CN104561526A - High-all-vanadium sodium modification roasting method - Google Patents
High-all-vanadium sodium modification roasting method Download PDFInfo
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- CN104561526A CN104561526A CN201510047857.3A CN201510047857A CN104561526A CN 104561526 A CN104561526 A CN 104561526A CN 201510047857 A CN201510047857 A CN 201510047857A CN 104561526 A CN104561526 A CN 104561526A
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- vanadium
- slag
- sodium
- tailings
- roasting method
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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
- C22B1/00—Preliminary treatment of ores or scrap
- C22B1/02—Roasting processes
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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
Abstract
The invention belongs to the field of vanadium extraction, and particularly relates to a high-all-vanadium sodium modification roasting method. The invention aims to provide a high-all-vanadium sodium modification roasting method which comprises the following steps: a. pretreatment: passing vanadium slag through a 120-mesh screen until the amount of the undersize is not less than 80%, and removing iron until the metallic iron content is less than or equal to 5% to obtain fine slag; b. proportioning: regulating the fine slag with tailings until all vanadium accounts for 6.5-7.0% of the total weight of the fine slag and tailings and the sodium salt is 1.5-1.7 times by weight of the vanadium pentoxide in the fine slag and tailings, and evenly mixing to obtain a mixture; and c. roasting: heating the mixture from 300 DEG C to 550-600 DEG C within 2-2.5 hours, heating to 750-800 DEG C within 2-3 hours, heating to 850 DEG C within 1-2 hours, cooling to not lower than 550 DEG C, and discharging. The method can be used for sodium modification roasting for recovering vanadium from vanadium slag with higher vanadium content.
Description
Technical field
The invention belongs to vanadium extractive technique field, be specifically related to a kind of sodium roasting method of high full vanadium.
Background technology
In water law process for extracting vanadium, the oxidation-sodium roasting of vanadium slag joins in rotary kiln or multiple hearth furnace by through pretreated vanadium slag, heat under oxidizing atmosphere, react with sodium salt after making it oxidation again and generate water-soluble vanadic acid sodium, in water, the height direct relation of the concentration of vanadic acid sodium the transformation efficiency of grog and total recovery rate of vanadium.
In the industrial production of reality, improve full vanadium in grog and can increase the production capacity of operation significantly, but the too high oxygen-consumption that can increase in oxidising process of full vanadium in grog, simultaneously at soda than under certain condition, the vanadic acid sodium generated in the sodium salt amount that the vanadium slag higher to content of vanadium is allocated into and furnace charge is more, causes the product of low melting point to increase, will cause the bonding of furnace charge, production can not normally be carried out, and therefore the full vanadium in grog controls below 6.5% by most domestic vanadium extraction producer.
The inventive method will overcome the charging binding problem that in the high full vanadium oxidising process of grog, oxygen-consumption and low melting point product cause.By conservative control exhausting, sodium temperature, sodium time, control the measures such as material composition, a difficult problem for the charging binding successfully solving oxygen-consumption in oxidising process and cause because of low melting point, in actual production process, the full vanadium of grog can reach 6.5 ~ 7.0%, transformation efficiency more than 84%, achieves good economic benefit.
Summary of the invention
For above-mentioned deficiency, the present invention, in order to overcome full content of vanadium in sodium roasting gained grog higher than the problem easily causing grog to bond after 6.5%, the invention provides a kind of sodium roasting method of high full vanadium.The method comprises the following steps:
A, pre-treatment: vanadium slag is pulverized, the screen underflow crossing 120 mesh sieves is not less than 80%, then deironing is to metallic iron≤5%, obtains smart slag;
B, batching: take raw material according to following weight relationships, tailings regulates smart slag to account for 6.5 ~ 7.0% of smart slag and tailings gross weight to full vanadium, and sodium salt is 1.5 ~ 1.7 times of Vanadium Pentoxide in FLAKES weight in smart slag and tailings, and tailings, smart slag, sodium salt mix to obtain compound;
C, roasting: compound is warming up to 550 ~ 600 DEG C from 300 DEG C in 2 ~ 2.5h, then in 2 ~ 3h, be warming up to 750 ~ 800 DEG C, then in 1 ~ 2h, be warming up to 850 DEG C, then be cooled to and be not less than 550 DEG C, get final product discharging.
Concrete, the sodium roasting method of the full vanadium of above-mentioned height, in step a, to vanadium-bearing hot metal, to be vanadium extraction by converter blowing method carry out that semisteel smelting extracts to described vanadium slag is rich in vanadium converter slag.
Concrete, the sodium roasting method of the full vanadium of above-mentioned height, in step a, the main component of described vanadium slag is SiO
215 ~ 20%, CaO2.0 ~ 5.0%, V
2o
512 ~ 17%, MFe10 ~ 18%.
Preferably, the sodium roasting method of the full vanadium of above-mentioned height, in step a, by weight, the V in described vanadium slag
2o
5/ CaO is more than 4.5.
Preferably, the sodium roasting method of the full vanadium of above-mentioned height, in step a, the SiO in described vanadium slag
2≤ 12%.
Preferably, the sodium roasting method of the full vanadium of above-mentioned height, in step a, described tailings is that vanadium slag is by sodium roasting and the slag obtained after carrying out water logging.
Concrete, the sodium roasting method of the full vanadium of above-mentioned height, in step b, described sodium salt is at least one of soda ash or sodium-chlor.
Further, the sodium roasting method of the full vanadium of above-mentioned height, in step b, described sodium salt is the mixture of soda ash and sodium-chlor, and soda ash accounts for 80 ~ 85% of sodium salt gross weight.
Concrete, the sodium roasting method of the full vanadium of above-mentioned height, in step c, controls oxygen level in tail gas and is not less than 8%.
In sodium roasting method of the present invention, in order to can solve content of vanadium 6.5 ~ 7.0% compound in roasting process grog bonding problem, contriver controls rational proportioning raw materials, when carrying out roasting, control the maturing temperature of rational zone of oxidation and roasting time by fully oxidized for the materials such as metallic iron, at a low price ferric oxide, thus reach the fully oxidized of Low Valent Vanadium further, improve the transformation efficiency of full vanadium; At the rational drop temperature of control, thus ensure that the transformation efficiency of full vanadium.In the inventive method, each proportioning raw materials and maturing temperature, time complement each other, thus obtain the good technique effect of transformation efficiency more than 84%, and, in roasting process, there is not the situation of ring formation of rotary kiln, the rate of recovery promoting operation production capacity and vanadium is had great importance.
Embodiment
A sodium roasting method for high full vanadium, comprises the following steps:
A, pre-treatment: vanadium slag is pulverized, the screen underflow crossing 120 mesh sieves is not less than 80%, then deironing is to metallic iron≤5%, obtains smart slag;
B, batching: take raw material according to following weight ratio, tailings regulates smart slag to account for 6.5 ~ 7.0% of smart slag and tailings gross weight to full vanadium, and sodium salt is 1.5 ~ 1.7 times of Vanadium Pentoxide in FLAKES weight in smart slag and tailings, and tailings, smart slag, sodium salt mix to obtain compound;
C, roasting: compound is warming up to 550 ~ 600 DEG C from 300 DEG C in 2 ~ 2.5h, then in 2 ~ 3h, be warming up to 750 ~ 800 DEG C from this temperature, then in 1 ~ 2h, be warming up to 850 DEG C from this temperature, then be cooled to and be not less than 550 DEG C, get final product discharging.
Concrete, the sodium roasting method of the full vanadium of above-mentioned height, in step a, to vanadium-bearing hot metal, to be vanadium extraction by converter blowing method carry out that semisteel smelting extracts to described vanadium slag is rich in vanadium converter slag.
Concrete, the sodium roasting method of the full vanadium of above-mentioned height, in step a, the main component of described vanadium slag is SiO
215 ~ 20%, CaO2.0 ~ 5.0%, V
2o
512 ~ 17%, MFe10 ~ 18%.
Preferably, the sodium roasting method of the full vanadium of above-mentioned height, in step a, by weight, the V in described vanadium slag
2o
5/ CaO is more than 4.5.
Preferably, the sodium roasting method of the full vanadium of above-mentioned height, in step a, the SiO in described vanadium slag
2≤ 12%.
Preferably, the sodium roasting method of the full vanadium of above-mentioned height, in step a, described tailings is that vanadium slag is by sodium roasting and the slag obtained after carrying out water logging.
Preferably, the sodium roasting method of the full vanadium of above-mentioned height, in step b, described sodium salt is at least one of soda ash or sodium-chlor.
Further, the sodium roasting method of the full vanadium of above-mentioned height, in step b, in order to the vanadic acid sodium produced after ensureing roasting is soluble in water, tailings filters faster, should add a small amount of sodium-chlor, so described sodium salt is the mixture of soda ash and sodium-chlor, and soda ash accounts for 80 ~ 85% of sodium salt gross weight.
Concrete, the sodium roasting method of the full vanadium of above-mentioned height, in step c, controls oxygen level in tail gas and is not less than 8%.
In the inventive method step b, full vanadium is scaled Vanadium Pentoxide in FLAKES and calculates by the weight of described Vanadium Pentoxide in FLAKES completely, and not merely calculates only with the part that Vanadium Pentoxide in FLAKES form exists.
Find through contriver: the temperature of vanadium slag roasting in stove, is actually continuously from low temperature to high temperature, then the process gradually changed from high temperature to low temperature.The reactions change process in stove according to vanadium slag and sodium salt, is divided into three bands: zone of oxidation, sodium band and cooling zone usually by stove:
(1) zone of oxidation: mainly vanadium slag dehydration and metallic iron, suboxide (FeO, V
2o
3deng) oxidation and decompose stage, be generally from vanadium slag enters in stove, to the stage that about 600 DEG C complete, principal reaction equation is as follows:
At about 300 DEG C metallic iron oxidation: Fe+1/2O
2→ FeO 2FeO+1/2O
2→ Fe
2o
3
At 500 ~ 600 DEG C, Binder Phase fayalite is oxidized and decomposes:
2FeOSiO
2+ 1/2O
2→ Fe
2o
3siO
2(suboxide oxidation)
Fe
2o
3siO
2→ Fe
2o
3+ SiO
2(composite oxides decomposition)
At 600 ~ 700 DEG C, spinel oxygenolysis: Fe
2o
3v
2o
5→ Fe
2o
3+ V
2o
5(decomposition)
(2) sodium band: the stage the highest to maturing temperature from 600 DEG C, the top temperature of roasting controls at about 800 DEG C to multiple hearth furnace, can suitably improve rotary kiln, this will determine according to the situation of furnace charge, temperature is too high easily causes load melting balling, affect normal running, principal reaction equation is as follows:
At 600 ~ 700 DEG C, Vanadium Pentoxide in FLAKES and sodium salt react and generate water-soluble vanadic acid sodium:
V
2O
5+Na
2CO
3→NaVO
3V
2O
5+Na
2CO
3→2NaVO
3+1/2O
2↑
(3) cooling zone: be reduced to about 600 DEG C these one-phases from roasting top temperature, is that is cooled to about 600 DEG C will come out of the stove, and controls at 700 DEG C to multiple hearth furnace orlop temperature, cooling of then coming out of the stove.To rotary kiln come out of the stove grog tapping temperature require more than 550 DEG C, cooling of then coming out of the stove.
Through contriver study find roasting terminate after grog tapping temperature be one of key condition ensureing vanadium transformation efficiency.After roasting, grog wants chilling after coming out of the stove, otherwise vanadium transformation efficiency will reduce, and when its major cause is Slow cooling, the solubility sodium metavanadate making to have generated deoxidation when crystallization is become water-fast vanadium bronze.Therefore, requirement must the temperature more than sodium metavanadate fusing point (about 550 DEG C) to be come out of the stove cooling, can reduce or avoid the generation of vanadium bronze, prevent transformation efficiency from reducing.
Roasting time can be divided into oxidization time and sodium time, oxidization time refers to the vanadium slag time of oxides required for high price state (zone of oxidation) at a middle or low price, and the sodium time refers to that Vanadium Pentoxide in FLAKES and sodium salt react and generates vanadic acid sodium (sodium band) institute elapsed time.
Find through contriver: according to the feature of vanadium slag composition, suboxide will be made in oxidization time to be oxidized, complete that the oxidation of metallic iron, at a low price ferric oxide are oxidized to high price, silicate decomposes, the process such as the oxidation of spinel and decomposition, after only having reaction above to complete, spinel could be oxidized Sum decomposition, in other words, only have iron etc. fully oxidized, just can carry out Low Valent Vanadium oxidation, iron is the reductive agent of pentavalent vanadium at a low price, and pentavalent vanadium is the oxygenant of iron at a low price.Therefore, must keep sufficient oxidization time that oxidizing reaction just can be made fully to carry out, and ensure higher vanadium transformation efficiency.According to the difference of the conditions such as vanadium slag composition, structure and granularity, general furnace charge is 2 ~ 2.5h in the time that zone of oxidation stops, and felicity condition exhausting can to ensure in tail gas that oxygen level is not less than 8% and can obtain good oxidation effectiveness simultaneously.
Certain vanadium slag is mainly containing following composition:
Table 1
| Project | V 2O 5 | SiO 2 | CaO | P | MFe | Cr 2O 3 | TiO 2 | MnO |
| Vanadium slag | 14.87 | 16.90 | 3.33 | 0.191 | 16.5 | 5.2 | 0.25 | 0.68 |
As can be seen from Table 1, the material in vanadium slag mainly contains V
2o
5, CaO, SiO
2, Cr
2o
3deng.
Discovery is studied: above-mentioned each material has different impacts to roasting conversion rate through contriver, wherein, V
2o
5" useful " composition with MnO, and CaO, SiO
2be " being harmful to " composition, find further, the objectionable constituent in vanadium slag to the relative ranks of the deleterious effect of roasting conversion rate are under same molar:
CaO＞＞SiO
2＞Cr
2O
3＞TiO
2
Further discovery, in vanadium slag, CaO on roasting conversion rate impact greatly, CaO and V in roasting process
2o
5the water-fast calcium vanadate CaOV of easy generation
2o
5or contain the vanadium bronze CaV of Ca
12o
30, the transformation efficiency of vanadium slag is sharply reduced, causes vanadium enter sediment and run off.Further find, in vanadium slag, CaO often increases by 1%, will make V
2o
5output reduces 8.03%.The disadvantageous effect of CaO is also relevant with the content of vanadium in vanadium slag, V
2o
5/ CaO ratio is higher, and CaO influence degree is less, otherwise CaO influence degree is larger, so, weight ratio V in preferred vanadium slag
2o
5the vanadium slag of/CaO more than 4.5 is raw material of the present invention.
On the other hand, contriver is found by research: silicate not only can hinder oxygen and sodium salt to inner transmission matter, and can under maturing temperature be greater than the condition of 750 DEG C, silicate and spinel, soda interact and generate glass silicon vanadic acid sodium, make vanadium with V
3+, V
4+, V
5+equivalent state enters glassy phase, forms insoluble vanadium compound, and the higher this effect of maturing temperature is just further obvious.SiO in vanadium slag is found through test
2content often increases by 1%, will make V
2o
5output reduces 1.48%, so, strictly must control SiO in vanadium slag
2content, so, SiO in preferred vanadium slag
2the vanadium slag of≤12% is raw material of the present invention.
In the inventive method, do not make specified otherwise, ratio, content, composition etc. all represent weight percent.
Embodiment 1
Vanadium slag is carried out fragmentation, deironing process, obtain smart slag, get 30 tons of smart slags, wherein full content of vanadium is 8.90%, and metal Ferrum content is 3.95%, crosses 120 order percent of pass and reaches 83%; Get 15 tons of tailings, wherein full content of vanadium is 1.70%; Above-mentioned smart slag and tailings are mixed in proportion, ensure that mixed full vanadium is 6.50%; Add soda ash 7.21 tons again, 1.80 tons, sodium-chlor, all raw materials are mixed in stirrer, compound is warming up to 595 DEG C from 300 DEG C in 2.3h, in 2.5h, be warming up to 780 DEG C from this temperature again, then in 1.6h, be warming up to 850 DEG C from this temperature, then be cooled to and be not less than 550 DEG C, get final product discharging, controlling oxygen level in rotary kiln tail gas during roasting is 12.5%.After baking end, carry out next step vanadium extraction by routine techniques.The vanadium transformation efficiency of the present embodiment is 85.13%, and in roasting process, balling, ring formation phenomenon do not appear in rotary kiln.
Embodiment 2
Vanadium slag is carried out fragmentation, deironing process, obtain smart slag, get 35 tons of smart slags, wherein full content of vanadium is 8.95%, and metal Ferrum content is 3.62%, crosses 120 order percent of pass and reaches 82.1%; Get 15 tons of tailings, wherein full content of vanadium is 1.78%; Above-mentioned smart slag and tailings are mixed in proportion, ensure that mixed full vanadium is 6.8%; Add soda ash 8.25 tons again, 2.07 tons, sodium-chlor, all raw materials are mixed in stirrer, under the condition of aerobic, compound is warming up to 590 DEG C from 300 DEG C in 2.2h, then in 2.3h, is warming up to 785 DEG C from this temperature, in 1.8h, 850 DEG C are warming up to again from this temperature, be cooled to and be not less than 550 DEG C, get final product discharging, controlling oxygen level in rotary kiln tail gas during roasting is 11.8%.After baking end, carry out next step vanadium extraction by routine techniques.The vanadium transformation efficiency of the present embodiment is 84.63%, and in roasting process, balling, ring formation phenomenon do not appear in rotary kiln.
Embodiment 3
Vanadium slag is carried out fragmentation, deironing process, obtain smart slag, get 45 tons of smart slags, wherein full content of vanadium is 8.75%, and metal Ferrum content is 3.65%, crosses 120 order percent of pass and reaches 83.5%; Get 15 tons of tailings, wherein full content of vanadium is 1.76%; Above-mentioned smart slag and tailings are mixed in proportion, ensure that mixed full vanadium is 7.0%; Add soda ash 10.20 tons again, 2.55 tons, sodium-chlor, all raw materials are mixed in stirrer, under the condition of aerobic, compound is warming up to 580 DEG C from 300 DEG C in 2.6h, then in 2.5h, is warming up to 795 DEG C from this temperature, in 1.6h, 850 DEG C are warming up to again from this temperature, be cooled to and be not less than 550 DEG C, get final product discharging, controlling oxygen level in rotary kiln tail gas during roasting is 12.8%.After baking end, carry out next step vanadium extraction by routine techniques.The vanadium transformation efficiency of the present embodiment is 84.89%, and in roasting process, balling, ring formation phenomenon do not appear in rotary kiln.
Claims (8)
1. a sodium roasting method for high full vanadium, is characterized in that: comprise the following steps:
A, pre-treatment: vanadium slag is pulverized, the screen underflow crossing 120 mesh sieves is not less than 80%, then deironing is to metallic iron≤5%, obtains smart slag;
B, batching: take raw material according to following weight relationships, tailings regulates smart slag to account for 6.5 ~ 7.0% of smart slag and tailings gross weight to full vanadium, and sodium salt is 1.5 ~ 1.7 times of Vanadium Pentoxide in FLAKES weight in smart slag and tailings, and tailings, smart slag, sodium salt mix to obtain compound;
C, roasting: compound is warming up to 550 ~ 600 DEG C from 300 DEG C in 2 ~ 2.5h, then in 2 ~ 3h, be warming up to 750 ~ 800 DEG C, then in 1 ~ 2h, be warming up to 850 DEG C, then be cooled to and be not less than 550 DEG C, get final product discharging.
2. the sodium roasting method of a kind of high full vanadium according to claim 1, is characterized in that: to vanadium-bearing hot metal, to be vanadium extraction by converter blowing method carry out that semisteel smelting extracts to described vanadium slag is rich in vanadium converter slag.
3. the sodium roasting method of a kind of high full vanadium according to claim 1, is characterized in that: described tailings is that vanadium slag is by sodium roasting and the slag obtained after carrying out water logging.
4. the sodium roasting method of a kind of high full vanadium according to claim 1, is characterized in that: by weight, the V in described vanadium slag
2o
5/ CaO is more than 4.5.
5. the sodium roasting method of a kind of high full vanadium according to claim 1, is characterized in that: the SiO in described vanadium slag
2≤ 12%.
6. the sodium roasting method of a kind of high full vanadium according to claim 1, is characterized in that: described sodium salt is at least one of soda ash or sodium-chlor.
7. the sodium roasting method of a kind of high full vanadium according to claim 6, is characterized in that: described sodium salt is the mixture of soda ash and sodium-chlor, and soda ash accounts for 80 ~ 85% of sodium salt gross weight.
8. the sodium roasting method of a kind of high full vanadium according to claim 1, is characterized in that: control oxygen level in tail gas and be not less than 8%.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107684974A (en) * | 2017-09-05 | 2018-02-13 | 攀枝花学院 | The method for preparing rich vanadium slag using vanadium iron smelting abrasive grit waste material |
| CN108893598A (en) * | 2018-08-21 | 2018-11-27 | 成渝钒钛科技有限公司 | A kind of production technology and its application reducing full vanadium in large-sized rotary kiln tailings |
| CN113428896A (en) * | 2021-06-22 | 2021-09-24 | 成都铬科高化工技术有限责任公司 | Method and device for preparing sodium vanadate by taking vanadium fine slag as raw material |
| CN113774237A (en) * | 2021-09-15 | 2021-12-10 | 中冶赛迪工程技术股份有限公司 | Method for preparing vanadium-rich liquid by using vanadium-rich slag |
| CN113981250A (en) * | 2021-10-27 | 2022-01-28 | 辽宁虹京实业有限公司 | Method for extracting vanadium by sodium salt roasting of vanadium slag |
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| CN86108218B (en) * | 1986-12-01 | 1988-08-03 | 冶金工业部攀枝花钢铁研究院 | One time vanadium dregs roasting in rotary furnace and extraction of vanadium by the aquo-soaking |
| CN102277482A (en) * | 2011-07-25 | 2011-12-14 | 四川省川威集团有限公司 | Method for preparing high-valence sodium salt compound of vanadium by sodiumizing and roasting all soda ash |
| CN101914673B (en) * | 2010-07-30 | 2012-07-25 | 四川省川威集团有限公司 | Sodium-translated roasting method of vanadium minerals |
| CN103643031A (en) * | 2013-11-28 | 2014-03-19 | 四川省川威集团有限公司 | Method of mixing and roasting vanadium-containing material |
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| CN86108218B (en) * | 1986-12-01 | 1988-08-03 | 冶金工业部攀枝花钢铁研究院 | One time vanadium dregs roasting in rotary furnace and extraction of vanadium by the aquo-soaking |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107684974A (en) * | 2017-09-05 | 2018-02-13 | 攀枝花学院 | The method for preparing rich vanadium slag using vanadium iron smelting abrasive grit waste material |
| CN107684974B (en) * | 2017-09-05 | 2019-10-01 | 攀枝花学院 | The method that abrasive grit waste material prepares rich vanadium slag is smelted using vanadium iron |
| CN108893598A (en) * | 2018-08-21 | 2018-11-27 | 成渝钒钛科技有限公司 | A kind of production technology and its application reducing full vanadium in large-sized rotary kiln tailings |
| CN113428896A (en) * | 2021-06-22 | 2021-09-24 | 成都铬科高化工技术有限责任公司 | Method and device for preparing sodium vanadate by taking vanadium fine slag as raw material |
| CN113774237A (en) * | 2021-09-15 | 2021-12-10 | 中冶赛迪工程技术股份有限公司 | Method for preparing vanadium-rich liquid by using vanadium-rich slag |
| CN113981250A (en) * | 2021-10-27 | 2022-01-28 | 辽宁虹京实业有限公司 | Method for extracting vanadium by sodium salt roasting of vanadium slag |
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Application publication date: 20150429 |