CN107312942A - The method of extract and separate vanadium and chromium from vanadium chromium slag pickle liquor - Google Patents
The method of extract and separate vanadium and chromium from vanadium chromium slag pickle liquor Download PDFInfo
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- CN107312942A CN107312942A CN201710537785.XA CN201710537785A CN107312942A CN 107312942 A CN107312942 A CN 107312942A CN 201710537785 A CN201710537785 A CN 201710537785A CN 107312942 A CN107312942 A CN 107312942A
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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
- C22B34/30—Obtaining chromium, molybdenum or tungsten
- C22B34/32—Obtaining chromium
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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
- C22B3/37—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds containing boron, silicon, selenium or tellurium
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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
- C22B7/007—Wet processes by acid leaching
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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
- C22B7/04—Working-up slag
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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
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Abstract
A kind of method of extract and separate vanadium and chromium during the present invention provides chromium slag pickle liquor from vanadium, including：S1, using extract the pentavalent vanadium and Cr VI in vanadium chromium slag pickle liquor are extracted into separated from the water after organic phase, obtain loading the organic phase of vanadium chromium；S2, using back washing agent the organic phase of the load vanadium chromium in step S1 is stripped, after back extraction terminates, obtained containing chromium back extraction extraction raffinate, ammonium metavanadate or ammonium poly-vanadate precipitation and regeneration of ionic liquid；S3, the ammonium metavanadate or ammonium poly-vanadate that are obtained in step S2 are deposited at 550 DEG C 600 DEG C calcining obtain barium oxide；S4, the Cr that will be stripped in step S2 in extraction raffinate6+Reduction generation Cr3+, adjust chromium after chromium pH and separated out with precipitation form, calcining obtains Cr2O3.The inventive method extraction efficiency is high, and rapid, no emulsion is layered after extraction, and ionic liquid has good lipophilic-hydrophobic property, in long-chain alcohol have preferable dissolubility, and with water base it is immiscible, can reduce because aqueous phase carry secretly or dissolve produce organic phase loss.
Description
Technical field
The invention belongs to the side of extract and separate vanadium and chromium in metallurgical technology field, more particularly to a kind of chromium slag pickle liquor from vanadium
Method.
Background technology
In modern industrial technology, vanadium and chromium are important valuable metal elements, are widely used in metallurgical industry and change
Learn industry.Contained heavy metal vanadium, chromium ion have preferably water-soluble and transfer ability in vanadium chromium slag pickle liquor, such as long-term dew
It is stored up, and can be dissolved in the water body that permeates the ground, and severe contamination is caused to environment and the mankind.In addition, vanadium therein, chromium are again
It is particularly important rare metal, is had a wide range of applications in aviation, automobile, shipbuilding, and national defense industry.
The method of current vanadium chromium separation mainly has chemical precipitation method, ion-exchange, electrolysis and extraction.For example, existing
There is a Chinese patent to disclose a kind of precipitation method separation vanadium chromium, but the recovery rate of chromium is not high, simultaneously because entrainment impurity, production
Product purity is low.Also current document is disclosed using ion-exchange and electrolysis separation vanadium chromium, though automation is easy to implement,
But and energy waste higher to pre-processing requirements is serious, therefore technique is complex.
The content of the invention
To solve technical problem of the prior art, the present invention provide one kind from vanadium chromium slag pickle liquor extract and separate vanadium and
The method of chromium.
The technical solution adopted by the present invention is as follows：
In a first aspect, the present invention a kind of chromium slag pickle liquor from vanadium is provided in extract and separate vanadium and chromium method, including：
S1, using extract the pentavalent vanadium and Cr VI in vanadium chromium slag pickle liquor are extracted into after organic phase and aqueous phase point
From, obtain load vanadium chromium organic phase；
S2, using back washing agent the organic phase of the load vanadium chromium in step S1 is stripped, after back extraction terminates, obtained down
Layer back extraction extraction raffinate containing chromium (aqueous solution), ammonium metavanadate or ammonium poly-vanadate precipitation and regeneration of ionic liquid；
S3, the ammonium metavanadate or ammonium poly-vanadate that are obtained in step S2 are deposited at 550 DEG C -600 DEG C calcining obtain vanadium oxygen
Compound；
S4, the Cr that will be stripped in step S2 in extraction raffinate6+Reduction generation Cr3+, adjust chromium after chromium pH and analysed with precipitation form
Go out, calcining obtains Cr2O3Powder.
Alternatively, before step S1, methods described also includes：
S0, the pH value of the pretreated vanadium chromium slag pickle liquor of regulation, it is 2~5 to make pH value；
Correspondingly, S1, the pentavalent vanadium in the immersion liquid that will be obtained using extract in step S0 and Cr VI are extracted into organic
It is separated from the water after phase, obtain loading the organic phase of vanadium chromium.
Alternatively, step S0 includes：
(ammoniacal liquor is anti-for adjusting extraction at this for addition inorganic acid and ammoniacal liquor in the good vanadium chromium slag pickle liquor of pre-oxidation
The pH's answered), the pH value of leachate is located at 2~5 intervals；Or,
Inorganic acid described in step S0 is sulfuric acid, hydrochloric acid or phosphoric acid.
Alternatively, the extract in the step S1 is obtained by the way that extractant is dissolved in into diluent；
The diluent is the alcohol that carbon number is 5.
Alternatively, extractant is 1- octyl groups -3- methyl-imidazoles tetrafluoroborate [Omim] BF4
Or,
Extractant is 1- decyls -3- methyl-imidazoles tetrafluoroborate [Deim] BF4；
Or,
Extractant is 1- dodecyl -3- methyl imidazolium tetrafluoroborates [Domim] BF4。
Alternatively, the back washing agent in step S2 is 0.5~1.25mol/L NH4Br solution.
Alternatively, extracted in step S1 using one-level in the immersion liquid obtained in mode or multitple extraction mode extraction step S0
Pentavalent vanadium and Cr VI.
Alternatively, using one-level back extraction or multistage back extraction mode having to the load vanadium chromium in step S1 in step S2
Machine is mutually stripped；
Alternatively, the extract is 10.0g/L -50.0g/L ionic liquid-amyl alcohol solution.
Alternatively, the extract is the ionic liquid that 1- octyl groups -3- methyl-imidazoles tetrafluoroborate is configured to amylalcohol
Body-organic phase solution；
Or,
The extract is, 1- decyls -3- methyl-imidazoles tetrafluoroborate [Deim] BF4The ion being configured to amylalcohol
Liquid-organic phase solution；
Or,
The extract is 1- dodecyl -3- methyl imidazolium tetrafluoroborates [Domim] BF4With amylalcohol be configured to from
Sub- liquid-organic phase solution.
Beneficial effect：
The present invention be based on the extractants such as 1- octyl group -3- methyl-imidazoles tetrafluoroborates pH=2~5 acidity to weak
Under acid condition, to Cr2O7 2-And VO3 -With very strong extracting power, first, by Cr in containing vanadium and chromium pickle liquor2O7 2-And VO3 -Extraction
Get organic phase, after extraction terminates, the organic phase of loaded metal ion is stripped using ammonium bromide, vanadium is preferentially and ammonium salt
With reference to generation ammonium metavanadate or ammonium poly-vanadate precipitation, chromium are present in back extraction extraction raffinate；Metal ion or generation precipitation are returned to
In aqueous phase, extractant is regenerated, generation novel ion liquid 1- octyl groups -3- methylimidazoles-bromide.
The inventive method extraction efficiency is high, is layered rapidly after equilibration time section, extraction, no emulsion is simple to operate, and
Ionic liquid has good lipophilic-hydrophobic property, immiscible with water base, can reduce because aqueous phase is carried secretly or dissolves the organic of generation
Mutually lose.
Brief description of the drawings
In order to illustrate more clearly about the embodiment of the present invention or technical scheme of the prior art, below will be to embodiment or existing
There is the accompanying drawing used required in technology description to be briefly described.
Fig. 1 is preparation manipulation scheme sketch of the invention；
Fig. 2 is the stereoscan photograph schematic diagram of barium oxide in the embodiment of the present invention 2；
Fig. 3 is the X ray diffracting spectrum of barium oxide in the embodiment of the present invention 2；
Fig. 4 is the lab diagram after chromium sediment calcination in the embodiment of the present invention 1.
Embodiment
Embodiment of the present invention is described in detail below in conjunction with embodiment, but those skilled in the art will
Understand, the following example is merely to illustrate the present invention, and is not construed as limiting the scope of the present invention.It is unreceipted specific in embodiment
Condition person, the condition advised according to normal condition or manufacturer is carried out.Agents useful for same or the unreceipted production firm person of instrument, be
The conventional products that can be obtained by commercially available purchase.
Currently, extraction is due to that less energy consumption, simple to operate, product purity be high, energy consumption is low and environmental pollution is small etc. is excellent
The separation of many kinds of substance is put and is widely used in, with good industrial applications prospect.
Ionic liquid is that a class is made up of organic cation and organic or inorganic anion, is in room temperature or near room temperature
The organic salt of liquid, compared with traditional volatile organic solvent, with volatility is low, hot and chemical stability is high, electrification
Many characteristics such as window is wide and ionic conductivity is high are learned, make it in organic synthesis, biology, the energy, lithium ion battery and catalysis
There is wide application and Research Prospects Deng field.Although ionic liquid is applied to the search time ability that metal ion extraction is separated
The time of several years, but got more and more people's extensive concerning, and it is applied to grinding for vanadium chromium separation specific to ion liquid abstraction agent
Study carefully and have not been reported.
In vanadium chromium slag leachate in following examples, H is there is+、Fe3+、VO3 -、Cr2O7 2-、SO4 2-、Na+、Ca2+Or
Cl-Etc. a variety of dissociated ions, according to hsab theory, wherein majority belongs to hard acid or hard base, but the wherein vanadium of most critical, chromium
Two kinds of elements are then with VO3 -、Cr2O7 2-" soft base " form is present, and this is also most this qualitative difference of vanadium chromium and other ions,
It is separation and Extraction vanadium and the most important theoretical foundation of chromium.And in ionic liquid organic cation " soft acid " attribute, with VO3 -、
Cr2O7 2-" soft base " has stronger binding ability, is the most important theoretical foundation that ionic liquid is applied as extractant.
Embodiment 1
A kind of method of extract and separate vanadium and chromium during the present embodiment provides chromium slag pickle liquor from vanadium, as shown in figure 1, method bag
Include：
The good vanadium chromium slag pickle liquor (2.5g/L containing vanadium, containing chromium 0.16g/L) of S0,100.0ml pre-oxidation, using 10~
50wt% sulfuric acid adjusts the pH value of leachate, and it is 3 to make pH value.
Pre-oxidation in this step is that the lower valency vanadium in vanadium chromium slag pickle liquor, lower valency chromium are oxidized into five in advance
The vanadium chromium slag pickle liquor of valency vanadium and Cr VI.Such as can add oxidant and can be hydrogen peroxide, sodium hypochlorite or potassium permanganate.
The pentavalent vanadium that will be obtained under 100.0ml extracts, normal temperature in step S0 is added in S1, the pickle liquor into step S0
It is extracted into Cr VI separated from the water after organic phase, obtains loading the organic phase of vanadium chromium, the extraction yield of vanadium single-stage is
85.02%, the extraction yield of chromium single-stage is 87.17%.
Extract is, using 1- octyl group -3- methyl-imidazoles tetrafluoroborates as extractant, to be prepared with organic solvent for n-amyl alcohol
Into ionic liquid-amyl alcohol solution of the 40.0g/L containing extractant.
In order to prevent high-valence state metal from occurring redox reaction with having the organic solvent Long Term Contact of reducing power,
The organic solvent that there is reproducibility using kerosene, sulfonated kerosene etc. should be avoided, therefore above-mentioned selection is that anti-reducing power is stronger
Organic solvent n-amyl alcohol.
Step S1 can carry out extraction mode realization using multitple extraction mode.The multitple extraction of the present embodiment is：Material
Liquid and raffinate are all in contact with fresh extractant, and extraction yield is higher.Multitple extraction is to ensure the metal in pickle liquor
Ion is all extracted, if single extraction rate is higher, does not need multitple extraction technique.
S2, the NH using 50.0ml 0.75mol/L4Organic phase of the Br ammonium bromide solutions to the load vanadium chromium in step S1
It is stripped, after back extraction terminates, carries out isolated lower floor back extraction extraction raffinate containing chromium (i.e. the aqueous solution), ammonium metavanadate or many vanadic acid
Ammonium is precipitated and regeneration of ionic liquid is 1- octyl groups -3- methylimidazoles-bromide.
In this step, vanadium combines generation ammonium metavanadate prior to ammonium ion or ammonium poly-vanadate is precipitated.
S3, the ammonium metavanadate or ammonium poly-vanadate that are obtained in step S2 are deposited at 550 DEG C -600 DEG C calcining obtain vanadium oxygen
Compound.
In this step, different calcination conditions can generate the barium oxide of different valence state.
The pH containing chromium back extraction extraction raffinate is 2 or so in S4, regulating step S2, according to the Cr in back extraction extraction raffinate6+Molar concentration
Excess NaHSO is added according to stoichiometric number30.15g is stirred to pH value of solution dimension with ensureing that Cr VI is reduced completely under normal temperature
Hold in 2 or so, i.e. Cr6+Reduction generation Cr completely3+, adjust chromium after chromium pH=8.0 and separated out with precipitation form, calcining produces Cr2O3,
As shown in figure 4, and then recyclable trivalent chromium, final vanadium recovery be 73.34%, chromium is 75.67%.
Cr2O7 2-+3HSO3-+5H+→2Cr3++3SO4 2-+4H2O(1.8<pH<2.2)
Fig. 4 is the X-ray diffraction using school's special detection XRD equipment detection, by carrying out X-ray diffraction to material,
Its diffracting spectrum is analyzed, the research meanses of the information such as the structure or form of composition, material internal atom or molecule of material are obtained.
X-ray diffraction spectrum be X-ray diffractometer with the whole diffraction region of 2 θ angle scanning, as angle change, be used as X-ray diffraction
The abscissa of spectrum is present.Different diffraction angle (being 2 θ, be not θ) diffraction maximum intensity as ordinate, so constitute XRD
Spectrum.In the present embodiment, after test sample, processing data, sample is chrome green.
Embodiment 2
The present embodiment uses sodium roasting vanadium chromium slag pickle liquor extract and separate vanadium chromium.Method includes：
The good vanadium chromium slag pickle liquor (2.5g/L containing vanadium, containing chromium 0.16g/L) of S0,100.0ml pre-oxidation, using 10~
50wt% sulfuric acid adjusts the pH value of leachate, and it is 4 to make pH value.
The pentavalent vanadium that will be obtained under 120.0ml extracts, normal temperature in step S0 is added in S1, the pickle liquor into step S0
It is extracted into Cr VI separated from the water after organic phase, obtains loading the organic phase of vanadium chromium, the extraction yield of vanadium single-stage is
88.59%, the extraction yield of chromium single-stage is 90.48%.
Extract is, using 1- decyl -3- methyl-imidazoles tetrafluoroborates as extractant, to be prepared with organic solvent for n-amyl alcohol
Into ionic liquid-amyl alcohol solution of the 45.0g/L containing extractant.
S2, using 1.0mol/L ammonium bromide solutions the organic phase of the load vanadium chromium in step S1 is stripped, be stripped
After end, lower floor's back extraction extraction raffinate containing chromium (aqueous solution), ammonium metavanadate or ammonium poly-vanadate precipitation and regeneration of ionic liquid i.e. 1- are obtained
Octyl group -3- methylimidazoles-bromide.
S3, the ammonium metavanadate or ammonium poly-vanadate that are obtained in step S2 are deposited at 550 DEG C calcining obtain barium oxide.
As shown in Figures 2 and 3.
Specifically, in the present embodiment, the atomic percent of the barium oxide in step S3 is as follows.
The atomic percent is measured by ESEM equipment, is all the data that equipment is provided, and form is also machine
The result provided afterwards is measured, analysis atomic percent show that product is vanadium oxide.
The pH containing chromium back extraction extraction raffinate is 2 or so in S4, regulating step S2, according to the Cr in back extraction extraction raffinate6+Molar concentration
Excess NaHSO is added according to stoichiometric number30.18g is stirred to pH value of solution dimension with ensureing that Cr VI is reduced completely under normal temperature
Hold in 2 or so, i.e. Cr6+Reduction generation Cr completely3+, adjust chromium after chromium pH=8.0 and separated out with precipitation form, calcining produces Cr2O3,
And then recyclable trivalent chromium, final vanadium recovery is 78.68%, and chromium is 82.95%.
Embodiment 3
The present embodiment uses sodium roasting vanadium chromium slag pickle liquor extract and separate vanadium chromium.Method includes：
The good pickle liquor of S0,100.0ml pre-oxidation (2.5g/L containing vanadium, containing chromium 0.16g/L), using 10~50wt%'s
Sulfuric acid adjusts the pH value of leachate, and it is 4.5 to make pH value.
The pentavalent vanadium that will be obtained under 150.0ml extracts, normal temperature in step S0 is added in S1, the pickle liquor into step S0
It is extracted into Cr VI separated from the water after organic phase, obtains loading the organic phase of vanadium chromium, the extraction yield of vanadium single-stage is
90.02%, the extraction yield of chromium single-stage is 92.84%.
It, using 1- dodecyl -3- methyl-imidazoles tetrafluoroborates as extractant, is n-amyl alcohol with organic solvent that extract, which is,
It is configured to ionic liquid-amyl alcohol solution of the 50.0g/L containing extractant.
S2, using 1.25mol/L ammonium bromide solutions the organic phase of the load vanadium chromium in step S1 is stripped, be stripped
After end, lower floor's back extraction extraction raffinate containing chromium (aqueous solution), ammonium metavanadate or ammonium poly-vanadate precipitation and regeneration of ionic liquid i.e. 1- are obtained
Octyl group -3- methylimidazoles-bromide；
S3, the ammonium metavanadate or ammonium poly-vanadate that are obtained in step S2 are deposited at 580 DEG C calcining obtain barium oxide；
The pH containing chromium back extraction extraction raffinate is 2 or so in S4, regulating step S2, according to the Cr in back extraction extraction raffinate6+Molar concentration
Excess NaHSO is added according to stoichiometric number30.2g is stirred to pH value of solution dimension with ensureing that Cr VI is reduced completely under normal temperature
Hold in 2 or so, i.e. Cr6+Reduction generation Cr completely3+, adjust chromium after chromium pH=8.0 and separated out with precipitation form, calcining obtains Cr2O3,
And then recyclable trivalent chromium, final vanadium recovery is 80.05%, and chromium is 85.78%.
In conventional art, extraction separation method is to instigate leachate and another not miscible solvent close contact, allows molten
Certain or several solutes in liquid enter in solvent, so that the process that they are separated with other interfering components in solution.Mesh
It is preceding to be studied using extract and separate vanadium/chromium, for example with amine extractant system, three phase extraction system, aqueous two-phase extraction body
System etc., reaches the purpose of vanadium/chromium separation.Extract and separate has that the separation of vanadium/chromium is big, technological process is short, it is easy to operate, into
This low advantage.Therefore, vanadium/chromium extraction isolation technics must be one of main method that following vanadium chromium slag is developed, and open
Exhibition research related to this is significant.
In metal ion extraction system, ionic liquid is only acted only as into " supporting role " as " green solvent " application and made
With, but because its is costly, so the possibility of industrial applications is minimum.As can be seen here, using ionic liquid as extractant,
Vanadium/chromium extraction separation is applied to the identity of " leading role " and yet there are no correlative study report.Although existing in vanadium chromium slag infusion solution
Up to ten several ions, but all exist with free state, and the zwitterion of ionic liquid is also to exist with free state
, therefore environmental basis is provided applied to vanadium/chromium extraction separation with " leading role " identity of " extractant " for ionic liquid.With new
Science, probe into using ionic liquid as extractant in vanadium/chromium separation system with " leading role " mode application, achieve
By " green solvent " " supporting role " identity to " leading role " identity of " extractant " big counteroffensive.
Ionic liquid is expensive in the prior art, is generally all to be used as green solvent, it is therefore desirable to quantity of solvent
Steeply rise, cost is high, be, as extractant, to be dissolved in n-amyl alcohol and constitute extract in the embodiment of the present invention, change
Traditional supporting role role of " green solvent " of ionic liquid, vanadium chromium slag is applied to by it with " leading role " new role of " extractant "
Recycling, breaks through cost " bottleneck " restriction of Industrialization of Ionic Liquids application, expands the application field of ionic liquid.
The technical principle of the present invention is described above in association with specific embodiment, these descriptions are intended merely to explain the present invention's
Principle, it is impossible to be construed to limiting the scope of the invention in any way.Based on explaining herein, those skilled in the art
Would not require any inventive effort can associate other embodiments of the present invention, and these modes fall within this hair
Within bright protection domain.
Claims (10)
1. a kind of method of extract and separate vanadium and chromium in chromium slag pickle liquor from vanadium, it is characterised in that including：
S1, using extract the pentavalent vanadium and Cr VI in vanadium chromium slag pickle liquor are extracted into separated from the water after organic phase, obtained
To the organic phase of load vanadium chromium；
S2, using back washing agent the organic phase of the load vanadium chromium in step S1 is stripped, after back extraction terminates, obtains lower floor and contain
Chromium back extraction extraction raffinate, ammonium metavanadate or ammonium poly-vanadate precipitation and regeneration of ionic liquid；
S3, the ammonium metavanadate or ammonium poly-vanadate that are obtained in step S2 are deposited at 550 DEG C -600 DEG C calcining obtain barium oxide；
S4, the Cr that will be stripped in step S2 in extraction raffinate6+Reduction generation Cr3+, adjust chromium after chromium pH and separated out with precipitation form, calcined
Obtain Cr2O3Powder.
2. according to the method described in claim 1, it is characterised in that before step S1, methods described also includes：
S0, the pH value of the pretreated vanadium chromium slag pickle liquor of regulation, it is 2~5 to make pH value；
Correspondingly, S1, the pentavalent vanadium in the immersion liquid that will be obtained using extract in step S0 and Cr VI are extracted into after organic phase
It is separated from the water, obtain loading the organic phase of vanadium chromium.
3. method according to claim 2, it is characterised in that step S0 includes：
Inorganic acid and ammoniacal liquor are added in the good vanadium chromium slag pickle liquor of pre-oxidation, the pH value of leachate is located at 2~5 intervals；
Or,
Inorganic acid described in step S0 is sulfuric acid, hydrochloric acid or phosphoric acid.
4. method according to claim 1 or 2, it is characterised in that extract in the step S1 is by by extractant
It is dissolved in diluent acquisition；
The diluent is the alcohol that carbon number is 5.
5. method according to claim 4, it is characterised in that extractant is 1- octyl group -3- methyl-imidazoles tetrafluoroborates
[Omim]BF4；
Or,
Extractant is 1- decyls -3- methyl-imidazoles tetrafluoroborate [Deim] BF4；
Or,
Extractant is 1- dodecyl -3- methyl imidazolium tetrafluoroborates [Domim] BF4。
6. method according to claim 1 or 2, it is characterised in that the back washing agent in step S2 is 0.5~1.25mol/L
NH4Br solution.
7. method according to claim 1 or 2, it is characterised in that mode or multistage extraction are extracted using one-level in step S1
Take the pentavalent vanadium and Cr VI in the immersion liquid obtained in mode extraction step S0.
8. method according to claim 1 or 2, it is characterised in that using one-level back extraction or multistage back extraction in step S2
Mode is taken to be stripped the organic phase of the load vanadium chromium in step S1.
9. method according to claim 1 or 2, it is characterised in that the extract for 10.0g/L -50.0g/L from
Sub- liquid-amyl alcohol solution.
10. method according to claim 9, it is characterised in that the extract is 1- octyl group -3- methyl-imidazoles tetrafluoros
Ionic liquid-organic phase solution that borate is configured to amylalcohol；
Or,
The extract is, 1- decyls -3- methyl-imidazoles tetrafluoroborate [Deim] BF4The ionic liquid being configured to amylalcohol-
Organic phase solution；
Or,
The extract is 1- dodecyl -3- methyl imidazolium tetrafluoroborates [Domim] BF4The ionic liquid being configured to amylalcohol
Body-organic phase solution.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108823408A (en) * | 2018-07-17 | 2018-11-16 | 东北大学 | A method of utilizing vanadium chromium in pyridine ionic liquid extraction and separation vanadium chromium slag |
| CN109207724A (en) * | 2018-09-12 | 2019-01-15 | 哈尔滨工业大学（威海） | It is a kind of from containing vanadium and chromium solution simultaneously extraction and separation vanadium chromium extractant and extracting process |
| CN116177601A (en) * | 2021-11-29 | 2023-05-30 | 中国科学院过程工程研究所 | Method for preparing high-purity vanadium pentoxide from ammonium polyvanadate |
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| CN109750169A (en) * | 2019-03-28 | 2019-05-14 | 攀钢集团攀枝花钢铁研究院有限公司 | The method of vanadium chromium is separated from vanadium chromium solution |
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| CN104694749A (en) * | 2015-02-12 | 2015-06-10 | 中国科学院过程工程研究所 | Method for extracting and separating vanadium and chromium from alkaline aqueous solution |
| CN106048261A (en) * | 2016-08-22 | 2016-10-26 | 东北大学 | Method for extracting vanadium from acidic solution by using ionic liquid [OMIM]BF4 |
| EP3178576A1 (en) * | 2015-12-11 | 2017-06-14 | Commissariat à l'Energie Atomique et aux Energies Alternatives | Method for recycling the silver contained in a photovoltaic cell |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104694749A (en) * | 2015-02-12 | 2015-06-10 | 中国科学院过程工程研究所 | Method for extracting and separating vanadium and chromium from alkaline aqueous solution |
| EP3178576A1 (en) * | 2015-12-11 | 2017-06-14 | Commissariat à l'Energie Atomique et aux Energies Alternatives | Method for recycling the silver contained in a photovoltaic cell |
| CN106048261A (en) * | 2016-08-22 | 2016-10-26 | 东北大学 | Method for extracting vanadium from acidic solution by using ionic liquid [OMIM]BF4 |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108823408A (en) * | 2018-07-17 | 2018-11-16 | 东北大学 | A method of utilizing vanadium chromium in pyridine ionic liquid extraction and separation vanadium chromium slag |
| CN108823408B (en) * | 2018-07-17 | 2020-05-15 | 东北大学 | Method for extracting and separating vanadium and chromium in vanadium-chromium slag by using pyridine ionic liquid |
| CN109207724A (en) * | 2018-09-12 | 2019-01-15 | 哈尔滨工业大学（威海） | It is a kind of from containing vanadium and chromium solution simultaneously extraction and separation vanadium chromium extractant and extracting process |
| CN116177601A (en) * | 2021-11-29 | 2023-05-30 | 中国科学院过程工程研究所 | Method for preparing high-purity vanadium pentoxide from ammonium polyvanadate |
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