CN102146524A - Method for preparing metal vanadium by smelting Panxi ore raw material - Google Patents
Method for preparing metal vanadium by smelting Panxi ore raw material Download PDFInfo
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Abstract
The invention relates to a method for preparing metal vanadium by smelting, in particular relates to a method for preparing metal vanadium by smelting a Panxi ore raw material. The method comprises the following steps: feeding aluminium metallicum, an auxiliary reducing agent, a calcium metallurgy auxiliary material, an inert material and a calcium-sodium processing agent in a mixing device for fully stirring until the materials are evenly mixed; after even mixing, putting the mixture in a reaction device which is preheated to 200 DEG C-300 DEG C, and igniting; after the reaction is finished, adding 30-50kg of retarder and cooling for 48-72 hours; and finally, separating vanadium from smelting slag. The method has the advantages that the sources of raw materials are defined, the produced vanadium is high in grade, the content of the produced vanadium can reach 92%-95%, and the contents of impurities are low, thus effectively reducing the harm generated by impurities which are brought possibly on steel balls and having a promotion sense on steel production alloying. By directly producing vanadium, the production processes that aluminium-vanadium alloy is generated by aluminothermic reduction, and then aluminium is removed in vacuum are changed, thereby avoiding the use of vacuum equipment to remove the aluminium, reducing production requirement and saving cost.
Description
Technical field
The present invention relates to a kind of vanadium metal the smelting and preparation method, particularly, the present invention relates to a kind of to climb the method for western vanadium raw materials smelting and preparing vanadium metal.
Background technology
Vanadium is a kind of silver-gray metal, now is silver gray metalluster and dendroid and the crystallization of sponge shape outward, and product must not have macroscopic inclusion.The fusing point of vanadium is 1890 ℃, and good solidity to corrosion, ductility and forging property are arranged.And have good corrosion resistance, the vitriolic resistance to corrosion is better than stainless steel and titanium.This is functional and be easy to machining deformation.Vanadium can be used for founding and becomes ingot to make pure vanadium section bar.Can synthesize vanadium-containing alloy with other element,, can make high speed nuclear breeder, nuclear fuel jacket, be used to make superconductor, the filament material of making valve tube and getter material etc. as the interpolation element of titanium base alloy and the interpolation element of high strength heat resistant special alloy.Be mainly used in alloying steel and non-ferrous metal alloy, also be used for making cathode for electron tube, grid, ray target and the getter of electronic industry, the fluor of electrode tube etc.
Vanadium still is a kind ofly to improve steel hardness, prevent the metal that it gets rusty.The vanadium steel alloy can be used for making tub, high-speed tool, superconducting magnet, aircraft engine etc.Vanadium metal is used as the protective material of atomic reactor, make the switching housing and the covering of rocket, guided missile, spaceship at aerospace and aircraft industry, the structured material of air dreadnought, shuttle, make the navigation parts of aircraft arrestment energy absorber and aircraft, airship, guided missile, the additive of the high energy fuels of rocket, guided missile, jet airplane.Be the additive of steel alloy in metallurgical industry, also be used to make refractory materials and special glass, unicircuit, antenna etc.Vanadium metal is much accounted of as a kind of brand-new material benefit, and its heat absorption capacity is strong, and stable mechanical performance is an indispensable valuable materials in nuclear power, rocket, guided missile, aviation, space travel and the metallurgical industry.
The metal current vanadium is produced (Preparation Of Vanaciilam Metal) and is adopted metal or carbon that barium oxide is reduced into the process of vanadium metal, is the important component part of vanadium metallurgical process.Mainly contain calciothermic reduction, vacuum carbothermal reduction, muriate magnesiothermic reduction and four kinds of methods of thermite reduction at present.Adopt thermit reduction to produce the crude metal vanadium as Germany.This method is Vanadium Pentoxide in FLAKES and fine aluminium to be placed on Reaktionsofen react, and generates vananum.Vananum is dealuminzation in the high temperature of 2063K and vacuum, can make the crude metal vanadium that contains vanadium 94%～97%.But the impure height of the vanadium raw materials of certain areas v-bearing titanomagnetite smelting, vanadium raw materials as the v-bearing titanomagnetite smelting of Panxi Diqu, using above-mentioned thermit reduction to produce vanadium metal has difficulties, above-mentioned thermit reduction is to generate earlier aluminum-vanadium alloy, carry out the vacuum dealuminzation again, but the vacuum dealuminzation is higher to equipment requirements, if adopt this method then cost can improve greatly.
Summary of the invention
At having the problems referred to above that the impure high v-bearing titanomagnetite smelting vanadium metal of raw material has difficulties now, now provide a kind of to climb the method for western vanadium raw materials smelting and preparing vanadium metal, the raw material sources of this method are determined, production technique is safe and reliable, vanadium is of high grade, and foreign matter content is low, forms stay-in-grade vanadium metal product, reduced production cost, and effectively reduced and to bring the harm that impurity produces steel grade into.
For achieving the above object, the present invention adopt with technical scheme as follows:
A kind of to climb the method for western vanadium raw materials smelting and preparing vanadium metal, it is characterized in that subsidiary material according to following processing step following weight proportion of adding in the rich vanadium raw materials of 100kg Panxi Diqu:
Metallic aluminium 40kg ~ 50kg, assistant reducing agent 0.5kg ~ 1.0kg, calcareous metallurgic auxiliary materials 1kg ~ 1.5kg, inert material 18kg ~ 22kg, calcium-sodium are treatment agent 0.5kg ~ 2.0kg;
Described rich vanadium raw materials main component is a Vanadium Pentoxide in FLAKES;
Described assistant reducing agent is a silicocalcium;
Described calcareous metallurgic auxiliary materials is calcium oxide and Calcium Fluoride (Fluorspan);
Described inert material is metallurgical slag, lime or refrigerant;
Described calcium-sodium is that treatment agent is the mixture of yellow soda ash, calcium oxide and Calcium Fluoride (Fluorspan);
Concrete processing step is as follows:
Take by weighing raw material and various subsidiary material by above-mentioned weight proportion, above-mentioned all material is sent into mixing equipment to be stirred well to evenly, put into reaction unit after mixing through being preheated to 200 ℃ ~ 300 ℃, light a fire, reaction finishes the back and adds 30 ~ 50 kg retardant, cooling 48～72h separates metallurgical slag and vanadium at last, puts in storage after check, finishing, packing.
The mass percent of Vanadium Pentoxide in FLAKES is not less than 99% in the described rich vanadium raw materials.
Described silicocalcium is a powdery, and what wherein silicon and calcium total amount accounted for silicocalcium is not less than 50%, and silicon and calcium are arbitrary proportion.
In the described calcareous metallurgic auxiliary materials Calcium Fluoride (Fluorspan) add-on be not higher than calcareous metallurgic auxiliary materials amount 10%, all the other are calcium oxide.
Calcium oxide content is not less than 85% in described metallurgical slag or the lime.
Described calcium-sodium be the amount of yellow soda ash in the treatment agent not to be higher than calcium-sodium be 3% of treatment agent, it is 5% of treatment agent that the amount of Calcium Fluoride (Fluorspan) is not higher than calcium-sodium, all the other are calcium oxide.
Described retardant is a lime, and the mass percent of calcium oxide is not less than 80% in the lime.
As follows to chemical principle of the present invention and process explanation below:
The present invention is with aluminium matter reductive agent (main composition Al), metallurgic auxiliary materials (main composition CaO), vanadium raw materials (main composition V
2O
5), inert material etc. is raw material, by reasonably combined raw material and heat, issues the cast alumin(i)um thermal reduction reaction in optimal temperature, aluminium matter reductive agent is with the V in the vanadium raw materials
2O
5Reduction produces vanadium metal, aluminum oxide, unreacted V that reaction generates
2O
5, form slag mutually with CaO, alloy phase is cooled off by slag phase covering protection, condensation process finishes the back and separates alloy product.
The raw material that the smelting process of vanadium metal is used is mainly by CaO, V
2O
5With compositions such as Al, under the condition that satisfies associated hot balance and material balance, different oxide compound constituent elements in the raw material and aluminium generation reduction reaction, main chemical equation is as follows, should be to change order to carry out mutually according to free energy and activity, reaction finishes the back at vanadium V and CaO-V
2O
5-Al
2O
3Form balance between slag system, obtain vanadium product and alloy slag after the refrigerated separation.Temperature decision speed of response, impurity such as Si, S and P distribute according to activity quotient, temperature and equilibrium constant step between slag and alloy.
3V
2O
5?+?10Al?→6V?+?5Al
2O
3 （1）
The vanadium iron smelting process has a large amount of Al
2O
3Produce Al
2O
3With CaO in conjunction with forming CaOAl
2O
3, CaO had both adjusted the ph balancing of slag, and the Sulfur capacity and the phosphorus that increase slag simultaneously hold, and improve sulphur phosphorus and remove ability.The CaO add-on is higher than calculated value, influences slag melting, is unfavorable for the mass transfer of P and S, and portion C aO raw material also can be brought a small amount of P and S into, and utilization sodium calcium based material comprehensively removes the sulphur phosphorus impurities in the test.
The invention has the advantages that:
1, raw material sources of the present invention are determined, the vanadium metal of production is of high grade, can reach 92% ~ 95%, and foreign matter content is low, effectively reduce may bring impurity into to the harm that steel grade produces, and the Iron and Steel Production alloying is had positive promotion meaning.
2, direct production vanadium has changed existing thermite reduction and has generated aluminum-vanadium alloy earlier, carries out the production process of vacuum dealuminzation again, avoids using the vacuum apparatus dealuminzation, has reduced production requirement, has saved cost.
3, solve the raw material impurity problem, improved the rate of recovery.
Embodiment
Embodiment 1
A kind of to climb the method for western vanadium raw materials smelting and preparing vanadium metal, in the rich vanadium raw materials of 100kg Panxi Diqu, add the subsidiary material of following weight proportion according to following processing step:
Metallic aluminium 40kg, assistant reducing agent 1.0kg, calcareous metallurgic auxiliary materials 1kg, inert material 22kg, calcium-sodium are treatment agent 0.5kg;
Rich vanadium raw materials main component is a Vanadium Pentoxide in FLAKES, and the mass percent of Vanadium Pentoxide in FLAKES is 99%.
Assistant reducing agent is a silicocalcium, and silicocalcium is a powdery, and what wherein silicon and calcium total amount accounted for silicocalcium is 50%, and silicon and calcium are 1 to 1.
Calcareous metallurgic auxiliary materials is calcium oxide and Calcium Fluoride (Fluorspan), the Calcium Fluoride (Fluorspan) add-on be calcareous metallurgic auxiliary materials amount 10%, all the other are calcium oxide.
Inert material is a metallurgical slag, and calcium oxide content is 85% in the metallurgical slag.
Calcium-sodium is that treatment agent is the mixture of yellow soda ash, calcium oxide and Calcium Fluoride (Fluorspan), and the amount of yellow soda ash is that calcium-sodium is 3% of treatment agent, and the amount of Calcium Fluoride (Fluorspan) is that calcium-sodium is 5% of treatment agent, and all the other are calcium oxide.
Retardant is a lime, and the mass percent of calcium oxide is 80% in the lime.
Concrete processing step is as follows:
Take by weighing raw material and various subsidiary material by above-mentioned weight proportion, above-mentioned all material is sent into mixing equipment to be stirred well to evenly, put into reaction unit after mixing through being preheated to 300 ℃, light a fire, reaction finishes the back and adds the 30kg retardant, cooling 72h separates metallurgical slag and vanadium at last, puts in storage after check, finishing, packing.The crude metal vanadium that can contain vanadium 92% at last.
Embodiment 2
A kind of to climb the method for western vanadium raw materials smelting and preparing vanadium metal, in the rich vanadium raw materials of 100kg Panxi Diqu, add the subsidiary material of following weight proportion according to following processing step:
Metallic aluminium 50kg, assistant reducing agent 0.5kgkg, calcareous metallurgic auxiliary materials 1.5kg, inert material 18kg, calcium-sodium are treatment agent 2.0kg;
Rich vanadium raw materials main component is a Vanadium Pentoxide in FLAKES, and the mass percent of Vanadium Pentoxide in FLAKES is 99.5%.
Assistant reducing agent is a silicocalcium, and silicocalcium is granular, and what wherein silicon and calcium total amount accounted for silicocalcium is 60%, and silicon and calcium are 2 to 1.
Calcareous metallurgic auxiliary materials is calcium oxide and Calcium Fluoride (Fluorspan), the Calcium Fluoride (Fluorspan) add-on be calcareous metallurgic auxiliary materials amount 8%, all the other are calcium oxide.
Inert material is a lime, and calcium oxide content is 90% in the lime.
Calcium-sodium is that treatment agent is the mixture of yellow soda ash, calcium oxide and Calcium Fluoride (Fluorspan), and the amount of yellow soda ash is that calcium-sodium is 2% of treatment agent, and the amount of Calcium Fluoride (Fluorspan) is that calcium-sodium is 4% of treatment agent, and all the other are calcium oxide.
Retardant is a lime, and the mass percent of calcium oxide is 90% in the lime.
Concrete processing step is as follows:
Take by weighing raw material and various subsidiary material by above-mentioned weight proportion, above-mentioned all material is sent into mixing equipment to be stirred well to evenly, put into reaction unit after mixing through being preheated to 200 ℃, light a fire, reaction finishes the back and adds 50 kg retardant, cooling 48h separates metallurgical slag and vanadium at last, puts in storage after check, finishing, packing.
Embodiment 3
A kind of to climb the method for western vanadium raw materials smelting and preparing vanadium metal, in the rich vanadium raw materials of 100kg Panxi Diqu, add the subsidiary material of following weight proportion according to following processing step:
Metallic aluminium 45kg, assistant reducing agent 0.7kg, calcareous metallurgic auxiliary materials 1.3kg, inert material 20kg, calcium-sodium are treatment agent 1.5kg;
Rich vanadium raw materials main component is a Vanadium Pentoxide in FLAKES, and the mass percent of Vanadium Pentoxide in FLAKES is 99%.
Assistant reducing agent is a silicocalcium, and silicocalcium is a powdery, and what wherein silicon and calcium total amount accounted for silicocalcium is 70%, and silicon and calcium are 1 to 2.
Calcareous metallurgic auxiliary materials is calcium oxide and Calcium Fluoride (Fluorspan), the Calcium Fluoride (Fluorspan) add-on be calcareous metallurgic auxiliary materials amount 7%, all the other are calcium oxide.
Inert material is a refrigerant, and refrigerant is a refrigerant well known in the art.
Calcium-sodium is that treatment agent is the mixture of yellow soda ash, calcium oxide and Calcium Fluoride (Fluorspan), and the amount of yellow soda ash is that calcium-sodium is 2.5% of treatment agent, and it is 3.5% of treatment agent that the amount of Calcium Fluoride (Fluorspan) is not higher than calcium-sodium, and all the other are calcium oxide.
Retardant is a lime, and the mass percent of calcium oxide is 95% in the lime.
Concrete processing step is as follows:
Take by weighing raw material and various subsidiary material by above-mentioned weight proportion, above-mentioned all material is sent into mixing equipment to be stirred well to evenly, put into reaction unit after mixing through being preheated to 250 ℃, light a fire, reaction finishes the back and adds the 40kg retardant, cooling 60h separates metallurgical slag and vanadium at last, puts in storage after check, finishing, packing.
Embodiment 4
A kind of to climb the method for western vanadium raw materials smelting and preparing vanadium metal, in the rich vanadium raw materials of 100kg Panxi Diqu, add the subsidiary material of following weight proportion according to following processing step:
Metallic aluminium 42kg, assistant reducing agent 0.8kg, calcareous metallurgic auxiliary materials 1.1kg, inert material 21kg, calcium-sodium are treatment agent 1kg;
Rich vanadium raw materials main component is a Vanadium Pentoxide in FLAKES, and the mass percent of Vanadium Pentoxide in FLAKES is 99%.
Assistant reducing agent is a silicocalcium, and silicocalcium is a powdery, and what wherein silicon and calcium total amount accounted for silicocalcium is 55%, and silicon and calcium are 3 to 1.
Calcareous metallurgic auxiliary materials is calcium oxide and Calcium Fluoride (Fluorspan), the Calcium Fluoride (Fluorspan) add-on be calcareous metallurgic auxiliary materials amount 3%, all the other are calcium oxide.
Inert material is a metallurgical slag, and calcium oxide content is 88% in the metallurgical slag.
Calcium-sodium is that treatment agent is the mixture of yellow soda ash, calcium oxide and Calcium Fluoride (Fluorspan), and the amount of yellow soda ash is that calcium-sodium is 1% of treatment agent, and the amount of Calcium Fluoride (Fluorspan) is that calcium-sodium is 2% of treatment agent, and all the other are calcium oxide.
Retardant is a lime, and the mass percent of calcium oxide is 92% in the lime.
Concrete processing step is as follows:
Take by weighing raw material and various subsidiary material by above-mentioned weight proportion, above-mentioned all material is sent into mixing equipment to be stirred well to evenly, put into reaction unit after mixing through being preheated to 220 ℃, light a fire, reaction finishes the back and adds the 45kg retardant, cooling 55h separates metallurgical slag and vanadium at last, puts in storage after check, finishing, packing.
Embodiment 5
A kind of to climb the method for western vanadium raw materials smelting and preparing vanadium metal, in the rich vanadium raw materials of 100kg Panxi Diqu, add the subsidiary material of following weight proportion according to following processing step:
Metallic aluminium 48kg, assistant reducing agent 0.6kg, calcareous metallurgic auxiliary materials 1.4kg, inert material 19kg, calcium-sodium are treatment agent 1.6kg;
Rich vanadium raw materials main component is a Vanadium Pentoxide in FLAKES, and the mass percent of Vanadium Pentoxide in FLAKES is 99.8%.
Assistant reducing agent is a silicocalcium, and silicocalcium is a powdery, and what wherein silicon and calcium total amount accounted for silicocalcium is 78%, and silicon and calcium are 3 to 1.
Calcareous metallurgic auxiliary materials is calcium oxide and Calcium Fluoride (Fluorspan), the Calcium Fluoride (Fluorspan) add-on be calcareous metallurgic auxiliary materials amount 7%, all the other are calcium oxide.
Inert material is a lime, and calcium oxide content is 96% in the lime.
Calcium-sodium is that treatment agent is the mixture of yellow soda ash, calcium oxide and Calcium Fluoride (Fluorspan), and the amount of yellow soda ash is that calcium-sodium is 2% of treatment agent, and the amount of Calcium Fluoride (Fluorspan) is that calcium-sodium is 4% of treatment agent, and all the other are calcium oxide.
Retardant is a lime, and the mass percent of calcium oxide is 96% in the lime.
Concrete processing step is as follows:
Take by weighing raw material and various subsidiary material by above-mentioned weight proportion, above-mentioned all material is sent into mixing equipment to be stirred well to evenly, put into reaction unit after mixing through being preheated to 280 ℃, light a fire, reaction finishes the back and adds 35 kg retardant, cooling 65h separates metallurgical slag and vanadium at last, puts in storage after check, finishing, packing.
The described rich vanadium raw materials of the application is for being rich in V
2O
5Vanadium raw materials, V wherein
2O
5Mass percentage content is to be formed by v-bearing titanomagnetite smelting more than or equal to 99%.Each related equipment of present method is existing installation.
Claims (7)
1. one kind to climb the method for western vanadium raw materials smelting and preparing vanadium metal, it is characterized in that adding in the rich vanadium raw materials of 100kg Panxi Diqu according to following processing step the subsidiary material of following weight proportion:
Metallic aluminium 40kg ~ 50kg, assistant reducing agent 0.5kg ~ 1.0kg, calcareous metallurgic auxiliary materials 1kg ~ 1.5kg, inert material 18kg ~ 22kg, calcium-sodium are treatment agent 0.5kg ~ 2.0kg;
Described rich vanadium raw materials main component is a Vanadium Pentoxide in FLAKES;
Described assistant reducing agent is a silicocalcium;
Described calcareous metallurgic auxiliary materials is calcium oxide and Calcium Fluoride (Fluorspan);
Described inert material is metallurgical slag, lime or refrigerant;
Described calcium-sodium is that treatment agent is the mixture of yellow soda ash, calcium oxide and Calcium Fluoride (Fluorspan);
Concrete processing step is as follows:
Take by weighing raw material and various subsidiary material by above-mentioned weight proportion, above-mentioned all material is sent into mixing equipment to be stirred well to evenly, put into reaction unit after mixing through being preheated to 200 ℃ ~ 300 ℃, light a fire, reaction finishes the back and adds 30 ~ 50 kg retardant, cooling 48～72h separates metallurgical slag and vanadium at last, puts in storage after check, finishing, packing.
2. according to claim 1 a kind of to climb the method for western vanadium raw materials smelting and preparing vanadium metal, it is characterized in that: the mass percent of Vanadium Pentoxide in FLAKES is not less than 99% in the described rich vanadium raw materials.
3. according to claim 1 a kind of to climb the method for western vanadium raw materials smelting and preparing vanadium metal, it is characterized in that: described silicocalcium is a powdery, and what wherein silicon and calcium total amount accounted for silicocalcium is not less than 50%, and silicon and calcium are arbitrary proportion.
4. according to claim 1 a kind of to climb the method for western vanadium raw materials smelting and preparing vanadium metal, it is characterized in that: in the described calcareous metallurgic auxiliary materials Calcium Fluoride (Fluorspan) add-on be not higher than calcareous metallurgic auxiliary materials amount 10%, all the other are calcium oxide.
5. according to claim 1 a kind of to climb the method for western vanadium raw materials smelting and preparing vanadium metal, it is characterized in that: in the described inert material in metallurgical slag or the lime calcium oxide content be not less than 85%.
6. according to claim 1 a kind of to climb the method for western vanadium raw materials smelting and preparing vanadium metal, it is characterized in that: described calcium-sodium is that not to be higher than calcium-sodium be 3% of treatment agent to the amount of yellow soda ash in the treatment agent, it is 5% of treatment agent that the amount of Calcium Fluoride (Fluorspan) is not higher than calcium-sodium, and all the other are calcium oxide.
7. according to claim 1 a kind of it is characterized in that: described retardant is a lime to climb the method for western vanadium raw materials smelting and preparing vanadium metal, and the mass percent of calcium oxide is not less than 80% in the lime.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102534271A (en) * | 2012-02-21 | 2012-07-04 | 四川省达州钢铁集团有限责任公司 | Production method of vanadium-aluminum alloy |
| CN106541335A (en) * | 2016-10-08 | 2017-03-29 | 河钢股份有限公司承德分公司 | The method for removing the oxide-film and alloy slag inclusion on vananum surface |
| CN110699561A (en) * | 2019-11-12 | 2020-01-17 | 四川大学 | Method for producing high-purity metal vanadium by adopting directional solidification |
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| WO2004055225A1 (en) * | 2002-12-17 | 2004-07-01 | Council Of Scientific And Industrial Research | A process for extraction of nickel from low grade chromite ore |
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| US5935866A (en) * | 1989-12-22 | 1999-08-10 | Binax Nh, Inc. | Preparation of sub 100 A magnetic particles and magnetic molecular switches |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102534271A (en) * | 2012-02-21 | 2012-07-04 | 四川省达州钢铁集团有限责任公司 | Production method of vanadium-aluminum alloy |
| CN102534271B (en) * | 2012-02-21 | 2013-09-25 | 四川省达州钢铁集团有限责任公司 | Production method of vanadium-aluminum alloy |
| CN106541335A (en) * | 2016-10-08 | 2017-03-29 | 河钢股份有限公司承德分公司 | The method for removing the oxide-film and alloy slag inclusion on vananum surface |
| CN110699561A (en) * | 2019-11-12 | 2020-01-17 | 四川大学 | Method for producing high-purity metal vanadium by adopting directional solidification |
| CN110699561B (en) * | 2019-11-12 | 2020-12-25 | 四川大学 | Method for producing high-purity metal vanadium by adopting directional solidification |
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|---|---|
| CN102146524B (en) | 2012-07-04 |
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Denomination of invention: Method for preparing metal vanadium by smelting Panxi ore raw material Effective date of registration: 20170224 Granted publication date: 20120704 Pledgee: Panzhihua commercial bank Limited by Share Ltd Commercial Street Branch Pledgor: Panzhihua Yinjiang Jinyong Industry and Trade Co., Ltd. Registration number: 2017510000012 |
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