CN110512097A - A method of improving the conversion ratio of sodium roasting process Vanadium in Vanadium Residue - Google Patents
A method of improving the conversion ratio of sodium roasting process Vanadium in Vanadium Residue Download PDFInfo
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- CN110512097A CN110512097A CN201910912025.1A CN201910912025A CN110512097A CN 110512097 A CN110512097 A CN 110512097A CN 201910912025 A CN201910912025 A CN 201910912025A CN 110512097 A CN110512097 A CN 110512097A
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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
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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
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
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Abstract
The invention discloses a kind of methods of conversion ratio for improving sodium roasting process Vanadium in Vanadium Residue.Described method includes following steps: (1) mixing vanadium slag, sodium carbonate and alkaline tailings, obtain mixed material；(2) mixed material is roasted, obtains roasting clinker；(3) the roasting clinker is leached, is obtained containing vanadium solution and leached mud.The present invention has excellent compatibility, improves the conversion ratio of vanadium during vanadium slag sodium roasting by adding alkaline tailings, alkaline tailings and vanadium slag during vanadium slag sodium roasting；Simultaneously, alkalinity tailings of the present invention looks for that also to contain vanadium, during extracting Vanadium in Vanadium Residue element, vanadium in alkaline tailings also can be effectively extracted, and then alkaline tailings can not only be utilized with simple effective method, cost has been saved, and has recycled the vanadium in vanadium slag and alkaline tailings, the high-efficiency cleaning for realizing vanadium utilizes.
Description
Technical field
The invention belongs to the utilizations of resources and environmental technology field, and in particular to a kind of raising sodium roasting process Vanadium in Vanadium Residue
Conversion ratio method.
Background technique
The technique basic principle of sodium roasting is with Na2CO3For additive, by high temperature sodium roasting by the vanadium of lower valency
It is converted into the sodium salt of water-soluble pentavalent vanadium, then to the direct water logging of sodium roasting product, obtains the leaching liquid containing vanadium, leachate removal of impurities
Acid ammonium salt precipitation is carried out afterwards and generates ammonium poly-vanadate (APV), and ammonium poly-vanadate generates vanadic anhydride after calcining or reduction
(V2O5) or vanadium trioxide (V2O3).Sodium roasting technique vanadium recovery is low, and it is 80% or so, In that single, which roasts vanadium recovery,
Harmful HCl, Cl can be generated in roasting process2Equal subversive gas, pollute environment.
CN101215005A proposes a kind of vanadium slag and sodium salt (sodium carbonate, sodium chloride) or sylvite (potassium carbonate, potassium chloride)
The method of roasting, the patent are suitable for the low vanadium vanadium slag of high silicon, are matched by control maturing temperature and salt, V in tailings2O5Content can
Reach 0.5~1%.CN1884597A has carried out different improvement to the additive and temperature schedule of sodium roasting technique, substantially former
Reason is all the additive (Na by using different ratio2CO3、NaCl、Na2SO4、Na2SO3Deng) and different temperature come to vanadium
Recovery rate is improved and is improved, but process above and traditional sodium roasting principle, operating process, the basic phase of operation temperature
Together, it not can avoid and generate toxic and harmful gas, the problems such as vanadium recovery is low.
In conclusion in the prior art during Leaching of Vanadium from Vanadium slag generally there are the vanadium conversion ratio rate of recovery is low, vanadium removal process
In the problems such as there are toxic gas and the discharges of a large amount of acid ammonia nitrogen waste water, it is therefore desirable to develop a kind of new method to improve vanadium
Conversion ratio.
Summary of the invention
The purpose of the present invention is to provide a kind of methods of conversion ratio for improving sodium roasting process Vanadium in Vanadium Residue.The present invention
The method can effectively recycle the vanadium in vanadium slag, improve the recovery rate of vanadium, realize the high-efficiency cleaning benefit of vanadium slag
With.
To achieve this purpose, the present invention adopts the following technical scheme:
One of the objects of the present invention is to provide a kind of method of conversion ratio for improving sodium roasting process Vanadium in Vanadium Residue, institutes
The method of stating includes the following steps:
(1) vanadium slag, sodium carbonate and alkaline tailings are mixed, obtains mixed material；
(2) mixed material is roasted, obtains roasting clinker；
(3) the roasting clinker is leached, is obtained containing vanadium solution and leached mud.
The present invention has excellent phase with vanadium slag by adding alkaline tailings, alkaline tailings during vanadium slag sodium roasting
Capacitive improves the conversion ratio of vanadium during vanadium slag sodium roasting；Meanwhile also containing vanadium unit in alkaline tailings of the present invention
Element, during extracting Vanadium in Vanadium Residue element, the vanadium in alkaline tailings also can be effectively extracted, and then can not only
It is enough that alkaline tailings is utilized with simple effective method, cost is saved, and recycled the vanadium in vanadium slag and alkaline tailings,
The high-efficiency cleaning for realizing vanadium utilizes.
The present invention is baking mixed by vanadium slag and alkaline tailings, without adding sodium salt, has saved cost, maturing temperature is also significant
It reduces.
Alkalinity tailings of the present invention is the material that vanadium slag passes through that alkaline medium is handled.
Preferably, in step (1) described vanadium slag V element content be 1~5wt%, such as 1.2wt%, 1.5wt%,
2wt%, 2.5wt%, 3wt%, 3.5wt%, 4wt%, 4.5wt% or 4.8wt% etc..
Preferably, step (1) the alkaline tailings is the alkaline tailings containing vanadium and sodium element.
Preferably, the pH value of the alkaline tailings is 8~10, such as 8,9 or 10 etc..
Preferably, V element content is 0.5~1.5wt% in the alkaline tailings, such as 0.6wt%, 0.7wt%,
0.8wt%, 0.9wt%, 1wt%, 1.1wt%, 1.2wt%, 1.3wt% or 1.4wt% etc..
Preferably, Na constituent content is 10~20wt% in the alkaline tailings, for example, 11wt%, 12wt%, 13wt%,
14wt%, 15wt%, 16wt%, 17wt%, 18wt% or 19wt% etc..
Preferably, the mass ratio of step (1) vanadium slag and sodium carbonate is 1:(0.05~0.15), such as 1:0.06,1:
0.07,1:0.08,1:0.09,1:0.1,1:0.11,1:0.12,1:0.13 or 1:0.14 etc..
Preferably, the mass ratio of step (1) vanadium slag and alkaline tailings is 1:(0.05~0.2), such as 1:0.06,1:
0.07,1:0.08,1:0.09,1:0.1,1:0.11,1:0.12,1:0.15,1:0.16 or 1:0.18 etc..
Preferably, the partial size of step (1) described vanadium slag be 80~150 mesh, such as 100 mesh, 110 mesh, 120 mesh, 130 mesh or
140 mesh etc..
Preferably, the granularity of the alkaline tailings is 80~160 mesh, such as 100 mesh, 110 mesh, 120 mesh, 130 mesh or 140
Mesh etc..
The partial size of vanadium slag of the present invention and alkaline tailings within this range, can be conducive to the extraction of subsequent vanadium.
Preferably, the temperature of step (2) described roasting be 700~850 DEG C, such as 720 DEG C, 740 DEG C, 750 DEG C, 760 DEG C,
780 DEG C, 800 DEG C, 820 DEG C or 840 DEG C etc..
The temperature of roasting of the present invention is too low, and vanadium slag cannot be fully oxidized, and causes the recovery rate of vanadium lower；Institute
The temperature for stating roasting is excessively high, and vanadium slag material during roasting oxidation is easy sintering, agglomeration.
Preferably, the time of step (2) described roasting be 0.5~2h, such as 0.6h, 0.8h, 1h, 1.2h, 1.4h,
1.5h, 1.6h or 1.8h etc..
Preferably, step (2) roasting carries out in Muffle furnace.
Preferably, step (3) leaching includes: and will roast clinker to leach in the water that temperature is 80~95 DEG C, such as
82 DEG C, 85 DEG C, 88 DEG C, 90 DEG C, 92 DEG C or 94 DEG C etc..
The temperature for the water that the present invention chooses is more advantageous to the dissolution of vanadium and sodium element in water in raising roasting clinker
Degree, is conducive to the extraction of vanadium and sodium element.
Preferably, the time of the leaching is 0.5~2h, such as 0.6h, 0.8h, 1h, 1.2h, 1.5h, 1.6h or 1.8h
Deng.
Preferably, the leaching process, the mass ratio for roasting clinker and water is 1:(1~3), such as 1:1.2,1:1.5,1:
1.6,1:1.8,1:2,1:2.2,1:2.5 or 1:2.8 etc..
Preferably, further include step (4) after step (3): step (3) leached mud being washed, tailings is obtained and washes
Wash liquid.
Preferably, the washing process of the leached mud includes: to wash the leached mud in the water that temperature is 80~95 DEG C
It washs, such as 82 DEG C, 85 DEG C, 88 DEG C, 90 DEG C, 92 DEG C or 94 DEG C etc..
Preferably, the time of the washing is 0.5~1h, such as 0.6h, 0.7h, 0.8h or 0.9h etc..
Preferably, the mass ratio of the washing process, leached mud and water is 1:(0.5~1), such as 1:0.6,1:0.7,1:
0.9 or 1:1 etc..
As optimal technical scheme, a kind of method for the conversion ratio improving sodium roasting process Vanadium in Vanadium Residue of the present invention
Include the following steps:
(1) the alkaline tailings that vanadium slag, sodium carbonate and partial size that granularity is 80~150 mesh are 80~160 mesh is mixed, is obtained
Mixed material, V element content is 1~5wt% in the vanadium slag, and V element content is 0.5~1.5wt% in the alkalinity tailings,
Na constituent content is 10~20wt%, and the mass ratio of the vanadium slag and sodium carbonate is 1:(0.05~0.15), the vanadium slag and alkali
Property tailings mass ratio be 1:(0.05~0.2)；
(2) mixed material is placed in Muffle furnace, 700~850 DEG C of 0.5~2h of roasting, obtains roasting clinker；
It (3) is that 0.5~2h is leached in 80~95 DEG C of water in temperature by the roasting clinker, the roasting clinker and water
Mass ratio is 1:(1~3), it obtains containing vanadium solution and leached mud；
(4) leached mud is washed into 0.5~1h, the quality of the leached mud and water in the water that temperature is 80~95 DEG C
Than for 1:(0.5~1), obtain tailings and cleaning solution.
Compared with the existing technology, the invention has the following advantages:
(1) present invention has excellent by adding alkaline tailings, alkaline tailings during vanadium slag sodium roasting with vanadium slag
Compatibility, improve the conversion ratio of vanadium during vanadium slag sodium roasting；Meanwhile alkaline tailings of the present invention looks for that also to contain
There is vanadium, during extracting Vanadium in Vanadium Residue element, the vanadium in alkaline tailings also can be effectively extracted, in turn
Cost can not only be saved, and recycled in vanadium slag and alkaline tailings with simple effective method using alkaline tailings
Vanadium, the high-efficiency cleaning for realizing vanadium utilize.
(2) present invention is baking mixed by vanadium slag and alkaline tailings, without adding sodium salt, has saved cost, maturing temperature
It significantly reduces.
Specific embodiment
The technical scheme of the invention is further explained by means of specific implementation.Those skilled in the art should be bright
, the described embodiments are merely helpful in understanding the present invention, should not be regarded as a specific limitation of the invention.
Embodiment 1
(1) it is crushed: vanadium slag is subjected to ball milling, being crushed to granularity is 100 mesh, and V element content is 3wt% in the vanadium slag；
(2) ingredient: vanadium slag, sodium carbonate and alkaline tailings being uniformly mixed by 1:0.1:0.07, obtain mixed material, described
V element content is 0.9wt% in alkaline tailings, and Na constituent content is 12wt%, and the pH value of alkaline tailings is 9；
(3) it roasts: mixed material is placed in Muffle furnace at 820 DEG C, roast 1.5h, obtain roasting clinker；
(4) leach: by the roasting clinker with 85 DEG C of hot water leaching 1h, the clinker and the mass ratio of water of roasting is 1:1,
It obtains containing vanadium solution and leached mud；
(5) it washs: the leached mud being washed into 0.5h with 80 DEG C of hot water, the mass ratio of the leached mud and water is 1:
0.5, obtain cleaning solution and tailings.
Embodiment 2
(1) it is crushed: vanadium slag is subjected to ball milling, being crushed to granularity is 80 mesh, and V element content is 4wt% in the vanadium slag；
(2) ingredient: vanadium slag, sodium carbonate and alkaline tailings being uniformly mixed by 1:0.08:0.1, obtain mixed material, described
V element content is 1wt% in alkaline tailings, and Na constituent content is 13wt%, and the pH value of alkaline tailings is 9；
(3) it roasts: mixed material is placed in Muffle furnace at 800 DEG C, roast 2h, obtain roasting clinker；
(4) leach: roasting 95 DEG C of hot water leachings of clinker are obtained containing vanadium solution and leached mud；
(5) wash: leached mud is washed with 85 DEG C of hot water, obtains cleaning solution and tailings.
Embodiment 3
(1) it is crushed: vanadium slag is subjected to ball milling, being crushed to granularity is 120 mesh, and V element content is 5wt% in the vanadium slag；
(2) ingredient: vanadium slag, sodium carbonate and alkaline tailings are uniformly mixed by 1:0.05:0.15, obtain mixed material, institute
Stating V element content in alkaline tailings is 1.2wt%, and Na constituent content is 15wt%, and the pH value of alkaline tailings is 10；
(3) it roasts: mixed material is placed in Muffle furnace at 780 DEG C, roast 0.5h, obtain roasting clinker；
(4) leach: roasting 90 DEG C of hot water leachings of clinker are obtained containing vanadium solution and leached mud；
(5) wash: leached mud is washed with 90 DEG C of hot water, obtains tailings and cleaning solution.
Embodiment 4
(1) it is crushed: vanadium slag is subjected to ball milling, being crushed to granularity is 110 mesh, and V element content is 2wt% in the vanadium slag；
(2) ingredient: vanadium slag, sodium carbonate and alkaline tailings are uniformly mixed by 1:0.12:0.05, obtain mixed material, institute
Stating V element content in alkaline tailings is 0.6wt%, and Na constituent content is 8wt%, pH value 8；
(3) it roasts: mixed material is placed in Muffle furnace at 750 DEG C, roast 1h, obtain roasting clinker；
(4) leach: roasting 80 DEG C of hot water leachings of clinker are obtained containing vanadium solution and leached mud；
(5) wash: leached mud is washed with 90 DEG C of hot water, obtains cleaning solution and tailings.
Embodiment 5
The difference from embodiment 1 is that the mass ratio of step (2) vanadium slag and sodium carbonate is 1:0.04.
Embodiment 6
The difference from embodiment 1 is that the mass ratio of step (2) vanadium slag and sodium carbonate is 1:0.2.
Comparative example 1
The difference from embodiment 1 is that step (2) the alkaline tailings to be replaced with to the sodium carbonate of equivalent.
Performance test:
The content of vanadium in the tailings that each embodiment and comparative example obtains is tested, and by containing vanadium solution and cleaning solution meter
Calculate total leaching rate of the vanadium in vanadium slag and alkaline tailings.
Table 1
It can be seen from Table 1 that the embodiment of the present invention 5 is higher relative to vanadium unit cellulose content in 1 tailings of embodiment, vanadium
Leaching rate is lower, because the mass ratio of vanadium slag and sodium carbonate is 1:0.04 in embodiment 5, the content of sodium carbonate is very few, leads to vanadium
Vanadium in slag is incomplete by the oxidation reaction of trivalent to pentavalent, causes leaching rate lower；It can be seen from Table 1 that this hair
Bright embodiment 6 is higher relative to vanadium unit cellulose content in 1 tailings of embodiment because in embodiment 6 vanadium slag and sodium carbonate mass ratio
For 1:0.2, the too high levels of sodium carbonate cause other impurities element in tailings to be also leached, and purity containing vanadium solution is lower, thus
Vanadium unit cellulose content is higher in tailings；Meanwhile the too high levels of sodium carbonate also result in vanadium slag and are easy balling, agglomeration, cause vanadium oxygen
Rate reduces, and then recovery rate is lower.
It can be seen from Table 1 that comparative example 1 of the present invention is higher relative to vanadium unit cellulose content in 1 tailings of embodiment, vanadium
Leaching rate is lower, because alkaline tailings to be replaced with to the sodium carbonate of equivalent in comparative example 1, basic matterial is more, and vanadium slag is easy knot
Ball, agglomeration lead to the reduction of vanadium oxygenation efficiency, while sodium carbonate is poor by the conversion process facilitation of trivalent to pentavalent for vanadium
(relative to alkaline tailings), therefore cause vanadium recovery rate lower.
Method detailed of the invention that the present invention is explained by the above embodiments, but the invention is not limited to it is above-mentioned in detail
Method, that is, do not mean that the invention must rely on the above detailed methods to implement.Person of ordinary skill in the field should
It is illustrated, any improvement in the present invention, addition, the concrete mode of equivalence replacement and auxiliary element to each raw material of product of the present invention
Selection etc., all of which fall within the scope of protection and disclosure of the present invention.
Claims (10)
1. a kind of method for the conversion ratio for improving sodium roasting process Vanadium in Vanadium Residue, which is characterized in that the method includes as follows
Step:
(1) vanadium slag, sodium carbonate and alkaline tailings are mixed, obtains mixed material；
(2) mixed material is roasted, obtains roasting clinker；
(3) the roasting clinker is leached, is obtained containing vanadium solution and leached mud.
2. preparation method as described in claim 1, which is characterized in that in step (1) described vanadium slag V element content be 1~
5wt%.
3. preparation method as claimed in claim 1 or 2, which is characterized in that step (1) the alkaline tailings is to contain vanadium
With the alkaline tailings of sodium element；
Preferably, the pH value of the alkaline tailings is 8~10；
Preferably, V element content is 0.5~1.5wt% in the alkaline tailings；
Preferably, Na constituent content is 10~20wt% in the alkaline tailings.
4. the preparation method as described in one of claim 1-3, which is characterized in that the matter of step (1) vanadium slag and sodium carbonate
Amount is than being 1:(0.05~0.15).
5. the preparation method as described in one of claim 1-4, which is characterized in that step (1) vanadium slag and alkaline tailings
Mass ratio is 1:(0.05~0.2).
6. the preparation method as described in one of claim 1-5, which is characterized in that the partial size of step (1) described vanadium slag be 80~
150 mesh；
Preferably, the granularity of the alkaline tailings is 80~160 mesh.
7. the preparation method as described in one of claim 1-6, which is characterized in that the temperature of step (2) described roasting be 700~
850℃；
Preferably, the time of step (2) described roasting is 0.5~2h；
Preferably, step (2) roasting carries out in Muffle furnace.
8. the preparation method as described in one of claim 1-7, which is characterized in that step (3) it is described leaching include: will roast it is ripe
Expect to leach in the water that temperature is 80~95 DEG C；
Preferably, the time of the leaching is 0.5~2h；
Preferably, the leaching process, the mass ratio for roasting clinker and water is 1:(1~3).
9. preparation method as described in one of claim 1-8, which is characterized in that further include step (4) after step (3): will
Step (3) the leached mud washing, obtains tailings and cleaning solution；
Preferably, the washing process of the leached mud includes: to wash the leached mud in the water that temperature is 80~95 DEG C；
Preferably, the time of the washing is 0.5~1h；
Preferably, the mass ratio of the washing process, leached mud and water is 1:(0.5~1).
10. preparation method as claimed in one of claims 1 to 9, which is characterized in that described method includes following steps:
(1) the alkaline tailings that vanadium slag, sodium carbonate and partial size that partial size is 80~150 mesh are 80~160 mesh is mixed, is mixed
Material, V element content is 1~5wt% in the vanadium slag, and V element content is 0.5~1.5wt%, Na member in the alkalinity tailings
Cellulose content is 10~20wt%, and the mass ratio of the vanadium slag and sodium carbonate is 1:(0.05~0.15), the vanadium slag and alkaline tail
The mass ratio of slag is 1:(0.05~0.2)；
(2) mixed material is placed in Muffle furnace, 700~850 DEG C of 0.5~2h of roasting, obtains roasting clinker；
(3) the roasting clinker is leached into 0.5~2h, the quality of the roasting clinker and water in the water that temperature is 80~95 DEG C
Than for 1:(1~3), it obtains containing vanadium solution and leached mud；
It (4) is that 0.5~1h is washed in 80~95 DEG C of water in temperature by the leached mud, the mass ratio of the leached mud and water is
1:(0.5~1), obtain tailings and cleaning solution.
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| 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 |
| CN113981208A (en) * | 2021-10-13 | 2022-01-28 | 河钢承德钒钛新材料有限公司 | Roasting method of secondary slag |
| CN114703362A (en) * | 2022-03-17 | 2022-07-05 | 四川省银河化学股份有限公司 | Method for combined sodium roasting of vanadium-containing and chromium-containing raw materials |
| CN115216648A (en) * | 2022-07-22 | 2022-10-21 | 攀枝花市阳润科技有限公司 | Method for extracting vanadium from vanadium-containing tailings |
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| CN113981208A (en) * | 2021-10-13 | 2022-01-28 | 河钢承德钒钛新材料有限公司 | Roasting method of secondary slag |
| CN114703362A (en) * | 2022-03-17 | 2022-07-05 | 四川省银河化学股份有限公司 | Method for combined sodium roasting of vanadium-containing and chromium-containing raw materials |
| CN114703362B (en) * | 2022-03-17 | 2024-04-05 | 四川明宏恒正科技股份有限公司 | Method for combined sodium roasting of vanadium-containing and chromium-containing raw materials |
| CN115216648A (en) * | 2022-07-22 | 2022-10-21 | 攀枝花市阳润科技有限公司 | Method for extracting vanadium from vanadium-containing tailings |
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Application publication date: 20191129 |