CN106282607A - One utilizes V5+the extracting and enriching method containing vanadium solution - Google Patents
One utilizes V5+the extracting and enriching method containing vanadium solution Download PDFInfo
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- CN106282607A CN106282607A CN201610785701.XA CN201610785701A CN106282607A CN 106282607 A CN106282607 A CN 106282607A CN 201610785701 A CN201610785701 A CN 201610785701A CN 106282607 A CN106282607 A CN 106282607A
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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
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/26—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds
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Abstract
The present invention relates to one and utilize V5+The extracting and enriching method containing vanadium solution, the pH value that vanadium-containing material first leaches stock solution regulates below 7, generates precipitation or floccule, adds oxidant the most under agitation and reacts, reaction solution gradually becomes crineous, and now the vanadium ion in reaction solution is oxidized to V5+, filtering reacting solution, it is thus achieved that filtrate for extraction stock solution；The pH value of extraction stock solution is regulated below 7, then uses the extraction organic facies that pH value is equal with extracting stock solution pH value will extract the V in stock solution5+Carry out counter-current extraction, it is thus achieved that enrichment V5+Organic facies and the remaining water of extraction, V will be enriched with5+Organic facies carry out back extraction process by back washing agent solution, it is thus achieved that enrichment V5+Turn one's coat and store, be obtained by V5+Extracting and enriching contains vanadium solution.The present invention is with V5+Valence state purification by liquid extraction, enrichment is containing vanadium solution, it is not necessary to repeatedly changing valence state, vanadium recovery is high.
Description
[technical field]
The present invention relates to field of metallurgy, be specifically related to one and utilize V5+The extracting and enriching method containing vanadium solution.
[background technology]
Be always the primary raw material of vanadium smelting containing vanadium mineral resources and vanadium-containing material, the most all have maturation process technology and
Production method, but along with being continually changing of the market quotation, the continuous lifting of environmental requirement, tradition V4+Extraction or the smelting of ion exchange
Refining mode cost remains high.
This is owing to the most unanimously thinking V5+Because the reasons such as dissolubility are unfavorable for extraction, therefore rare people uses.
Tradition is with V4+The technique of extraction can only be to V4+Extract, so must be by V5+Restore All is V4+Rear extraction, the most again by V4 +All it is oxidized to V5+Just can carry out precipitation operation, valence state changes repeatedly, and consumptive material is time-consuming.And with V4+Extraction technique have with
Lower shortcoming:
1, main employing ion-type extractant, saturation is low, and extracting power is very limited.
2、V4+Extraction, due to extracting power reason, extraction progression is many, general >=more than 6 grades.
3、V4+Conventional extractant has certain absorbability to Fe, therefore extraction process purifies not, and product F e is the most higher；
4、V4+Extracting concentration of turning one's coat relatively low, treating capacity is little；
5、V4+Extraction acid consumption height, environmental protection treatment is expensive, sewage can not circular treatment uses, extraction fills out that groove amount is big, take
The shortcomings such as metal is many, use Hazardous Chemical Substances simultaneously in a large number, and managing risk is big.
[summary of the invention]
It is an object of the invention to overcome problem present in technology, it is provided that one utilizes V5+Extracting and enriching is containing vanadium solution
Method, it is not necessary to repeatedly change the valence state of vanadium ion, and extraction yield is high.
In order to achieve the above object, the present invention adopts the following technical scheme that
Comprise the following steps:
(1) pH value that vanadium-containing material leaches stock solution regulates below 7, generates precipitation or floccule, then at stirring bar
Adding oxidant under part to react, reaction solution gradually becomes crineous, and now the vanadium ion in reaction solution is oxidized to V5+,
Filtering reacting solution, it is thus achieved that filtrate for extraction stock solution；
(2) pH value of extraction stock solution is regulated below 7, then use the extraction that pH value is equal with extraction stock solution pH value organic
By the V in extraction stock solution5+Carry out counter-current extraction, it is thus achieved that enrichment V5+Organic facies and the remaining water of extraction, V will be enriched with5+Organic
Back extraction process is carried out mutually, it is thus achieved that enrichment V by back washing agent solution5+Turn one's coat and store, be obtained by V5+Extracting and enriching is molten containing vanadium
Liquid；
Wherein, by mass percentage, extraction organic facies is composed of the following components: 5～the extractant of 30%, 2～15%
Synergic reagent, surplus is solvent.
Further, the vanadium-containing material of step (1) leaches the vanadium ion in stock solution containing+5 ,+4 ,+3 and+2, and if
All vanadium ions all generate V205Time, V205Concentration is 2g/L～20g/L.
Further, the oxidant in step (1) include hydrogen peroxide, sodium thiosulfate, calcium chlorate, sodium chlorate, potassium chlorate,
A kind of or the most two or more mixture in calcium hypochlorite, postassium hypochlorite and chlorine.
Further, step (1) aoxidizes until detecting V4+It is converted into V2O5Concentration terminate when below 1g/L.
Further, the extraction stock solution during vanadium-containing material leaches stock solution, step (2) in step (1) and extraction organic facies
PH value is all adjusted to 1.3～2.7 by pH value regulator, and pH value regulator includes: sulphuric acid, hydrochloric acid, nitric acid, sodium hydroxide, hydrogen
A kind of or the most two or more in potassium oxide, calcium oxide, calcium hydroxide, magnesium carbonate, sodium carbonate and natural whiting stone powder
Mixture；
Back washing agent solution in step (2) is that back washing agent is dissolved in water mixing all by the mass percent of 2～15%
Even obtain；Back washing agent is sodium hydroxide/potassium, sodium carbonate/potassium, sodium bicarbonate/potassium, sodium oxide and the one of potassium oxide or any
Two or more mixture, or a kind of or the most two or more mixture of sulphuric acid, hydrochloric acid and nitric acid.
Further, the oxidizing reaction temperature in step (1) and the extraction temperature in step (2) are all at 25～50 DEG C.
Further, extractant include tri-n-octyl amine, trioctylamine, Mextral 54-100, N235, Alamine 336,
A kind of or the most two or more mixture in N263, N1923, HBL101 and P507；Synergic reagent includes n-octyl alcohol, different pungent
Alcohol, sec-octyl alcohol or tributyl phosphate；Solvent includes the one in solvent kerosene, sulfonated kerosene, benzene, chloroform or 2 one ethyl hexanols
Or the most two or more mixture.
Further, the extraction progression of counter-current extraction is 2～4 grades, and extraction is in a ratio of organic facies: aqueous phase=1:(1～5),
Extract stream speed ratio is organic facies: aqueous phase=1:(1～5)；Extraction is no less than 3 minutes time of contact.
Further, the extraction progression that back extraction processes is 2～5 grades, and back extraction is in a ratio of organic facies: aqueous phase=(1～5): 1,
Back extraction velocity ratio is organic facies: aqueous phase=(1～5): 1；Back extraction is no less than 5 minutes time of contact.
Further, the extraction organic facies after back extraction processes is regenerated by regenerant solution, and the organic facies after regeneration is backflowed
To extraction organic facies groove, regeneration progression is 1～2 grade, and regeneration is in a ratio of organic facies: aqueous phase=(1～5): 1, regeneration velocity ratio is
Organic facies: aqueous phase=(5～10): 1；Regenerant solution is to be dissolved in water mixed by regenerative agent by the mass percent of 2～10%
Conjunction uniformly obtains, and regenerative agent is a kind of or the most two or more mixture in sodium carbonate, ammonium carbonate and sodium hydroxide, or
Person is one or both mixture in sulphuric acid and hydrochloric acid.
Compared with prior art, the present invention has a following useful technique effect:
The present invention will contain vanadium solution and use with V5+Or the method that its complex extracting and enriching purifies, the requirement of raw material is wide in range,
Various all can use containing vanadium solution；Generating unit fractional precipitation impurity content be can reduce when pH regulator simultaneously, extraction and later stage alleviated
The remove impurity pressure purified；Can be selected for non-phosphorus-contained extractant, only need to contain vanadium solution and be oxidized to V5+State, avoids the need for the most repeatedly becoming
Changing valence state, reduce operation and energy resource consumption, extraction organic facies saturation is high, up to 50g/L, decreases extraction progression, minimum
Need 2 grades of extractions, substantially increase extraction disposal ability；Extraction yield is up to more than 97.5%, and stripping rate reaches more than 99%, V5+
Equivalent V2O5Concentration can be enriched with and reach 150g/L, V5+Extraction treating capacity is greatly improved, and improves yield, cost-effective.This
The bright vanadium material that will contain leaches, dissolves hydrometallurgy again, with V5+Valence state purification by liquid extraction, enrichment containing vanadium solution, technique is simple, cost
Low, vanadium recovery is high, effect is far superior to V4+Extracting process, have broad application prospects, on vanadium metallurgy industry impact huge
Greatly.
Further, extractant of the present invention does not has absorbability to Fe, and beneficially extraction process purifies.
[detailed description of the invention]
The present invention is to pass through V5+The mode of extraction is by a kind of production technology of vanadium extraction Enrichment purification in vanadium material.
The present invention utilizes V5+Purification by liquid extraction, Vanadium Concentrationin production stage as follows:
One, extraction stock solution is obtained: certain density vanadium-containing material is leached stock solution stirring and adds soda acid adjustment pH value necessarily
Scope after, then low price V ionic oxide formation is V by oxidizer5+, strictly control V4+Concentration, will after precipitate filter, filtrate
It is extraction stock solution；Wherein vanadium-containing material leach stock solution, can be Leaching by strong acid curing liquid, diluted acid leaching liquid, alkaline leaching liquid or in
Property leachate；In stock solution, vanadium can be that various valence state exists；
A, regulation pH value and temperature: vanadium-containing material water logging, acidleach or alkali leached leaches stock solution, the wherein various valencys of V
State, such as the vanadium ion of+5 ,+4 ,+3 and+2, and if all vanadium ions all generate V205Time, V205Concentration control 2～
20g/L, stirring adds pH adjusting agent regulation acidity, and the pH value that vanadium-containing material leaches stock solution controls between 1.3～2.7, adjusts
Joint temperature, between 25～50 DEG C, now can produce precipitation or the floccule of white；
B, oxidation: the solution good by a step process, be added slowly with stirring oxidant (powder or solution) and carry out
Reaction, the color of reaction solution is gradually become crineous from green, and now the vanadium ion in reaction solution is the most all oxidized to V5+,
By detection V4+It is converted into V2O5Concentration terminate when below 1g/L reaction, be aged standby after being sufficiently stirred for.Wherein, oxidant
Comprise: one in hydrogen peroxide, sodium thiosulfate, calcium chlorate, sodium chlorate, potassium chlorate, calcium hypochlorite, postassium hypochlorite and chlorine or
The most two or more mixture；Wherein chlorine is to be passed through, and other oxidant can directly add.
C, filtration: the reaction mass after b process being processed is by filter press or band filter, by precipitate or wadding
Shape thing and solution separating, it is thus achieved that filtrate be extraction stock solution, store for future use, solid dries another use.
Two, adjusting extraction stock solution pH value is 1.3～2.7 (aqueous phase extraction stock solutions), then by extraction organic facies by V5+Extraction
Purification is enriched in organic facies, and major impurity stays in remaining liquid after the extraction, for remaining water, more repeatedly will be enriched in aqueous phase back washing agent
V5+Organic facies back extraction, make V5+It is enriched in strip aqueous, for turning one's coat.
D, the configuration of extraction organic facies: by extractant, synergic reagent and solvent according to 5～30%:2～15%: the matter of surplus
Amount ratio prepares.Concrete volume calculates according to volume of production and volume of equipment；Then regulation temperature and acidity, the same a of acidity regulator
The regulator of step, the overall pH value holding ensureing extraction organic facies and extract stock solution is consistent or close, is also 1.3～2.7, no
Then can cause untoward reaction；Temperature regulation uses steam-heated mode, to extraction stock solution, temperature regulation is kept consistent, storage
Deposit standby.
Wherein extractant is probably: tri-n-octyl amine (TOA), trioctylamine, Mextral 54-100, N235 (7301),
A kind of or the most two or more mixture of Alamine336, N263, N1923, HBL101 and P507 etc.；Synergic reagent mainly wraps
Include: n-octyl alcohol, isooctanol, sec-octyl alcohol or tributyl phosphate (TBP)；Solvent (diluent) including: solvent kerosene, sulfonated kerosene,
A kind of or the most two or more mixture in benzene, chloroform or 2 one ethyl hexanols；
Extraction stock solution during vanadium-containing material leaches stock solution, step 2 in the step one of the present invention and the pH value of extraction organic facies
All being regulated by pH value regulator, extraction stock solution pH adjusting agent includes: sulphuric acid, hydrochloric acid, nitric acid, sodium hydroxide, potassium hydroxide, oxygen
Change a kind of or the most two or more mixing in calcium, calcium hydroxide, magnesium carbonate, sodium carbonate and natural whiting stone powder etc.
Thing.
E, the configuration of back washing agent solution: back washing agent is dissolved in water by the mass percent of 2～15%, stirs i.e.
Can.
Back washing agent comprise the one in sodium hydroxide/potassium, sodium carbonate/potassium, sodium bicarbonate/potassium, sodium oxide and potassium oxide or
The most two or more mixture, or a kind of or the most two or more mixture of sulphuric acid, hydrochloric acid and nitric acid；
F, the configuration of regenerant solution of extraction organic facies: regenerative agent is dissolved in water by the mass percent of 2～10%
In, stir.Regenerative agent is a kind of or the most two or more mixing in sodium carbonate, ammonium carbonate and sodium hydroxide
Thing, or be a kind of in sulphuric acid and hydrochloric acid or both mixture.
G, extraction: take the mode (aqueous phase and organic facies reverse flow extraction) of counter-current extraction, selected extraction progression be 2～
4 grades, extraction phase ratio (connects ratio): organic facies (O): aqueous phase (A)=1:(1～5)；Effusion meter is set, extract stream speed ratio by flow ratio:
Organic facies (O): aqueous phase (A)=1:(1～5)；Extraction is no less than 3 minutes time of contact；
Back extraction progression is 2～5 grades, and back extraction is compared: organic facies (O): aqueous phase (A)=(1～5): 1；Back extraction velocity ratio is:
Organic facies (O): aqueous phase (A)=(1～5): 1；Back extraction is no less than 5 minutes time of contact；
Extraction organic facies regeneration progression is 1～2 grade, and regeneration is in a ratio of: organic facies (O): aqueous phase (A)=(1～5): 1；Stream
Ratio is: organic facies (O): aqueous phase (A)=(5～10): 1；Regeneration is no less than 5 minutes time of contact.
1. extraction organic be harmonious, extract stock solution, back washing agent, regenerant solution carry out filling out groove according to the set ratio that connects: unlatching
Extraction operation, extracts water more than the extraction that stock solution becomes faint yellow or colourless after the extraction organic extractant phase that pH value is 1.3～2.7
(Yu Shui), the V in extraction stock solution5+Enter in extraction organic facies, it is thus achieved that enrichment V5+Organic facies；As V in the remaining water of extraction2O5% <
Water can be immediately discharged to after 0.5g/L process；Extraction process temperature is 25～50 DEG C.
2. V it is enriched with5+Organic facies carry out back extraction process by back washing agent solution, it is thus achieved that enrichment V5+Turn one's coat after store,
To utilizing V5+Extracting and enriching contains vanadium solution；Concentration enrichment reaches equivalent V2O5Concentration be 30～150g/L directly be available for use routine
The operations such as remove impurity, purification, dephosphorization, precipitation use.
3. the extraction organic facies after back extraction processes is regenerated by regenerant solution, and the extraction of backflowing of the organic facies after regeneration has
Machine phase storage tank recycles, and periodically supplements by waste.
Extraction controls: in extraction process, and timing is observed extraction two-phase laminated flow situation, controlled the height of profit liquid level, observes
The production of three-phase thing, detection controls the temperature of extraction liquids and pH value well, otherwise there will be profit be difficult to separate, organic facies
The bad phenomenon such as caking, remaining water content of vanadium are higher.
Embodiment one:
A adjusts: will leach the solution (the various valence states of V) being about 5g/L containing vanadium with the acid solution that pH value is 1, constantly
Stirring, with the aqueous solution that mass concentration is 20% sodium carbonate, by pH regulator to 1.6, adjusts the temperature to 40 DEG C, now in solution
Can gradually produce precipitation or the floccule of partial white；
B aoxidizes: being added slowly with stirring oxidant sodium chlorate and carry out oxidation reaction, reaction solution is by initial light green
After gradually becoming crineous eventually, detect V4+It is converted into V2O5Concentration terminate when below 0.05g/L reaction, be sufficiently stirred for after the most quiet
Only ageing.
C filters: the filter press of the reaction mass after b process being processed filters, by precipitate or floccule and solution
Separating, liquid is extraction stock solution, the pH value of extraction stock solution is adjusted to 1.6, stores for future use；Solid dries and utilizes separately.
The configuration of d extraction organic facies: extractant is tri-n-octyl amine (TOA)；Synergic reagent is TBP；Solvent is sulfonated kerosene 260
Number.By extractant, synergic reagent and solvent according to mass ratio 15%:5%:80% configuration extraction organic facies, concrete volume according to
Volume of production and volume of equipment calculate；Then regulation temperature is 40 DEG C, and regulation pH value is 1.6.
The configuration of e back washing agent solution: preparation mass concentration is the sodium carbonate liquor of 5%, and temperature is with extracting organic facies.
The configuration of f regenerant solution: preparation mass concentration is the aqueous sulfuric acid of 5%, and temperature is with extracting organic facies.
G extracts: take the mode of counter-current extraction, and selected extraction progression is 2 grades, will extraction organic facies, extraction stock solution, back extraction
Agent, regenerant solution carry out filling out groove according to the set ratio that connects: extraction phase compares: organic facies (O): aqueous phase (A)=1:3；According to organic
Phase (O): the good flow of flow set of aqueous phase (A)=1:3, extraction time of contact be 10 minutes；Back extraction progression is 3 grades, back extraction
It is in a ratio of: organic facies (O): aqueous phase (A)=3:1, according to organic facies (O): the good flow of flow set of aqueous phase (A)=3:1, back extraction
Taking time of contact is 15 minutes；Opening extraction operation, it is (remaining that extraction stock solution becomes water more than faint yellow or colourless extraction after extraction
Water), as V in the remaining water of extraction2O5% < can be immediately discharged to cesspool, strip aqueous enrichment V after 0.5g/L5+Rear storage, extraction yield
Up to 98.3%, stripping rate reaches 99.2%.
Organic facies regeneration after back extraction: regeneration progression is 1 grade, and regeneration is in a ratio of: organic facies (O): aqueous phase (A)=3:1；Stream
Ratio is: organic facies (O): aqueous phase (A)=5:1, regeneration time of contact be 15 minutes；Organic facies after regeneration returns organic facies storage
Groove, recycling, is periodically supplemented by loss.
Strip aqueous uses: concentration of turning one's coat reaches 30～150g/L and i.e. can be directly used for vanadium extraction subsequent purification, dephosphorization, heavy
The operations such as vanadium use.
Embodiment two:
A adjusts: will go out the solution containing vanadium about 10g/L (the various valence states of V) that pH value is about 7, constantly with water logging
Stirring, with the sulfuric acid solution of pH=1 by stock solution pH adjust 1.9, now solution can gradually produce partial white precipitation or
Floccule；Adjust the temperature to 45 DEG C；
B aoxidizes: is added slowly with stirring oxidant potassium chlorate and carries out oxidation reaction, and the color of observing response solution becomes,
Eventually become crineous, detect V4+It is converted into V2O5Concentration terminate when below 0.4g/L reaction, be sufficiently stirred for after static the oldest
Change.
C filters: precipitate or floccule, by band filter, are divided by the reaction mass after b process being processed with solution
From, liquid is extraction stock solution, the pH value of extraction stock solution is adjusted to 1.9, stores for future use；Solid dries manages use separately.
The configuration of d extraction organic facies: extractant is HBL01；Synergic reagent is sec-octyl alcohol；Solvent is sulfonated kerosene 260.Will
Extractant, synergic reagent and solvent are according to mass ratio 15%:10%:75% configuration extraction organic facies, and concrete volume is according to production
Amount and volume of equipment calculate；Then regulation temperature is 45 DEG C, and regulation pH value is 1.9.
The configuration of e back washing agent solution: preparation mass concentration is the back washing agent solution of 2%, and back washing agent uses sodium carbonate and carbon
The mixture of acid potassium arbitrary proportion, temperature is with extracting organic facies.
The configuration of f regenerant solution: preparation mass concentration is the regenerative agent aqueous solution of 2%, and regenerative agent uses sulphuric acid and salt
The mixture of acid arbitrary proportion, temperature is with extracting organic facies.
G extracts: take the mode of counter-current extraction, and selected extraction progression is 3 grades, will extraction organic facies, extraction stock solution, back extraction
Agent, regenerant solution carry out filling out groove according to the set ratio that connects: extraction phase compares: organic facies (O): aqueous phase (A)=1:2；According to organic
Phase (O): the good flow of flow set of aqueous phase (A)=1:3, extraction time of contact be 5 minutes；Back extraction progression is 4 grades, back extraction phase
Ratio is: organic facies (O): aqueous phase (A)=2:1, according to organic facies (O): the good flow of flow set of aqueous phase (A)=2:1, back extraction
Time of contact is 8 minutes；Opening extraction operation, it is (remaining that extraction stock solution becomes water more than faint yellow or colourless extraction after extraction
Water), as V in the remaining water of extraction2O5% < can be immediately discharged to cesspool, strip aqueous enrichment V after 0.5g/L5+Rear storage, qualified instead
Water i.e. can be directly used for the operations such as purification, dephosphorization, precipitation and uses, and extraction yield is up to 98.6%, and stripping rate reaches 99%.
Organic facies regeneration after back extraction: regeneration progression is 1 grade, and regeneration is in a ratio of: organic facies (O): aqueous phase (A)=2:1；Stream
Ratio is: organic facies (O): aqueous phase (A)=8:1, regeneration time of contact be 8 minutes；Organic facies after regeneration returns organic facies storage tank,
Recycling, is periodically supplemented by loss.
Embodiment three:
A adjusts: by the solution containing vanadium 2g/L (the various valence states of V) that the pH value leached with alkali is 11, be stirred continuously,
Salpeter solution and sodium hydroxide solution with pH=1 coordinate simultaneously, are controlled by pH 2.0, now meeting gradually generating unit in solution
Divide precipitation or the floccule of white；Adjust the temperature to 50 DEG C；
B aoxidizes: is added slowly with stirring oxidant sodium thiosulfate and carries out oxidation reaction, the color of observing response solution
Become, eventually become pompeian red or crineous, detect V4+It is converted into V2O5Concentration terminate when below 1g/L reaction, solution simultaneously
The middle precipitation that can produce white or floccule, static ageing after being sufficiently stirred for.
C filters: precipitate or floccule, by band filter, are divided by the reaction mass after b process being processed with solution
From, liquid is extraction stock solution, the pH value of extraction stock solution is adjusted to 2.0, stores for future use；Solid dries and utilizes separately.
The configuration of d extraction organic facies: extractant is N263；Synergic reagent is n-octyl alcohol；Solvent is sulfonated kerosene 260.Will
Extractant, synergic reagent and solvent are according to mass ratio 10%:5%:85% configuration extraction organic facies, and then regulation temperature is 50
DEG C, regulation pH value is 2.
The configuration of e back washing agent solution: preparation mass concentration is the sodium hydroxide solution of 8%, and temperature is with extracting organic facies.
The configuration of f regenerant solution: preparation mass concentration is the aqueous sulfuric acid of 8%, and temperature is with extracting organic facies.
G extracts: take the mode of counter-current extraction, and selected extraction progression is 3 grades, will extraction organic facies, extraction stock solution, back extraction
Agent, regenerant solution carry out filling out groove according to the set ratio that connects: extraction phase compares: organic facies (O): aqueous phase (A)=1:4；According to organic
Phase (O): the good flow of flow set of aqueous phase (A)=1:3, extraction time of contact be 8 minutes；Back extraction progression is 3 grades, back extraction phase
Ratio is: organic facies (O): aqueous phase (A)=4:1, according to organic facies (O): the good flow of flow set of aqueous phase (A)=4:1, back extraction
Time of contact is 11 minutes；Opening extraction operation, it is (remaining that extraction stock solution becomes water more than faint yellow or colourless extraction after extraction
Water), as V in the remaining water of extraction2O5% < can be immediately discharged to cesspool, strip aqueous enrichment V after 0.5g/L5+Rear storage, qualified instead
Water is directly available for the operations such as purification, dephosphorization, precipitation and uses, and extraction yield is up to 99%, and stripping rate reaches 99.4%.
Organic facies regeneration after back extraction: regeneration progression is 1 grade, and regeneration is in a ratio of: organic facies (O): aqueous phase (A)=5:1；Stream
Ratio is: organic facies (O): aqueous phase (A)=10:1, regeneration time of contact be 11 minutes；Organic facies after regeneration returns organic facies storage
Groove, recycling, is periodically supplemented by loss.
Embodiment four:
A adjusts: by the solution containing vanadium 15g/L (the various valence states of V) that the pH value leached with alkali is 11, constantly stir
Mix, coordinate with hydrochloric acid solution and salpeter solution and aqua calcis simultaneously, pH is controlled 1.3, now can be by solution
Gradually produce precipitation or the floccule of partial white；Adjust the temperature to 35 DEG C；
B aoxidizes: be added slowly with stirring oxidant hypochlorous acid's calcium, and is passed through chlorine and carries out oxidation reaction, observing response
The color of solution becomes, and eventually becomes pompeian red or crineous, detects V4+It is converted into V2O5Concentration terminate when below 0.8g/L
Reaction, can produce precipitation or the floccule of white, static ageing after being sufficiently stirred for simultaneously in solution.
C filters: precipitate or floccule, by band filter, are divided by the reaction mass after b process being processed with solution
From, liquid is extraction stock solution, the pH value of extraction stock solution is adjusted to 1.3, stores for future use；Solid dries and utilizes separately.
The configuration of d extraction organic facies: extractant is N1923；Synergic reagent is n-octyl alcohol；Solvent is solvent kerosene.Will extraction
Agent, synergic reagent and solvent are according to mass ratio 30%:10%:60% configuration extraction organic facies, and then regulation temperature is 35 DEG C, adjusts
Joint pH value is 1.3.
The configuration of e back washing agent solution: preparation mass concentration is the potassium oxide solution of 4%, and temperature is with extracting organic facies.
The configuration of f regenerant solution: preparation mass concentration is the aqueous hydrochloric acid solution of 4%, and temperature is with extracting organic facies.
G extracts: take the mode of counter-current extraction, and selected extraction progression is 3 grades, will extraction organic facies, extraction stock solution, back extraction
Agent, regenerant solution carry out filling out groove according to the set ratio that connects: extraction phase compares: organic facies (O): aqueous phase (A)=1:1；According to organic
Phase (O): the good flow of flow set of aqueous phase (A)=1:1, extraction time of contact be 12 minutes；Back extraction progression is 2 grades, back extraction
It is in a ratio of: organic facies (O): aqueous phase (A)=1:1, according to organic facies (O): the good flow of flow set of aqueous phase (A)=1:1, back extraction
Taking time of contact is 15 minutes；Opening extraction operation, it is (remaining that extraction stock solution becomes water more than faint yellow or colourless extraction after extraction
Water), as V in the remaining water of extraction2O5% < can be immediately discharged to cesspool, strip aqueous enrichment V after 0.5g/L5+Rear storage, qualified instead
Water is directly available for the operations such as purification, dephosphorization, precipitation and uses, and extraction yield is up to 98.5%, and stripping rate reaches 99.1%.
Organic facies regeneration after back extraction: regeneration progression is 1 grade, and regeneration is in a ratio of: organic facies (O): aqueous phase (A)=1:1；Stream
Ratio is: organic facies (O): aqueous phase (A)=6:1, regeneration time of contact be 15 minutes；Organic facies after regeneration returns organic facies storage
Groove, recycling, is periodically supplemented by loss.
Embodiment five:
A adjusts: by the solution containing vanadium 20g/L (the various valence states of V) that the pH value leached with alkali is 11, constantly stir
Mix, with hydrochloric acid solution, pH is controlled 2.2, solution now can gradually produce precipitation or the floccule of partial white；Regulation temperature
Degree is to 30 DEG C；
B aoxidizes: is added slowly with stirring oxidant calcium chlorate, sodium chlorate and potassium chlorate and enters with the mixture of arbitrary proportion
Row oxidation reaction, the color of observing response solution becomes, and eventually becomes pompeian red or crineous, detects V4+It is converted into V2O5Concentration
Terminate reaction when below 0.6g/L, solution can produce precipitation or the floccule of white, static ageing after being sufficiently stirred for simultaneously.
C filters: precipitate or floccule, by band filter, are divided by the reaction mass after b process being processed with solution
From, liquid is extraction stock solution, the pH value of extraction stock solution is adjusted to 2.2, stores for future use；Solid dries and utilizes separately.
The configuration of d extraction organic facies: extractant is P507；Synergic reagent is n-octyl alcohol；Solvent is solvent kerosene.Will extraction
Agent, synergic reagent and solvent are according to mass ratio 25%:2%:73% configuration extraction organic facies, and then regulation temperature is 30 DEG C, adjusts
Joint pH value is 2.2.
The configuration of e back washing agent solution: preparation mass concentration is the sulfuric acid solution of 6%, and temperature is with extracting organic facies.
The configuration of f regenerant solution: preparation mass concentration is the regenerative agent aqueous solution of 6%, and regenerative agent is sodium carbonate and carbon
Acid ammonium is with the mixture of arbitrary proportion；Temperature is with extracting organic facies.
G extracts: take the mode of counter-current extraction, and selected extraction progression is 2 grades, will extraction organic facies, extraction stock solution, back extraction
Agent, regenerant solution carry out filling out groove according to the set ratio that connects: extraction phase compares: organic facies (O): aqueous phase (A)=1:5；According to organic
Phase (O): the good flow of flow set of aqueous phase (A)=1:5, extraction time of contact be 15 minutes；Back extraction progression is 2 grades, back extraction
It is in a ratio of: organic facies (O): aqueous phase (A)=5:1, according to organic facies (O): the good flow of flow set of aqueous phase (A)=5:1, back extraction
Taking time of contact is 18 minutes；Opening extraction operation, it is (remaining that extraction stock solution becomes water more than faint yellow or colourless extraction after extraction
Water), as V in the remaining water of extraction2O5% < can be immediately discharged to cesspool, strip aqueous enrichment V after 0.5g/L5+Rear storage, qualified instead
Water is directly available for the operations such as purification, dephosphorization, precipitation and uses, and extraction yield is up to 97.5%, and stripping rate reaches 99.2%.
Organic facies regeneration after back extraction: regeneration progression is 1 grade, and regeneration is in a ratio of: organic facies (O): aqueous phase (A)=4:1；Stream
Ratio is: organic facies (O): aqueous phase (A)=7:1, regeneration time of contact be 18 minutes；Organic facies after regeneration returns organic facies storage
Groove, recycling, is periodically supplemented by loss.
Embodiment six:
A adjusts: by the solution containing vanadium 6g/L (the various valence states of V) that the pH value leached with alkali is 11, be stirred continuously,
Coordinating with hydrochloric acid solution and natural whiting stone powder controls 1.5 by pH, now can gradually produce partial white in solution
Precipitation or floccule；Adjust the temperature to 25 DEG C；
B aoxidizes: be added slowly with stirring oxidant hypochlorous acid's calcium, postassium hypochlorite carries out oxygen with the mixture of arbitrary proportion
Changing reaction, the color of observing response solution becomes, and eventually becomes pompeian red or crineous, detects V4+It is converted into V2O5Concentration exist
Terminate reaction during below 0.7g/L, solution can produce precipitation or the floccule of white, static ageing after being sufficiently stirred for simultaneously.
C filters: precipitate or floccule, by filter press, are divided by the reaction mass after b process being processed with solution
From, liquid is extraction stock solution, the pH value of extraction stock solution is adjusted to 1.5, stores for future use；Solid dries and utilizes separately.
The configuration of d extraction organic facies: extractant is 7301；Synergic reagent is isooctanol；Solvent is benzene.By extractant, association's extraction
Agent and solvent are according to mass ratio 5%:3%:92% configuration extraction organic facies, and then regulation temperature is 25 DEG C, and regulation pH value is
1.5。
The configuration of e back washing agent solution: preparation mass concentration is the hydrochloric acid solution of 10%, and temperature is with extracting organic facies.
The configuration of f regenerant solution: preparation mass concentration is the ammonium carbonate solution of 10%, and temperature is with extracting organic facies.
G extracts: take the mode of counter-current extraction, and selected extraction progression is 2 grades, will extraction organic facies, extraction stock solution, back extraction
Agent, regenerant solution carry out filling out groove according to the set ratio that connects: extraction phase compares: organic facies (O): aqueous phase (A)=1:2；According to organic
Phase (O): the good flow of flow set of aqueous phase (A)=1:2, extraction time of contact be 9 minutes；Back extraction progression is 2 grades, back extraction phase
Ratio is: organic facies (O): aqueous phase (A)=2:1, according to organic facies (O): the good flow of flow set of aqueous phase (A)=2:1, back extraction
Time of contact is 10 minutes；Opening extraction operation, it is (remaining that extraction stock solution becomes water more than faint yellow or colourless extraction after extraction
Water), as V in the remaining water of extraction2O5% < can be immediately discharged to cesspool, strip aqueous enrichment V after 0.5g/L5+Rear storage, qualified instead
Water is directly available for the operations such as purification, dephosphorization, precipitation and uses, and extraction yield is up to 98%, and stripping rate reaches 99.1%.
Organic facies regeneration after back extraction: regeneration progression is 2 grades, and regeneration is in a ratio of: organic facies (O): aqueous phase (A)=2:1；Stream
Ratio is: organic facies (O): aqueous phase (A)=9:1, regeneration time of contact be 10 minutes；Organic facies after regeneration returns organic facies storage
Groove, recycling, is periodically supplemented by loss.
Embodiment seven:
A adjusts: by the solution containing vanadium 8g/L (the various valence states of V) that the pH value leached with alkali is 11, be stirred continuously,
Coordinating with sulfuric acid solution, hydrochloric acid solution, salpeter solution and calcium oxide controls 2.7 by pH, now meeting gradually generating unit in solution
Divide precipitation or the floccule of white；Adjust the temperature to 28 DEG C；
B aoxidizes: be added slowly with stirring oxidant sodium thiosulfate, calcium chlorate, sodium chlorate and postassium hypochlorite with arbitrarily
The mixture of ratio carries out oxidation reaction, and the color of observing response solution becomes, and eventually becomes pompeian red or crineous, detects V4+Folding
It is combined into V2O5Concentration terminate when below 0.5g/L reaction, solution can produce simultaneously white precipitation or floccule, fully stir
Static ageing after mixing.
C filters: precipitate or floccule, by filter press, are divided by the reaction mass after b process being processed with solution
From, liquid is extraction stock solution, the pH value of extraction stock solution is adjusted to 2.7, stores for future use；Solid dries and utilizes separately.
The configuration of d extraction organic facies: extractant is N263, N1923, HBL101 and P507 mixture with arbitrary proportion；
Synergic reagent is isooctanol；Solvent is chloroform.Extractant, synergic reagent and solvent are configured according to mass ratio 20%:15%:65%
Extraction organic facies, then regulation temperature is 28 DEG C, and regulation pH value is 2.7.
The configuration of e back washing agent solution: preparation mass concentration is the back washing agent solution of 12%, and back washing agent is sodium carbonate, carbonic acid
Potassium, sodium bicarbonate and potassium bicarbonate are with the mixture of arbitrary proportion, and temperature is with extracting organic facies.
The configuration of f regenerant solution: preparation mass concentration is the hydrochloric acid solution of 12%, and temperature is with extracting organic facies.
G extracts: take the mode of counter-current extraction, and selected extraction progression is 4 grades, will extraction organic facies, extraction stock solution, back extraction
Agent, regenerant solution carry out filling out groove according to the set ratio that connects: extraction phase compares: organic facies (O): aqueous phase (A)=1:2.5；According to having
Machine phase (O): the good flow of flow set of aqueous phase (A)=1:2.5, extraction time of contact be 6 minutes；Back extraction progression is 3 grades, back extraction
Take and be in a ratio of: organic facies (O): aqueous phase (A)=2.5:1, according to organic facies (O): the flow set of aqueous phase (A)=2.5:1 flows well
Amount, back extraction time of contact is 8 minutes；Opening extraction operation, extraction stock solution becomes faint yellow or colourless extraction after extraction
Yu Shui (Yu Shui), as V in the remaining water of extraction2O5% < can be immediately discharged to cesspool, strip aqueous enrichment V after 0.5g/L5+Rear storage
Depositing, qualified operations such as being directly available for purification, dephosphorization, precipitation of turning one's coat uses, and extraction yield is up to 98.3%, and stripping rate reaches
99.1%.
Organic facies regeneration after back extraction: regeneration progression is 2 grades, and regeneration is in a ratio of: organic facies (O): aqueous phase (A)=2.5:1；
Flow ratio is: organic facies (O): aqueous phase (A)=5.5:1, regeneration time of contact be 8 minutes；Organic facies after regeneration returns organic facies
Storage tank, recycling, is periodically supplemented by loss.
Embodiment eight:
A adjusts: by the solution containing vanadium 12g/L (the various valence states of V) that the pH value leached with alkali is 11, constantly stir
Mix, coordinate with sulfuric acid solution and potassium hydroxide and pH is controlled 2.4, now solution can gradually produce partial white precipitation or
Floccule；Adjust the temperature to 32 DEG C；
B aoxidizes: is added slowly with stirring oxidant hydrogen peroxide and carries out oxidation reaction, and the color of observing response solution becomes,
Eventually become pompeian red or crineous, detect V4+It is converted into V2O5Concentration terminate when below 1g/L reaction, simultaneously in solution
Precipitation or the floccule of white, static ageing after being sufficiently stirred for can be produced.
C filters: precipitate or floccule, by filter press, are divided by the reaction mass after b process being processed with solution
From, liquid is extraction stock solution, the pH value of extraction stock solution is adjusted to 2.4, stores for future use；Solid dries and utilizes separately.
The configuration of d extraction organic facies: extractant is Mextral 54-100 and the N235 mixture with arbitrary proportion；Association's extraction
Agent is isooctanol；Solvent is 2 one ethyl hexanols.Extractant, synergic reagent and solvent are joined according to mass ratio 12%:6%:82%
Putting extraction organic facies, then regulation temperature is 32 DEG C, and regulation pH value is 2.4.
The configuration of e back washing agent solution: preparation mass concentration is the potassium bicarbonate solution of 14%, and temperature is with extracting organic facies.
The configuration of f regenerant solution: preparation mass concentration is the hydrochloric acid solution of 14%, and temperature is with extracting organic facies.
G extracts: take the mode of counter-current extraction, and selected extraction progression is 4 grades, will extraction organic facies, extraction stock solution, back extraction
Agent, regenerant solution carry out filling out groove according to the set ratio that connects: extraction phase compares: organic facies (O): aqueous phase (A)=1:3.5；According to having
Machine phase (O): the good flow of flow set of aqueous phase (A)=1:3.5, extraction time of contact be 3 minutes；Back extraction progression is 4 grades, back extraction
Take and be in a ratio of: organic facies (O): aqueous phase (A)=3.5:1, according to organic facies (O): the flow set of aqueous phase (A)=6.5:1 flows well
Amount, back extraction time of contact is 5 minutes；Opening extraction operation, extraction stock solution becomes faint yellow or colourless extraction after extraction
Yu Shui (Yu Shui), as V in the remaining water of extraction2O5% < can be immediately discharged to cesspool, strip aqueous enrichment V after 0.5g/L5+Rear storage
Depositing, qualified operations such as being directly available for purification, dephosphorization, precipitation of turning one's coat uses, and extraction yield is up to 98.8%, and stripping rate reaches
99%.
Organic facies regeneration after back extraction: regeneration progression is 2 grades, and regeneration is in a ratio of: organic facies (O): aqueous phase (A)=3.5:1；
Flow ratio is: organic facies (O): aqueous phase (A)=6.5:1, regeneration time of contact be 5 minutes；Organic facies after regeneration returns organic facies
Storage tank, recycling, is periodically supplemented by loss.
Embodiment nine:
A adjusts: by the solution containing vanadium 16g/L (the various valence states of V) that the pH value leached with alkali is 11, constantly stir
Mix, coordinate with sulfuric acid solution and magnesium carbonate solution and pH is controlled 2.5, solution now can gradually produce the precipitation of partial white
Or floccule；Adjust the temperature to 44 DEG C；
B aoxidizes: is under agitation slowly introducing oxidant chlorine and carries out oxidation reaction, and the color of observing response solution becomes,
Become pompeian red or crineous eventually, detect V4+It is converted into V2O5Concentration terminate when below 1g/L reaction, meeting in solution simultaneously
Produce precipitation or the floccule of white, static ageing after being sufficiently stirred for.
C filters: precipitate or floccule, by filter press, are divided by the reaction mass after b process being processed with solution
From, liquid is extraction stock solution, the pH value of extraction stock solution is adjusted to 2.5, stores for future use；Solid dries and utilizes separately.
The configuration of d extraction organic facies: extractant is trioctylamine；Synergic reagent is TBP；Solvent is solvent kerosene and sulfonated kerosene
Mixture with arbitrary proportion.Extractant, synergic reagent and solvent is organic according to mass ratio 16%:9%:75% configuration extraction
Phase, then regulation temperature is 44 DEG C, and regulation pH value is 2.5.
The configuration of e back washing agent solution: preparation mass concentration is the back washing agent solution of 15%, back washing agent be hydrochloric acid and nitric acid with
The mixture of arbitrary proportion；Temperature is with extracting organic facies.
The configuration of f regenerant solution: preparation mass concentration is the regenerant solution of 15%, and regenerative agent is sodium carbonate, carbonic acid
Ammonium and sodium hydroxide are with the mixture of arbitrary proportion；Temperature is with extracting organic facies.
G extracts: take the mode of counter-current extraction, and selected extraction progression is 4 grades, will extraction organic facies, extraction stock solution, back extraction
Agent, regenerant solution carry out filling out groove according to the set ratio that connects: extraction phase compares: organic facies (O): aqueous phase (A)=1:4.5；According to having
Machine phase (O): the good flow of flow set of aqueous phase (A)=1:4.5, extraction time of contact be 4 minutes；Back extraction progression is 4 grades, back extraction
Take and be in a ratio of: organic facies (O): aqueous phase (A)=4.5:1, according to organic facies (O): the flow set of aqueous phase (A)=4.5:1 flows well
Amount, back extraction time of contact is 6 minutes；Opening extraction operation, extraction stock solution becomes faint yellow or colourless extraction after extraction
Yu Shui (Yu Shui), as V in the remaining water of extraction2O5% < can be immediately discharged to cesspool, strip aqueous enrichment V after 0.5g/L5+Rear storage
Depositing, qualified operations such as being directly available for purification, dephosphorization, precipitation of turning one's coat uses, and extraction yield is up to 99.2%, and stripping rate reaches
99.5%.
Organic facies regeneration after back extraction: regeneration progression is 2 grades, and regeneration is in a ratio of: organic facies (O): aqueous phase (A)=4.5:1；
Flow ratio is: organic facies (O): aqueous phase (A)=7.5:1, regeneration time of contact be 6 minutes；Organic facies after regeneration returns organic facies
Storage tank, recycling, is periodically supplemented by loss.
Embodiment ten:
A adjusts: by the solution containing vanadium 14g/L (the various valence states of V) that the pH value leached with alkali is 11, constantly stir
Mix, with salpeter solution, pH is controlled 1.8, solution now can gradually produce precipitation or the floccule of partial white；Regulation temperature
Degree is to 36 DEG C；
B aoxidizes: is added slowly with stirring oxidant sodium thiosulfate and carries out oxidation reaction, the color of observing response solution
Become, eventually become pompeian red or crineous, detect V4+It is converted into V2O5Concentration terminate when below 1g/L reaction, solution simultaneously
The middle precipitation that can produce white or floccule, static ageing after being sufficiently stirred for.
C filters: precipitate or floccule, by filter press, are divided by the reaction mass after b process being processed with solution
From, liquid is extraction stock solution, the pH value of extraction stock solution is adjusted to 1.8, stores for future use；Solid dries and utilizes separately.
The configuration of d extraction organic facies: extractant is Alamine 336, N263 and the N1923 mixture with arbitrary proportion；
Synergic reagent is sec-octyl alcohol；Solvent is benzene, chloroform and the 2 one ethyl hexanols mixture with arbitrary proportion.By extractant, synergic reagent and
Solvent is according to mass ratio 18%:12%:70% configuration extraction organic facies, and then regulation temperature is 36 DEG C, and regulation pH value is
1.8。
The configuration of e back washing agent solution: preparation mass concentration is the potassium hydroxide solution of 9%, and temperature is with extracting organic facies.
The configuration of f regenerant solution: preparation mass concentration is the sulfuric acid solution of 15%, and temperature is with extracting organic facies.
G extracts: take the mode of counter-current extraction, and selected extraction progression is 4 grades, will extraction organic facies, extraction stock solution, back extraction
Agent, regenerant solution carry out filling out groove according to the set ratio that connects: extraction phase compares: organic facies (O): aqueous phase (A)=1:1.5；According to having
Machine phase (O): the good flow of flow set of aqueous phase (A)=1:1.5, extraction time of contact be 7 minutes；Back extraction progression is 4 grades, back extraction
Take and be in a ratio of: organic facies (O): aqueous phase (A)=1.5:1, according to organic facies (O): the flow set of aqueous phase (A)=1.5:1 flows well
Amount, back extraction time of contact is 10 minutes；Opening extraction operation, extraction stock solution becomes faint yellow or colourless extraction after extraction
Yu Shui (Yu Shui), as V in the remaining water of extraction2O5% < can be immediately discharged to cesspool, strip aqueous enrichment V after 0.5g/L5+Rear storage
Depositing, qualified operations such as being directly available for purification, dephosphorization, precipitation of turning one's coat uses, and extraction yield is up to 99.3%, and stripping rate reaches
99.5%.
Organic facies regeneration after back extraction: regeneration progression is 2 grades, and regeneration is in a ratio of: organic facies (O): aqueous phase (A)=1.5:1；
Flow ratio is: organic facies (O): aqueous phase (A)=8.5:1, regeneration time of contact be 10 minutes；Organic facies after regeneration returns organic facies
Storage tank, recycling, is periodically supplemented by loss.
The use of strip aqueous: qualified operations such as i.e. can be directly used for vanadium extraction subsequent purification, dephosphorization, precipitation of turning one's coat makes
With.
The present invention leaches stock solution acidity and vanadium ion concentration according to vanadium-containing material, under agitation by containing vanadium thing
Material leaches stock solution oxidizer or ventilation body and acid adding, alkali, adjustment tetravalence vanadium 0--2g/L, pH value 1.3～2.7 scope
In, temperature is 25～50 DEG C, by naturally clarifying or overanxious clay content reduces and be less than 0.03%.What clay content was high can be again
Separating, the pretreated stillness of night or filtrate are extraction stock solution；Then with extractant: synergic reagent: solvent=5～30%:2
～15%: the extraction organic extractant phase of surplus quality proportioning, by V5+Purification by liquid extraction, be enriched in extraction organic facies in, extraction yield is big
In 97.5%, impurity is mainly by taking away (Yu Shui), then with the aqueous phase back extraction containing back washing agent 2-15% in the stock solution after extraction
Liquid will be enriched in V repeatedly5+Full have back extraction, makes V5+It is enriched in strip aqueous (turning one's coat)；Wait to turn one's coat and be enriched to equivalent V2O5Concentration
During for 30-150g/L, can be used as the remove impurity of routine, purification, the raw material of precipitation operation.The technique of the present invention takes V5+Extraction
Method, overcomes V4+Valence state changes repeatedly, extractant saturation is low in extraction, the extraction shortcomings such as progression is many, impurity F e should not separate.
This extraction process low cost, simple and reliable, the extraction yield of vanadium can >=97.5%, stripping rate reaches more than 99%, clean and safe
Environmental protection, sewage is recycled into use, and effect is far superior to V4+Extracting process, on vanadium metallurgy industry impact huge, have wide
Application prospect.
Claims (10)
1. one kind utilizes V5+The extracting and enriching method containing vanadium solution, it is characterised in that: comprise the following steps:
(1) pH value that vanadium-containing material leaches stock solution regulates below 7, generates precipitation or floccule, the most under agitation
Adding oxidant to react, reaction solution gradually becomes crineous, and now the vanadium ion in reaction solution is oxidized to V5+, filter
Reaction solution, it is thus achieved that filtrate for extraction stock solution；
(2) pH value of extraction stock solution is regulated below 7, then use the extraction organic facies that pH value is equal with extraction stock solution pH value to incite somebody to action
V in extraction stock solution5+Carry out counter-current extraction, it is thus achieved that enrichment V5+Organic facies and the remaining water of extraction, V will be enriched with5+Organic communicate
Cross back washing agent solution and carry out back extraction process, it is thus achieved that enrichment V5+Turn one's coat and store, be obtained by V5+Extracting and enriching contains vanadium solution；
Wherein, by mass percentage, extraction organic facies is composed of the following components: 5～the extractant of 30%, 2～the association of 15%
Extraction agent, surplus is solvent.
One the most according to claim 1 utilizes V5+The extracting and enriching method containing vanadium solution, it is characterised in that: step (1)
Vanadium-containing material leach in stock solution the vanadium ion containing+5 ,+4 ,+3 and+2, and if all vanadium ions all generate V205Time,
V205Concentration is 2g/L～20g/L.
One the most according to claim 1 utilizes V5+The extracting and enriching method containing vanadium solution, it is characterised in that: step (1)
In oxidant include hydrogen peroxide, sodium thiosulfate, calcium chlorate, sodium chlorate, potassium chlorate, calcium hypochlorite, postassium hypochlorite and chlorine
In a kind of or the most two or more mixture.
One the most according to claim 1 utilizes V5+The extracting and enriching method containing vanadium solution, it is characterised in that: step (1)
Middle oxidation is until detecting V4+It is converted into V2O5Concentration terminate when below 1g/L.
One the most according to claim 1 utilizes V5+The extracting and enriching method containing vanadium solution, it is characterised in that: step (1)
Middle vanadium-containing material is leached the pH value of the extraction stock solution in stock solution, step (2) and extraction organic facies and is all regulated by pH value regulator
Being 1.3～2.7, pH value regulator includes: sulphuric acid, hydrochloric acid, nitric acid, sodium hydroxide, potassium hydroxide, calcium oxide, calcium hydroxide, carbon
A kind of or the most two or more mixture in acid magnesium, sodium carbonate and natural whiting stone powder；
Back washing agent solution in step (2) is by the mass percent of 2～15%, back washing agent to be dissolved in water mix homogeneously obtain
Arrive；Back washing agent is sodium hydroxide/potassium, sodium carbonate/potassium, sodium bicarbonate/potassium, sodium oxide and the one of potassium oxide or any two kinds
Above mixture, or a kind of or the most two or more mixture of sulphuric acid, hydrochloric acid and nitric acid.
One the most according to claim 1 utilizes V5+The extracting and enriching method containing vanadium solution, it is characterised in that: step (1)
In oxidizing reaction temperature and extraction temperature in step (2) all at 25～50 DEG C.
One the most according to claim 1 utilizes V5+The extracting and enriching method containing vanadium solution, it is characterised in that: extractant bag
Include in tri-n-octyl amine, trioctylamine, Mextral 54-100, N235, Alamine 336, N263, N1923, HBL101 and P507
Or the most two or more a kind of mixture；Synergic reagent includes n-octyl alcohol, isooctanol, sec-octyl alcohol or tributyl phosphate；Solvent bag
Include a kind of or the most two or more mixture in solvent kerosene, sulfonated kerosene, benzene, chloroform or 2 one ethyl hexanols.
One the most according to claim 1 utilizes V5+The extracting and enriching method containing vanadium solution, it is characterised in that: counter-current extraction
Extraction progression be 2～4 grades, extraction be in a ratio of organic facies: aqueous phase=1:(1～5), extract stream speed ratio is organic facies: aqueous phase=
1:(1～5)；Extraction is no less than 3 minutes time of contact.
One the most according to claim 1 utilizes V5+The extracting and enriching method containing vanadium solution, it is characterised in that: back extraction processes
Extraction progression be 2～5 grades, back extraction is in a ratio of organic facies: aqueous phase=(1～5): 1, and back extraction velocity ratio is organic facies: aqueous phase=
(1～5): 1；Back extraction is no less than 5 minutes time of contact.
One the most according to claim 1 utilizes V5+The extracting and enriching method containing vanadium solution, it is characterised in that: at back extraction
Extraction organic facies after reason is regenerated by regenerant solution, and the organic facies after regeneration is backflowed to and extracted organic facies groove, regenerates progression
Being 1～2 grade, regeneration is in a ratio of organic facies: aqueous phase=(1～5): 1, and regeneration velocity ratio is for organic facies: aqueous phase=(5～10): 1；
Regenerant solution is by the mass percent of 2～10%, regenerative agent to be dissolved in water mix homogeneously obtain, and regenerative agent is carbon
A kind of or the most two or more mixture in acid sodium, ammonium carbonate and sodium hydroxide, or be the one in sulphuric acid and hydrochloric acid
Or two kinds of mixture.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108754187A (en) * | 2018-05-08 | 2018-11-06 | 重庆大学 | A method of with microemulsion from solution Selective Separation vanadium phosphorus |
| CN111378836A (en) * | 2018-12-29 | 2020-07-07 | 陕西华地矿业有限公司 | Method for generating vanadium pentoxide by pentavalent vanadium extraction method |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101565775A (en) * | 2009-02-17 | 2009-10-28 | 昆明理工大学 | Method for recovering medium-concentration and low-concentration vanadium in industrial sewage resulted from stone coal vanadium extraction |
| CN102181635A (en) * | 2011-04-08 | 2011-09-14 | 北京矿冶研究总院 | Method for preparing vanadium pentoxide from stone coal vanadium ore sulfuric acid leaching solution |
| CN102851500A (en) * | 2012-09-19 | 2013-01-02 | 中南大学 | Method for extracting vanadium from vanadium-containing highly concentrated sulfuric acid solution and application of extracting agent |
-
2016
- 2016-08-30 CN CN201610785701.XA patent/CN106282607B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101565775A (en) * | 2009-02-17 | 2009-10-28 | 昆明理工大学 | Method for recovering medium-concentration and low-concentration vanadium in industrial sewage resulted from stone coal vanadium extraction |
| CN102181635A (en) * | 2011-04-08 | 2011-09-14 | 北京矿冶研究总院 | Method for preparing vanadium pentoxide from stone coal vanadium ore sulfuric acid leaching solution |
| CN102851500A (en) * | 2012-09-19 | 2013-01-02 | 中南大学 | Method for extracting vanadium from vanadium-containing highly concentrated sulfuric acid solution and application of extracting agent |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108754187A (en) * | 2018-05-08 | 2018-11-06 | 重庆大学 | A method of with microemulsion from solution Selective Separation vanadium phosphorus |
| CN111378836A (en) * | 2018-12-29 | 2020-07-07 | 陕西华地矿业有限公司 | Method for generating vanadium pentoxide by pentavalent vanadium extraction method |
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