CN108330370A - A kind of production method of vananum - Google Patents
A kind of production method of vananum Download PDFInfo
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- CN108330370A CN108330370A CN201810228430.7A CN201810228430A CN108330370A CN 108330370 A CN108330370 A CN 108330370A CN 201810228430 A CN201810228430 A CN 201810228430A CN 108330370 A CN108330370 A CN 108330370A
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- aluminium
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- vanadic anhydride
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- vananum
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C27/00—Alloys based on rhenium or a refractory metal not mentioned in groups C22C14/00 or C22C16/00
- C22C27/02—Alloys based on vanadium, niobium, or tantalum
- C22C27/025—Alloys based on vanadium, niobium, or tantalum alloys based on vanadium
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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
- C22B34/20—Obtaining niobium, tantalum or vanadium
- C22B34/22—Obtaining vanadium
-
- 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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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
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- Mechanical Engineering (AREA)
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Abstract
The invention discloses a kind of production methods of vananum, belong to metallurgical technology field.The technical problem to be solved by the present invention is to improve vananum yield rate and quality, reduce vananum impurity content, and expands its production scale, reduces cost.A kind of production method of vananum, including：First batch of vanadic anhydride and aluminium is added into the graphite crucible with drilling lid, igniting carries out thermite reaction, after the reaction was complete, sequentially add subsequent batches vanadic anhydride and aluminium, thermite reaction is carried out respectively, until vanadic anhydride and aluminium are all added simultaneously, the reaction was complete, and the separation of slag gold obtains vananum.The method of the present invention, using the graphite crucible with drilling lid as furnace body is smelted, expands production scale by the way of batch charging, the yield for improving vanadium, without adding slag making coolant, cost is lower, gained alloy purity and quality higher comply fully with the requirement that industry produces greatly.
Description
Technical field
The invention belongs to metallurgical technology fields, and in particular to a kind of production method of vananum.
Background technology
Aluminothermic process is a kind of method that the reproducibility using aluminium obtains refractory metal simple substance.Thermite refers to aluminium and metal oxygen
The mixture of compound.After aluminium powder and a certain amount of refractory metal oxide (such as iron oxide) are mixed, ignited with magnesium rod, it can
To see aluminium powder vigorous reaction at a higher temperature, a large amount of heat is released in reaction, and is given out great brilliancy.Product is oxygen
Change the simple substance of aluminium and the refractory metal.Thermit reaction is very fierce, is difficult control after lighting so being difficult to extinguish after lighting
Reaction process.The reaction is to be packed into furnace charge, and generate (1700 DEG C~3000 DEG C) of high temperature rapidly in an instant after firing and make
Furnace charge is in molten condition, and then carries out alloy refinement.The advantages of this smelting mode, is to be not required to input electric heating, and low energy consumption,
It is lower than electric arc furnace smelting method production cost.
Vananum is a kind of basic material for titanium alloy, is currently that second largest after application of RE in the steel answers after vanadium
Use field.Ti-6Al-4V and Ti-8Al-1Mo-1V, both titanium alloys account for the 50% of titanium alloy market in total, are mainly used for giving birth to
Produce jet engine, high-speed aircraft skeleton and rocket engine casing.Titanium alloy production vanadium used is with vananum shape
Formula is added.The country such as Japan, the U.S., Britain is also in the further application study increased containing V-Ti in civilian industry.
Currently, generally using vanadic anhydride as raw material in vananum production technology, vananum is produced using aluminothermic process.
Since vanadic anhydride and metal reactive aluminum release a large amount of heat, heat is substantially superfluous, it is explosive so that reaction is presented, in thermal insulation
In the case of be enough that the temperature of system is made to be increased to 3000 DEG C or more.Therefore, a certain amount of inert material is usually incorporated in furnace charge
Matter (being commonly called as the thermit powder that disappears) controls the Wen Sheng of reaction speed and reaction product.Due to disappear thermit powder always contain a certain amount of Fe, Si,
P and heavy metal element, therefore impurity content is higher in the vananum produced.
A kind of preparation method of vanadium-aluminum alloy material is disclosed in patent document CN200910117560.4, which presses quality
Percentages weigh powdered Al20%~33.1%, V2O550%~66.9%, it mixes 8~16 hours in the ball mill
Afterwards, it is placed in copper mould and is compacted under the pressure of 60~80MPa with forcing press, the mold equipped with the reaction mass pressed is put in
In thermit reaction container, detonator is placed on material, and remaining air is blown out with inert gas, under the protection of 2~7MPa argon gas,
It is heated to 300 DEG C or so to be reacted, obtains vananum, wherein according to mass percent, V is that 75%~95%, Al is
5.0%~25.0%, S content about 0.15%, Fe contents about 0.50%.Obviously in above-mentioned technique, Fe in the product obtained
It is higher with the impurity contents such as S, this is because some impurity can be introduced in the ball mill by mixing 8~16 hours.In addition, due to aluminothermy
Reaction carries out in closed pressure vessel, therefore strongly limits the yield of vananum, further, since requiring the resistance to of equipment
It presses performance strong, therefore manufacturing cost can be improved.
Invention content
Contain the technical problem to be solved by the present invention is to improve vananum yield rate and quality, reduce vananum impurity
Amount, and expand its production scale, reduce cost.
We solve technical solution used by above-mentioned technical problem, and there is provided a kind of production methods of vananum, should
Method includes the following steps：
First batch of vanadic anhydride and aluminium are added into the graphite crucible with drilling lid, it is anti-that igniting carries out aluminothermic reduction
It answers, after the reaction was complete, sequentially adds subsequent batches vanadic anhydride and aluminium, carry out thermite reaction respectively, until five oxidations
All simultaneously the reaction was complete for addition for two vanadium and aluminium, and the separation of slag gold obtains vananum.
Wherein, in the production method of vananum described above, the total mass ratio of the vanadic anhydride and aluminium is
1.15~1.8：1.
Wherein, in the production method of vananum described above, total addition of the vanadic anhydride is no more than
2000kg。
Wherein, in the production method of vananum described above, the batch that vanadic anhydride and aluminium is added is 2~4 batches.
Wherein, in the production method of vananum described above, the gross mass of vanadic anhydride in terms of 100%, aluminium
Gross mass is 100% meter：When the batch that vanadic anhydride and aluminium is added is 2 batches, first vanadic anhydride being added and the
The mass percent of the vanadic anhydride of two batches of additions is 90%~60%：10%~40%；First aluminium and second being added
The mass ratio for criticizing the aluminium being added is 90%~60%：10%~40%.
Wherein, in the production method of vananum described above, the gross mass of vanadic anhydride in terms of 100%, aluminium
Gross mass is 100% meter：When the batch that vanadic anhydride and aluminium is added is 3 batches, first vanadic anhydride being added, second
The mass ratio for criticizing the vanadic anhydride that the vanadic anhydride being added is added with third batch is 70%~60%：20%~30%：
10%；The mass ratio for the aluminium that the aluminium that first aluminium being added, second batch are added is added with third batch is 70%~60%：20%~
30%：10%.
Wherein, in the production method of vananum described above, the gross mass of vanadic anhydride in terms of 100%, aluminium
Gross mass is 100% meter：When the batch that vanadic anhydride and aluminium is added is 4 batches, first vanadic anhydride being added, second
Criticize the vanadic anhydride being added, third criticizes the vanadic anhydride being added and the mass ratio of the 4th batch of vanadic anhydride being added is
50%：30%：10%：10%；The aluminium for the aluminium, third batch addition that first aluminium being added is added with second batch and the 4th batch of addition
Aluminium mass ratio be 50%：30%：10%：10%.
Wherein, in the production method of vananum described above, purity >=99.7% of the vanadic anhydride.
Wherein, in the production method of vananum described above, purity >=99.85% of the aluminium.
Wherein, in the production method of vananum described above, the granularity of the aluminium is 1~10mm.
Wherein, in the production method of vananum described above, it is described drilling lid hole density be 15~20/
m2；A diameter of 1~2cm in the hole.
Wherein, in the production method of vananum described above, the inner wall of the graphite crucible is coated with electric-melting magnesium chamotte.
Wherein, in the production method of vananum described above, the criterion that the reaction was complete is graphite cap bore
Locate no apparent flare.
Wherein, in the production method of vananum described above, all simultaneously the reaction was complete for addition for vanadic anhydride and aluminium
Afterwards, it stands and is no less than 30min, then the separation of slag gold.
The present invention also provides the vananum that the production method by vananum described above is prepared, chemistry
Ingredient is：V65.9wt%~90.13wt%, Al33.72wt%~9.49wt%, Fe≤0.10wt%, Si≤0.18wt%.
The beneficial effects of the invention are as follows：
The method of the present invention is using vanadic anhydride and aluminum shot as raw material, by the way of batch charging, and keeps aluminium excessive, can make
The alloy pig long period is kept molten by, and expands production scale, improves the yield of vanadium；Using the stone with drilling lid
Black crucible carries out electric-melting magnesium chamotte coating as smelting furnace body, and in inner wall, and reduction reaction can be controlled to suitable temperature, be not necessarily to
It adds the slag making coolants such as conventional lime and controls heat, cost is lower, it is possible to reduce the introducing of impurity is conducive to further subtract
The content of impurity, gained alloy purity higher in few vananum；And the graphite crucible used can either with drilling lid
It prevents from the aluminium alloy splash of smelting process from can play the process of heat preservation again to detach conducive to slag gold, alloy presentation quality is more smooth whole
Clean, alloy mass higher is carrying out that when alloy cake is broken higher yield rate can be obtained, and comply fully with that industry produces greatly wants
It asks.
Specific implementation mode
Specifically, a kind of production method of vananum, includes the following steps：
First batch of vanadic anhydride and aluminium are added into the graphite crucible with drilling lid, it is anti-that igniting carries out aluminothermic reduction
It answers, after the reaction was complete, sequentially adds subsequent batches vanadic anhydride and aluminium, carry out thermite reaction respectively, until five oxidations
All simultaneously the reaction was complete for addition for two vanadium and aluminium, and the separation of slag gold obtains vananum.
The mass ratio that the method for the present invention controls total addition of raw material vanadic anhydride and aluminium first is 1.15~1.8：1,
Total addition of vanadic anhydride is no more than 2000kg, using excessive aluminium, can pass through aluminium and gold during reduction reaction
The fusion for belonging to vanadium forms vananum, then uses batch charging mode, the alloy pig long period is made to be kept molten by, to expand
Big production scale (currently, the production scale of vananum is generally 500kg, the present invention can be expanded to 1t or so), and improve
The yield of vanadium；Total addition of vanadic anhydride can be selected according to actual conditions, but preferably no more than 2000kg.
Experiment is found, vanadic anhydride and 2~4 batches of addition progress thermite reactions of aluminium point is more suitable, in batches mistake
It is more, it is unfavorable for improving production efficiency, and generate spot segregation to influence product quality；The tool for carrying out thermite reaction is added portionwise
Gymnastics conduct：First vanadic anhydride and aluminium is added, igniting carries out thermite reaction, and after the reaction was complete, second batch is added
Thermite reaction is carried out, and so on, until vanadic anhydride and aluminium are all added simultaneously, the reaction was complete；Since aluminothermic reduction is anti-
(generally 30s or so) very short between seasonable, can be according to not having apparent flare, to judge that reaction is complete at graphite cap bore；In addition,
In addition to first addition vanadic anhydride and aluminium need to light a fire, subsequent batches need not light a fire again, complete by in-furnace temperature
Thermit reaction can occur again.
In order to control reaction rhythm, heat size utilization rate is improved, the gross mass of vanadic anhydride is in terms of 100%, total matter of aluminium
Amount is 100% meter：When dividing 2 batches to be added, the matter for the vanadic anhydride that first vanadic anhydride being added is added with second batch
It is 90%~60% to measure percentage：10%~40%；The mass ratio for the aluminium that first aluminium being added is added with second batch is 90%
~60%：10%~40%；When dividing 3 batches to be added, vanadic anhydride of first addition, the vanadic anhydride of second batch addition
The mass ratio for the vanadic anhydride being added with third batch is 70%~60%：20%~30%：10%；First aluminium being added,
The mass ratio for the aluminium that the aluminium that second batch is added is added with third batch is 70%~60%：20%~30%：10%；Add when dividing 4 batches
It is fashionable, vanadic anhydride that vanadic anhydride that first vanadic anhydride being added, second batch are added, third batch are added and the
The mass ratio of the vanadic anhydride of four batches of additions is 50%：30%：10%：10%；First aluminium being added is added with second batch
Aluminium, the aluminium that third batch is added and the aluminium of the 4th batch of addition mass ratio be 50%：30%：10%：10%.
During reduction reaction, furnace body is smelted since the present invention is used as using the graphite crucible with drilling lid, control
The density in the hole of system drilling lid is 15~20/m2, a diameter of 1~2cm in hole, and carry out electric-melting magnesium chamotte painting in its inner wall
Layer can control reaction temperature at 1600 DEG C~1900 DEG C, there is no need to add the slag making coolant such as conventional lime to control heat,
Production cost is not only reduced, the introducing of impurity can be more reduced, is conducive to be further reduced the content of impurity in vananum,
Gained alloy purity higher.In addition, the graphite crucible used can either prevent the aluminium alloy of smelting process from spraying with drilling lid
It splashes and the process of heat preservation can be played and detached conducive to slag gold；It is smelted using graphite crucible, alloy presentation quality is compared with than knotting stove
The alloy of body is more smooth clean and tidy, alloy mass higher, is carrying out that when alloy cake is broken higher yield rate can be obtained, is according with completely
Close the requirement that industry produces greatly.
In the method for the present invention, igniting reduction igniting agent used is barium peroxide and aluminium powder, is ignited using magnesium ribbon.
In order to be further reduced the content of impurity in vananum, purity >=99.7% of the vanadic anhydride, institute
Purity >=99.85% of aluminium is stated, the granularity of aluminium is 1~10mm.
After vanadic anhydride and aluminium are all added and the reaction was complete, in order to keep the separation of slag gold more thorough, improve vanadium yield and
Alloy finished product rate can stand no less than 30min, then carry out slag gold separation.
The present invention is improved by the production method to vananum, is expanded the production scale of vananum, is reduced
Production cost, the chemical composition for preparing gained vananum are：V65.9wt%~90.13wt%, Al33.72wt%~
9.49wt%, Fe≤0.10wt%, Si≤0.18wt%, quality meet the requirement that finishing operations continue processing.
Below by embodiment, invention is further described in detail, but does not therefore limit the scope of the present invention
Among the embodiment described range.
Embodiment 1
Take 100kg vanadic anhydrides, 55.7kg aluminum shots are raw material, and the weight proportion of vanadic anhydride and aluminum shot is 1.68：
1, to analyze pure barium peroxide as igniting agent, inner wall be coated with electric-melting magnesium chamotte with drilling lid (density in hole is 15/
m2；A diameter of 1.5cm in the hole) graphite crucible in carry out thermite reaction, the first batch of material (90kg vanadic anhydrides
+ 50.13kg aluminium), after the completion of thermit reaction, the second batch of material (10kg vanadic anhydride+5.57kg aluminium) is added, after the completion of reaction,
30min is stood, the separation of slag gold obtains 62.3kg vananum products, wherein 90.06wt% containing V, Al 9.63wt%, Fe
0.10wt%, Si0.16wt%.
Embodiment 2
Take 200kg vanadic anhydrides, 127.4kg aluminum shots are raw material, and the weight proportion of vanadic anhydride and aluminum shot is 1.58：
1, to analyze pure barium peroxide as igniting agent, inner wall be coated with electric-melting magnesium chamotte with drilling lid (density in hole is 16/
m2；A diameter of 1.7cm in the hole) graphite crucible in carry out thermite reaction, (the oxidations of 140kg five two of the first batch of material
Vanadium+89.18kg aluminium), after the completion of thermit reaction, the second batch of material (40kg vanadic anhydride+25.48kg aluminium), thermit reaction is added
After the completion, third batch of material (20kg vanadic anhydride+12.74kg aluminium) is added, after the completion of reaction, stands 30min, slag gold detaches,
133.52kg vananum products are obtained, wherein 85.04wt% containing V, Al 14.6wt%, Fe 0.09wt%, Si
0.13wt%.
Embodiment 3
Take 300kg vanadic anhydrides, 250.2kg aluminum shots are raw material, and the weight proportion of vanadic anhydride and aluminum shot is 1.15：
1, to analyze pure barium peroxide as igniting agent, the density with drilling lid aperture that electric-melting magnesium chamotte is coated in inner wall is 17/
m2；A diameter of 1.8cm in the hole) graphite crucible in carry out thermite reaction, (the oxidations of 180kg five two of the first batch of material
Vanadium+150.12kg aluminium), after the completion of thermit reaction, the second batch of material (90kg vanadic anhydride+75.06kg aluminium), thermit reaction is added
After the completion, third batch of material (30kg vanadic anhydride+25.02kg aluminium) is added, after the completion of reaction, stands 30min, slag gold detaches,
269.4kg vananum products are obtained, wherein 65.9wt% containing V, Al 33.8wt%, Fe 0.1wt%, Si 0.13wt%.
Embodiment 4
Take 2000kg vanadic anhydrides, 1280kg aluminum shots are raw material, and the weight proportion of vanadic anhydride and aluminum shot is 1.56：
1, to analyze pure barium peroxide as igniting agent, inner wall be coated with electric-melting magnesium chamotte with drilling lid (density in hole is 20/
m2；A diameter of 2cm in the hole) graphite crucible in carry out thermite reaction, the first batch of material (1000kg vanadic anhydrides
+ 640kg aluminium), after the completion of thermit reaction, the second batch of material (600kg vanadic anhydride+384kg aluminium) is added, thermit reaction is completed
Afterwards, third batch of material (200kg vanadic anhydride+128kg aluminium) is added, the 4th batch of material (200kg vanadic anhydrides+128kg is added
Aluminium), after the completion of reaction, 30min is stood, the separation of slag gold obtains 1260kg vananum products, wherein 85.14wt% containing V, Al
13.9wt%, Fe 0.09wt%, Si 0.18wt%.
By Examples 1 to 4 it is found that V content 65.9wt%~90.06wt% of the obtained vananum product of the present invention,
Fe≤0.15wt%, Si≤0.19wt% meet the requirement that finishing operations continue processing.
Claims (10)
1. the production method of vananum, it is characterised in that：Include the following steps：
First batch of vanadic anhydride and aluminium are added into the graphite crucible with drilling lid, igniting carries out thermite reaction, instead
Should completely after, sequentially add subsequent batches vanadic anhydride and aluminium, carry out thermite reaction respectively, until vanadic anhydride and
Aluminium is all added and the reaction was complete, and the separation of slag gold obtains vananum.
2. the production method of vananum according to claim 1, it is characterised in that：The vanadic anhydride and aluminium it is total
Mass ratio is 1.15~1.8：1；Total addition of the vanadic anhydride is no more than 2000kg.
3. the production method of vananum according to claim 1 or 2, it is characterised in that：Vanadic anhydride and aluminium is added
Batch be 2~4 batches.
4. the production method of vananum according to claim 3, it is characterised in that：The gross mass of vanadic anhydride with
The gross mass of 100% meter, aluminium is 100% meter：
When the batch that vanadic anhydride and aluminium is added is 2 batches, first vanadic anhydride being added and the five of second batch addition
The mass percent of V 2 O is 90%~60%：10%~40%；The aluminium that first aluminium being added is added with second batch
Mass ratio is 90%~60%：10%~40%；
When the batch that vanadic anhydride and aluminium is added is 3 batches, vanadic anhydride of first addition, five oxygen of second batch addition
The mass ratio for changing the vanadic anhydride that two vanadium are added with third batch is 70%~60%：20%~30%：10%；First is added
Aluminium, the mass ratio of aluminium and third batch aluminium being added that is added of second batch be 70%~60%：20%~30%：10%；
When the batch that vanadic anhydride and aluminium is added is 4 batches, vanadic anhydride of first addition, five oxygen of second batch addition
The mass ratio for changing two vanadium, third batch vanadic anhydride being added and the vanadic anhydride of the 4th batch of addition is 50%：30%：
10%：10%；The quality of the aluminium of aluminium, the aluminium that third batch is added and the 4th batch of addition that first aluminium being added is added with second batch
Than being 50%：30%：10%：10%.
5. the production method of vananum according to claim 1, it is characterised in that：The purity of the vanadic anhydride
>=99.7%；Purity >=99.85% of the aluminium；The granularity of the aluminium is 1~10mm.
6. the production method of vananum according to claim 1, it is characterised in that：The density in the hole of the drilling lid
For 15~20/m2；A diameter of 1~2cm in the hole.
7. the production method of vananum according to claim 1, it is characterised in that：The inner wall of the graphite crucible is coated with
Electric-melting magnesium chamotte.
8. the production method of vananum according to claim 1, it is characterised in that：The criterion that the reaction was complete
There is no apparent flare at graphite cap bore.
9. the production method of vananum according to claim 1, it is characterised in that：Vanadic anhydride and aluminium are all added
And after the reaction was complete, stand and be no less than 30min, then the separation of slag gold.
10. the vananum that the production method of claim 1~9 any one of them vananum is prepared, feature exist
In：The chemical composition of the vananum is：V65.9wt%~90.13wt%, Al33.72wt%~9.49wt%, Fe≤
0.10wt%, Si≤0.18wt%.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113957274A (en) * | 2021-09-24 | 2022-01-21 | 攀钢集团攀枝花钢铁研究院有限公司 | Vanadium-aluminum alloy and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102925722A (en) * | 2012-09-24 | 2013-02-13 | 河北钢铁股份有限公司承德分公司 | Method for smelting vanadium-aluminum alloy by electro-aluminothermic process |
| CN104611601A (en) * | 2015-02-12 | 2015-05-13 | 攀钢集团攀枝花钢铁研究院有限公司 | Vanadium-aluminum alloy and preparation method thereof |
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2018
- 2018-03-20 CN CN201810228430.7A patent/CN108330370A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102925722A (en) * | 2012-09-24 | 2013-02-13 | 河北钢铁股份有限公司承德分公司 | Method for smelting vanadium-aluminum alloy by electro-aluminothermic process |
| CN104611601A (en) * | 2015-02-12 | 2015-05-13 | 攀钢集团攀枝花钢铁研究院有限公司 | Vanadium-aluminum alloy and preparation method thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113957274A (en) * | 2021-09-24 | 2022-01-21 | 攀钢集团攀枝花钢铁研究院有限公司 | Vanadium-aluminum alloy and preparation method thereof |
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