CN110042248A - The method for preparing ferric vandate as raw material using dephosphorization mud - Google Patents
The method for preparing ferric vandate as raw material using dephosphorization mud Download PDFInfo
- Publication number
- CN110042248A CN110042248A CN201910360298.XA CN201910360298A CN110042248A CN 110042248 A CN110042248 A CN 110042248A CN 201910360298 A CN201910360298 A CN 201910360298A CN 110042248 A CN110042248 A CN 110042248A
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- CN
- China
- Prior art keywords
- raw material
- dephosphorization
- mud
- ferric vandate
- dephosphorization mud
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Classifications
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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
- 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
- C22B7/007—Wet processes by acid leaching
-
- 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The invention belongs to hydrometallurgical process fields, and in particular to a method of ferric vandate is prepared using dephosphorization mud as raw material.Technical problem to be solved by the invention is to provide the methods for preparing ferric vandate as raw material using dephosphorization mud, comprising the following steps: a, acidleach: using vitriol lixiviation dephosphorization mud, separation of solid and liquid obtains immersion liquid containing vanadic acid；B, it precipitates: molysite is added in immersion liquid containing vanadic acid, adjustment system pH to 1.5~2.0 is precipitated to get ferric vandate.The method of the present invention has many advantages, such as short production procedure, environmental protection and energy saving, vanadium high income.
Description
Technical field
The invention belongs to hydrometallurgical process fields, and in particular to a kind of side that ferric vandate is prepared using dephosphorization mud as raw material
Method more particularly to a kind of method from the clay standby ferric vandate of alkaline vanadium leachate dephosphorization.
Background technique
Vanadium is a kind of important strategic resource, is widely used in steel, chemistry, machine-building, automobile, railway, bridge, boat
The fields such as empty space flight, the high-tech most advanced branches of science, military project and new energy.The raw material of production vanadium product has vanadium titano-magnetite at present
(or the vanadium slag produced by vanadium titano-magnetite), bone coal, dead catalyst, the petroleum residue of China etc., wherein 80% or more vanadium produces
Product derive from vanadium titano-magnetite or vanadium slag.Using sodium-salt calcination-water logging process for extracting vanadium from vanadium slag when vanadium extraction, vanadium is in clinker water logging
Enter alkaline leaching liquid in the process, but the impurity such as phosphorus also leach into vanadium leachate.Due to the phosphorus meeting in alkaline vanadium leachate
Heteropoly acid is formed with ammonium, vanadium, to influence vanadium rate of deposition and final products quality.At present vanadium enterprise usually use calcium salt, magnesium salts and
Aluminium salt dephosphorization can make a small amount of vanadium enter dephosphorization mud when wherein using calcium salt dephosphorization.Dephosphorization mud usually returns to roaster rotary kiln
Carry out after baking.Although the method has recycled vanadium, but since the calcium content in dephosphorization mud is high, while reducing roasting effect,
It causes the impurity recyclings such as phosphorus, silicon to be enriched with, brings difficulty to production.
Wet-treating is carried out to alkaline vanadium leachate dephosphorization mud in document or patent at present, produces ammonium metavanadate, more vanadic acid
The problems such as products such as ammonium or calcium vanadate respectively have advantage, but generally existing process flow is longer and vanadium yield is relatively low.
Jinzhou Fan Ye company is studied using the vanadium in secondary alkali soaking technology extraction dephosphorization underflow slag, V leaching rate
Up to 75% or more, but filter cake moisture content reaches 70% or more.CN102910674A discloses the new of the clay standby calcium vanadate of dephosphorization
Technique, the technique leach dephosphorization mud with alkaline aqueous solution first, remove silicon again after obtaining leachate；Then again under alkaline condition,
With solubility calcium reactant salt, vanadic acid calcium precipitate is obtained, but the method vanadium yield is relatively low.CN103911521A using sodium oxalate or
The Leaching Vanadium from dephosphorization mud such as potassium oxalate produces ammonium metavanadate after ammonium salt precipitation is added, but oxalates Leaching Vanadium is only up to
85% or so.CN102337409A recycles vanadium using sulfuric acid solution from dephosphorization mud, leaches dephosphorization mud with sulfuric acid solution first and obtains
To vanadium leachate is contained, ammonium metavanadate or more then is obtained with chemical method or ion-exchange purification or Vanadium Concentrationin, then ammonium salt precipitation
Barium oxide is finally made in ammonium vanadate.The vanadium yield of the technique is 91% or so, but the process flow is long, high production cost.
Therefore, from current report or patent, there has been no the works that ferric vandate is produced from alkaline vanadium leachate dephosphorization mud
Skill.
Summary of the invention
Technical problem to be solved by the invention is to provide one kind to prepare vanadic acid using alkaline vanadium leachate dephosphorization mud as raw material
The method of iron.Method includes the following steps:
A, acidleach: using vitriol lixiviation dephosphorization mud, and separation of solid and liquid obtains immersion liquid containing vanadic acid；
B, it precipitates: molysite is added in immersion liquid containing vanadic acid, adjustment system pH to 1.5~2.0 is precipitated to get vanadic acid
Iron.
Specifically, above-mentioned prepare in the method and step a of ferric vandate by raw material of dephosphorization mud, the dephosphorization mud is by vanadium slag sodium
The alkaline leaching liquid that roasting-water logging generates is obtained by the calcium salt dephosphorization process.
Further, above-mentioned to be prepared in the method and step a of ferric vandate by raw material of dephosphorization mud, the dephosphorization mud primary chemical
Composition are as follows: V 8~13%, Ca7~18%, Fe 4~15%, Si 5~8%, Na 4~8%.
Preferably, above-mentioned to be prepared in the method and step a of ferric vandate by raw material of dephosphorization mud, the sulfuric acid concentration be 2.3~
3.0mol·L-1。
Specifically, above-mentioned prepare in the method and step a of ferric vandate by raw material of dephosphorization mud, the acidleach temperature is 30~90
℃.Leaching time is 20~40min.
Specifically, above-mentioned prepare in the method and step a of ferric vandate by raw material of dephosphorization mud, the liquid-solid ratio of the acidleach is 4 ﹕
1~6 ﹕ 1mL/g.
Specifically, above-mentioned prepare in the method and step a of ferric vandate by raw material of dephosphorization mud, vanadium is dense in the immersion liquid containing vanadic acid
Degree is 10g/L or more.
Specifically, above-mentioned prepare in the method and step b of ferric vandate by raw material of dephosphorization mud, the molysite be ferrous sulfate,
At least one of ferric sulfate or iron chloride.
Preferably, above-mentioned to prepare in the method and step b of ferric vandate by raw material of dephosphorization mud, the molysite is ferric sulfate.
Specifically, above-mentioned prepare in the method and step b of ferric vandate by raw material of dephosphorization mud, the additional amount of the molysite be containing
V in vanadic acid immersion liquid2O51.5~2 times of quality.
Preferably, above-mentioned to prepare in the method and step b of ferric vandate by raw material of dephosphorization mud, the precipitation temperature is 40~95
℃。
It is furthermore preferred that above-mentioned prepare in the method and step b of ferric vandate by raw material of dephosphorization mud, the precipitation temperature is 90
℃。
Specifically, above-mentioned prepare in the method and step b of ferric vandate by raw material of dephosphorization mud, the sedimentation time is 1~2h.
The present invention has the advantage that in the method that alkaline vanadium leachate dephosphorization mud prepares ferric vandate as raw material
1, production procedure is short: the pickle liquor after the leaching of dephosphorization mud acid directly being prepared ferric vandate and utilizes alkaline leaching system with existing
Standby ammonium poly-vanadate or ammonium metavanadate are compared, and production procedure is short, and step is few and at low cost.
2, environmental protection and energy saving: not generating ammonia nitrogen waste water in production process, ferric vandate can be directly used for smelting low vanadium iron.Vanadium at present
Three oxidations that the raw material that iron uses obtains after the vanadic anhydride or reduction that ammonium poly-vanadate or ammonium metavanadate melt
Two vanadium.
3, vanadium high income: the acidleach vanadium yield of the method for the present invention processing dephosphorization mud is up to 98% or more, molysite deposition yield
Also reach 92% or more, total recovery is more than 90%.
Specific embodiment
The method that the present invention prepares ferric vandate as raw material using the alkaline vanadium leachate mud of dephosphorization containing vanadium, comprising the following steps:
A, acidleach: will contain vanadium dephosphorization mud vitriol lixiviation, be separated by solid-liquid separation, and obtain slag and liquid, and liquid is to contain vanadic acid leaching
Liquid；
B, it precipitates: molysite being added into immersion liquid containing vanadic acid, then adjusts system pH to 1.5~2.0 with liquid alkaline, precipitating obtains vanadium
Sour iron.
In the method for the present invention step a, the alkaline leaching liquid that the dephosphorization mud is generated by vanadium slag sodium roasting-water logging is in calcium salt
Obtained by dephosphorization process.Further, dephosphorization mud primary chemical forms are as follows: V 8~13%, Ca7~18%, Fe 4~15%, Si5
~8%, Na 4~8%, moisture 25~45%.
In the method for the present invention step a, the purpose of using vitriol lixiviation be by dephosphorization mud with vanadium existing for pyrovanadic acid calcium form
It is leached in immersion liquid containing vanadic acid, the vanadium in immersion liquid containing vanadic acid is with vanadium oxygroup VO2 +Form exist.The chemical equation related generally to
Formula is Ca2V2O7+6H++2SO4 2-→2CaSO4+2VO2 ++3H2O.The sulfuric acid concentration is 2.3~3.0molL-1.The acidleach
Temperature is 30~90 DEG C.Leaching time is 20~40min.The liquid-solid ratio of the acidleach is 4 ﹕, 1~6 ﹕ 1mL/g.
In the method for the present invention step b, the molysite is at least one of ferrous sulfate, ferric sulfate or iron chloride.It is preferred that iron
Salt is ferric sulfate.The additional amount of ferric sulfate is vanadium in immersion liquid containing vanadic acid (with V2O5Meter) 1.5~2 times of quality.
In the method for the present invention step b, if system pH < 1.5, the vanadium Yishui River parses V2O5If system pH > 2, the ferric iron Yishui River
Solution forms Fe (OH)3Precipitating, so needing control system pH is 1.5~2.0.
In the method for the present invention step b, temperature has certain influence to precipitating crystal form and sedimentation time, and it is advantageous to precipitation temperatures
Control is 40~95 DEG C.More preferable 90 DEG C.
In the method for the present invention, not yet explicitly illustrate, percentage, content etc. indicate mass percent.
Embodiment 1
It takes 1kg dephosphorization mud to be placed in reaction kettle, 2.5molL is added-1Sulfuric acid 5L, then leaching under the conditions of 70 DEG C
It is separated by solid-liquid separation after 30min, obtains [V] 11.6gL-1Pickle liquor.Take 4L pickle liquor that 160g ferric sulfate is added at normal temperature
Afterwards, pickle liquor pH value is adjusted to 1.8, after precipitating 2h with sodium hydroxide solution under the conditions of 90 DEG C of temperature, stirring intensity 250rpm
It is separated by solid-liquid separation, then by precipitated product washing, drying, show that content of vanadium is 38.2% ferric vandate.
The present embodiment acidleach vanadium yield 98.7%, precipitating vanadium yield 93.1%, process total recovery 91.9%；Gained ferric vandate
Chemical composition: V 38.2%, Fe5.2%, Si0.2%, P0.5%.
Embodiment 2
It takes 2kg dephosphorization mud to be placed in reaction kettle, 2.7molL is added-1Sulfuric acid 10L, leaching is then stirred under the conditions of 80 DEG C
It is separated by solid-liquid separation after 40min out, obtains [V] 12.8gL-1Pickle liquor.Take 5L pickle liquor that 200g sulfuric acid is added at normal temperature
After iron, pickle liquor pH value is adjusted to 2.0 with sodium hydroxide solution under the conditions of 90 DEG C of temperature, stirring intensity 250rpm, is precipitated
It is separated by solid-liquid separation after 1.5h, then by precipitated product washing, drying, show that content of vanadium is 40.3% ferric vandate.
The present embodiment acidleach vanadium yield 99.2%, precipitating vanadium yield 93.5%, process total recovery 92.8%；Gained ferric vandate
Chemical composition: V40.3%, Fe6.2%, Si0.2%, P0.3%.
Claims (10)
1. the method for preparing ferric vandate as raw material using dephosphorization mud, it is characterised in that: the following steps are included:
A, acidleach: using vitriol lixiviation dephosphorization mud, and separation of solid and liquid obtains immersion liquid containing vanadic acid；
B, it precipitates: molysite is added in immersion liquid containing vanadic acid, adjustment system pH to 1.5~2.0 is precipitated to get ferric vandate.
2. the method according to claim 1 for preparing ferric vandate as raw material using dephosphorization mud, it is characterised in that: in step a, institute
Alkaline leaching liquid that dephosphorization mud is generated as vanadium slag sodium roasting-water logging is stated obtained by the calcium salt dephosphorization process；Further, described to remove
Phosphorus mud primary chemical composition are as follows: V 8~13%, Ca7~18%, Fe 4~15%, Si 5~8%, Na 4~8%.
3. the method according to claim 1 or 2 for preparing ferric vandate as raw material using dephosphorization mud, it is characterised in that: step a
In, the sulfuric acid concentration is 2.3~3.0molL-1。
4. the method according to claim 1 or 2 for preparing ferric vandate as raw material using dephosphorization mud, it is characterised in that: step a
In, the acidleach temperature is 30~90 DEG C；Leaching time is 20~40min.
5. the method according to claim 1 or 2 for preparing ferric vandate as raw material using dephosphorization mud, it is characterised in that: step a
In, the liquid-solid ratio of the acidleach is 4 ﹕, 1~6 ﹕ 1mL/g.
6. the method according to claim 1 or 2 for preparing ferric vandate as raw material using dephosphorization mud, it is characterised in that: step a
In, vanadium concentration is 10g/L or more in the immersion liquid containing vanadic acid.
7. described in any item methods for preparing ferric vandate as raw material using dephosphorization mud according to claim 1~3, it is characterised in that:
In step b, the molysite is at least one of ferrous sulfate, ferric sulfate or iron chloride；Preferably sulfuric acid iron.
8. described in any item methods for preparing ferric vandate as raw material using dephosphorization mud according to claim 1~3, it is characterised in that:
In step b, the additional amount of the molysite is V in immersion liquid containing vanadic acid2O51.5~2 times of quality.
9. described in any item methods for preparing ferric vandate as raw material using dephosphorization mud according to claim 1~3, it is characterised in that:
In step b, the precipitation temperature is 40~95 DEG C；It is preferred that 90 DEG C.
10. described in any item methods for preparing ferric vandate as raw material using dephosphorization mud according to claim 1~3, it is characterised in that:
In step b, the sedimentation time is 1~2h.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110951970A (en) * | 2019-11-28 | 2020-04-03 | 攀钢集团钒钛资源股份有限公司 | Method for recovering vanadium from vanadium-containing underflow slag |
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| CN110951970A (en) * | 2019-11-28 | 2020-04-03 | 攀钢集团钒钛资源股份有限公司 | Method for recovering vanadium from vanadium-containing underflow slag |
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