of phegma temperature, tower top pressure -1-3kPa is adopted
Go out speed for charging rate is 2%；Obtain titanium tetrachloride experimental liquid；
(4) it is 11 by the weight ratio of titanium tetrachloride experimental liquid and aluminium powder：1 ratio in titanium tetrachloride experimental liquid to adding aluminium
Powder, reacts at 130-140 DEG C, is made refining titanic chloride；
(5) reactor concentration is the vitriol lixiviation 2 days that 8%, temperature is 50-60 DEG C, is then washed with water, after drying,
Reactor wall presses inner wall surface area 25g/m2After smearing titanium；To refining titanic chloride and magnesium is added in reactor, tetrachloro is refined
The weight ratio for changing titanium and magnesium is 10:23, it is warming up to 800-950 DEG C and oozes titanium, obtain final product.
Embodiment 2.
A kind of method for preparing titanium sponge, comprises the following steps：
(1) take at ilmenite, 1600-1900 DEG C, be 6 by ilmenite and anthracitic weight ratio:1 ratio adds smokeless
Coal carries out reduction reaction, is made titanium slag, standby；
(2) by weight it is 8 by titanium slag and petroleum coke:After 1 mixing, it is suspended in sodium chloride fused salt, is passed through chlorine, obtains slightly
Titanium tetrachloride processed；
(3) rough titanium tetrachloride carries out rectifying in rectifying column, controls each parameter of rectifying column to be：Charging rate 12t/h, enters
65-75 DEG C of material temperature degree, reflux ratio 80,130-135 DEG C of tower top temperature, 80-90 DEG C of phegma temperature, tower top pressure -1-3kPa is adopted
Go out speed for charging rate is 4%；Obtain titanium tetrachloride experimental liquid；
(4) it is 12 by the weight ratio of titanium tetrachloride experimental liquid and aluminium powder：1 ratio in titanium tetrachloride experimental liquid to adding aluminium
Powder, reacts at 130-140 DEG C, is made refining titanic chloride；
(5) reactor concentration is 10%, and temperature is 50-60 DEG C of hot acid acidleach 3 days, is then washed with water, after drying,
Reactor wall presses inner wall surface area 30g/m2After smearing titanium；To refining titanic chloride and magnesium is added in reactor, tetrachloro is refined
The weight ratio for changing titanium and magnesium is 5-15:23；It is warming up to 800-950 DEG C and oozes titanium, obtains final product.
Embodiment 3.
A kind of method for preparing titanium sponge, comprises the following steps：
(1) take at ilmenite, 1600-1900 DEG C, be 4 by ilmenite and anthracitic weight ratio:1 ratio adds smokeless
Coal carries out reduction reaction, is made titanium slag, standby；
(2) by weight it is 6 by titanium slag and petroleum coke:After 1 mixing, it is suspended in sodium chloride fused salt, is passed through chlorine, obtains slightly
Titanium tetrachloride processed；
(3) rough titanium tetrachloride carries out rectifying in rectifying column, controls each parameter of rectifying column to be：Charging rate 10t/h, enters
65-75 DEG C of material temperature degree, reflux ratio 50,130-135 DEG C of tower top temperature, 80-90 DEG C of phegma temperature, tower top pressure -1-3kPa is adopted
Go out speed for charging rate is 1%；Obtain titanium tetrachloride experimental liquid；
(4) it is 10 by the weight ratio of titanium tetrachloride experimental liquid and aluminium powder：1 ratio in titanium tetrachloride experimental liquid to adding aluminium
Powder, reacts at 130-140 DEG C, is made refining titanic chloride；
(5) reactor temperature is the vitriol lixiviation 1 day that 50-60 DEG C of concentration is 5%, is then washed with water, after drying, anti-
Device inwall is answered by inner wall surface area 20g/m2After smearing titanium；To refining titanic chloride and magnesium is added in reactor, four chlorinations are refined
The weight ratio of titanium and magnesium is 5:23；It is warming up to 800-950 DEG C and oozes titanium, obtains final product.
Claims (8)
1. a kind of method for preparing titanium sponge, it is characterised in that：Comprise the following steps：
(1) take at ilmenite, 1600-1900 DEG C, be 4-6 by ilmenite and anthracitic weight ratio:1 ratio adds anthracite
Reduction reaction is carried out, titanium slag is made, it is standby；
(2) by weight it is 6-8 by titanium slag and petroleum coke:After 1 mixing, it is suspended in sodium chloride fused salt, is passed through chlorine, obtains rough
Titanium tetrachloride；
(3) rough titanium tetrachloride carries out rectifying in rectifying column, controls each parameter of rectifying column to be：Charging rate 10-12t/h, enters
65-75 DEG C of material temperature degree, reflux ratio 50-80,130-135 DEG C of tower top temperature, 80-90 DEG C of phegma temperature, tower top pressure -1-
3kPa, rate of withdrawal is that charging rate is 1-4%；Obtain titanium tetrachloride experimental liquid；
(4) it is 10-12 by the weight ratio of titanium tetrachloride experimental liquid and aluminium powder：1 ratio in titanium tetrachloride experimental liquid to adding aluminium
Powder, reacts at 130-140 DEG C, is made refining titanic chloride；
(5) reactor is soaked 1-3 days with hot acid, is then washed with water, after drying, inner wall surface area 20-30g/m is pressed in reactor wall2
After smearing titanium；To refining titanic chloride and magnesium is added in reactor, it is warming up to 800-950 DEG C and oozes titanium, obtains final product.
2. the method for preparing titanium sponge as claimed in claim 1, it is characterised in that：In the step (1), the ilmenite and nothing
The weight ratio of bituminous coal is 5:1.
3. the method for preparing titanium sponge as claimed in claim 1, it is characterised in that：The step (3) is：Rough titanium tetrachloride in
Rectifying is carried out in rectifying column, controls each parameter of rectifying column to be：Charging rate 11t/h, 65-75 DEG C of feeding temperature, reflux ratio 65, tower
130-135 DEG C of the temperature in top, 80-90 DEG C of phegma temperature, tower top pressure -1-3kPa, rate of withdrawal is that charging rate is 2%；
To titanium tetrachloride experimental liquid.
4. the method for preparing titanium sponge as claimed in claim 1, it is characterised in that：In the step (4), titanium tetrachloride experimental liquid
It is 11 with the weight ratio of aluminium powder：1.
5. the method for preparing titanium sponge as claimed in claim 1, it is characterised in that：In the step (5), the temperature of hot acid is
50-60℃。
6. the method for preparing titanium sponge as claimed in claim 1, it is characterised in that：In the step (5), hot acid is that concentration is 5-
10% sulfuric acid.
7. the method for preparing titanium sponge as claimed in claim 1, it is characterised in that：In the step (5),
The weight ratio of refining titanic chloride and magnesium is 5-15:23.
8. the method for preparing titanium sponge as claimed in claim 7, it is characterised in that：The weight ratio of the refining titanic chloride and magnesium
It is 10:23.
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| CN201710040045.5A CN106834747A (en) | 2017-01-18 | 2017-01-18 | A kind of method for preparing titanium sponge |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108754144A (en) * | 2018-08-08 | 2018-11-06 | 成都先进金属材料产业技术研究院有限公司 | The production method of low iron content high-quality titanium sponge |
| CN111549240A (en) * | 2020-04-30 | 2020-08-18 | 广州上仕工程管理有限公司 | Preparation method of non-ferrous metal alloy material |
| CN112029996A (en) * | 2020-08-31 | 2020-12-04 | 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 |
| CN115896542A (en) * | 2022-12-07 | 2023-04-04 | 云南国钛金属股份有限公司 | Titanium white sponge titanium co-production coupling production method |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104004987A (en) * | 2014-06-18 | 2014-08-27 | 四川恒为制钛科技有限公司 | Titanizing method of reactor for sponge titanium production |
| CN104150529A (en) * | 2014-06-25 | 2014-11-19 | 陕西高华知本化工科技有限公司 | Method for refining titanium tetrachloride by removing vanadium through aluminum powder |
| CN105271385A (en) * | 2015-11-06 | 2016-01-27 | 攀钢集团攀枝花钢铁研究院有限公司 | Method of removing silicon in coarse titanium tetrachloride |
-
2017
- 2017-01-18 CN CN201710040045.5A patent/CN106834747A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104004987A (en) * | 2014-06-18 | 2014-08-27 | 四川恒为制钛科技有限公司 | Titanizing method of reactor for sponge titanium production |
| CN104150529A (en) * | 2014-06-25 | 2014-11-19 | 陕西高华知本化工科技有限公司 | Method for refining titanium tetrachloride by removing vanadium through aluminum powder |
| CN105271385A (en) * | 2015-11-06 | 2016-01-27 | 攀钢集团攀枝花钢铁研究院有限公司 | Method of removing silicon in coarse titanium tetrachloride |
Non-Patent Citations (1)
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| 《钛工业进展》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108754144A (en) * | 2018-08-08 | 2018-11-06 | 成都先进金属材料产业技术研究院有限公司 | The production method of low iron content high-quality titanium sponge |
| CN111549240A (en) * | 2020-04-30 | 2020-08-18 | 广州上仕工程管理有限公司 | Preparation method of non-ferrous metal alloy material |
| CN112029996A (en) * | 2020-08-31 | 2020-12-04 | 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 |
| CN115896542A (en) * | 2022-12-07 | 2023-04-04 | 云南国钛金属股份有限公司 | Titanium white sponge titanium co-production coupling production method |
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