CN107312942B - The method of extraction and separation vanadium and chromium from vanadium chromium slag pickle liquor - Google Patents
The method of extraction and separation vanadium and chromium from vanadium chromium slag pickle liquor Download PDFInfo
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- CN107312942B CN107312942B CN201710537785.XA CN201710537785A CN107312942B CN 107312942 B CN107312942 B CN 107312942B CN 201710537785 A CN201710537785 A CN 201710537785A CN 107312942 B CN107312942 B CN 107312942B
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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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Abstract
A kind of method that the present invention provides extraction and separation vanadium and chromium in the chromium slag pickle liquor from vanadium, including：S1, using extract liquor by vanadium chromium slag pickle liquor pentavalent vanadium and Cr VI be extracted into separated from the water after organic phase, obtain the organic phase of load vanadium chromium；S2, the organic phase of the load vanadium chromium in step S1 is stripped using back washing agent, after back extraction, is obtained containing chromium back extraction extraction raffinate, ammonium metavanadate or ammonium poly-vanadate precipitation and regeneration of ionic liquid；S3, it the ammonium metavanadate or ammonium poly-vanadate that are obtained in step S2 is deposited at 550 DEG C -600 DEG C calcining obtains barium oxide；S4, the Cr that will be stripped in step S2 in extraction raffinate6+Reduction generates Cr3+, chromium is precipitated with precipitation form after adjusting chromium pH, and calcining obtains Cr2O3.The method of the present invention 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 water phase carry secretly or dissolve generate organic phase loss.
Description
Technical field
The invention belongs to the sides of extraction and separation 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 element, are widely used in metallurgical industry and change
Learn industry.Heavy metal vanadium, chromium ion contained in vanadium chromium slag pickle liquor have preferable water-soluble and transfer ability, such as long-term dew
Its stockpiling, can be dissolved in permeating the ground water body, cause seriously to pollute 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 vanadium chromium separation at present 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 detaches vanadium chromium using ion-exchange and electrolysis, though it is easy to implement automation,
But and energy waste higher to pre-processing requirements is serious, therefore the process is more complicated.
Invention content
For solve in the prior art the technical issues of, the present invention provide one kind from vanadium chromium slag pickle liquor extraction and separation vanadium and
The method of chromium.
The technical solution adopted by the present invention is as follows：
In a first aspect, a kind of method that the present invention provides extraction and separation vanadium and chromium in the chromium slag pickle liquor from vanadium, including：
S1, using extract liquor by vanadium chromium slag pickle liquor pentavalent vanadium and Cr VI be extracted into after organic phase and water phase point
From, obtain load vanadium chromium organic phase；
S2, the organic phase of the load vanadium chromium in step S1 is stripped using back washing agent, after back extraction, is obtained down
Layer back extraction extraction raffinate containing chromium (aqueous solution), ammonium metavanadate or ammonium poly-vanadate precipitation and regeneration of ionic liquid；
S3, it the ammonium metavanadate or ammonium poly-vanadate that are obtained in step S2 is deposited at 550 DEG C -600 DEG C calcining obtains vanadium oxygen
Compound；
S4, the Cr that will be stripped in step S2 in extraction raffinate6+Reduction generates Cr3+, chromium is analysed with precipitation form after adjusting chromium pH
Go out, calcining obtains Cr2O3Powder.
Optionally, before step S1, the method further includes：
S0, the pH value for adjusting pretreated vanadium chromium slag pickle liquor, it is 2~5 to make pH value；
Correspondingly, S1, using extract liquor by the immersion liquid obtained in step S0 pentavalent vanadium and Cr VI be extracted into it is organic
It is separated from the water after phase, obtain the organic phase of load vanadium chromium.
Optionally, step S0 includes：
(ammonium hydroxide is anti-for adjusting extraction at this for addition inorganic acid and ammonium hydroxide in the good vanadium chromium slag pickle liquor of pre-oxidation
The pH's answered), so that the pH value of leachate is located at 2~5 sections；Alternatively,
Inorganic acid described in step S0 is sulfuric acid, hydrochloric acid or phosphoric acid.
Optionally, the extract liquor in the step S1 is obtained by the way that extractant is dissolved in diluent；
The diluent is the alcohol that carbon atom number is 5.
Optionally, extractant is 1- octyl -3- methyl-imidazoles Si Fupengsuanyans [Omim]BF4
Alternatively,
Extractant is 1- decyl -3- methyl-imidazoles Si Fupengsuanyans [Deim]BF4；
Or
Extractant is 1- dodecyl -3- Jia Jimizuosifupengsuanyans [Domim]BF4。
Optionally, the back washing agent in step S2 is the NH of 0.5~1.25mol/L4Br solution.
Optionally, using in the immersion liquid obtained in level-one extraction mode or multitple extraction mode extraction step S0 in step S1
Pentavalent vanadium and Cr VI.
Optionally, using level-one back extraction or multistage back extraction mode having to the load vanadium chromium in step S1 in step S2
Machine is mutually stripped；
Optionally, the extract liquor is ionic liquid-amyl alcohol solution of 10.0g/L -50.0g/L.
Optionally, the extract liquor is the ionic liquid that 1- octyls -3- methyl-imidazoles tetrafluoroborate is configured to amylalcohol
Body-organic phase solution；
Alternatively,
The extract liquor is, 1- decyl -3- methyl-imidazoles Si Fupengsuanyans [Deim]BF4The ion being configured to amylalcohol
Liquid-organic phase solution；
Alternatively,
The extract liquor is 1- dodecyl -3- Jia Jimizuosifupengsuanyans [Domim]BF4With amylalcohol be configured to from
Sub- liquid-organic phase solution.
Advantageous effect：
The present invention be based on the extractants such as 1- octyl -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
Organic phase is got, after extraction, the organic phase of loaded metal ion is stripped using ammonium bromide, vanadium is preferentially and ammonium salt
In conjunction with generation ammonium metavanadate or ammonium poly-vanadate precipitation, chromium are present in back extraction extraction raffinate；Metal ion generates precipitation or returns to
In water phase, extractant is regenerated, and generates novel ion liquid 1- octyls -3- methylimidazoles-bromide.
The method of the present invention extraction efficiency is high, is layered rapidly after equilibration time section, extraction, and no emulsion is easy to operate, and
Ionic liquid has good lipophilic-hydrophobic property, immiscible with water base, can reduce because water phase is carried secretly or dissolves the organic of generation
Mutually lose.
Description of the drawings
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technology description to be briefly described.
Fig. 1 is the preparation manipulation scheme schematic diagram of the present 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.
Specific implementation mode
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 invention.It is not specified in embodiment specific
Condition person carries out according to conventional conditions or manufacturer's recommended conditions.Reagents or instruments used without specified manufacturer is
The conventional products that can be obtained by commercially available purchase.
Currently, extraction is since with less energy consumption, that easy to operate, product purity is high, low energy consumption and environmental pollution is small etc. is excellent
The separation of many kinds of substance is put and be widely used in, there is good industrial applications foreground.
Ionic liquid is that one kind is made of organic cation and organic or inorganic anion, is in room temperature or near room temperature
The organic salt of liquid has that volatility is low, hot and chemical stability is high, electrochemical compared with traditional volatile organic solvent
It learns that window is wide and many characteristics such as ionic conductivity is high, makes it in organic synthesis, biology, the energy, lithium ion battery and catalysis
Equal fields have wide application and Research Prospects.Although ionic liquid is applied to the search time of metal ion extraction separation
Several years time, 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 has not been reported.
In vanadium chromium slag leachate in following embodiment, there is H+、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 exists, 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
The present embodiment provides a kind of methods of extraction and separation vanadium and chromium in chromium slag pickle liquor from vanadium, as shown in Figure 1, method packet
It includes：
The good vanadium chromium slag pickle liquor of S0,100.0ml pre-oxidation (2.5g/L containing vanadium, contain chromium 0.16g/L), using 10~
The sulfuric acid of 50wt% adjusts the pH value of leachate, and it is 3 to make pH value.
Pre-oxidation in this step is that lower valency vanadium, the lower valency chromium in vanadium chromium slag pickle liquor are oxidized to five in advance
The vanadium chromium slag pickle liquor of valence vanadium and Cr VI.Such as it can be hydrogen peroxide, sodium hypochlorite or potassium permanganate etc. that oxidant, which can be added,.
100.0ml extract liquors, the pentavalent vanadium that will be obtained in step S0 under room temperature are added in S1, the pickle liquor into step S0
It is extracted into Cr VI separated from the water after organic phase, obtains the organic phase of load vanadium chromium, the extraction yield of vanadium single-stage is
85.02%, the extraction yield of chromium single-stage is 87.17%.
Extract liquor is to be prepared for n-amyl alcohol with organic solvent using 1- octyl -3- methyl-imidazoles tetrafluoroborates as extractant
At ionic liquid-amyl alcohol solution of the 40.0g/L containing extractant.
In order to prevent high-valence state metal with reducing power organic solvent Long Term Contact and redox reaction occurs,
It should avoid using the organic solvent with reproducibility such as kerosene, sulfonated kerosene, therefore above-mentioned selection is that anti-reducing power is stronger
Organic solvent n-amyl alcohol.
Step S1 can be used multitple extraction mode and carry out extraction mode realization.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 all extracts, if single extraction rate is higher, does not need multitple extraction technique.
S2, using the NH of 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, carries out isolated lower layer back extraction extraction raffinate containing chromium (i.e. aqueous solution), ammonium metavanadate or more vanadic acid
Ammonia-sinking shallow lake and regeneration of ionic liquid, that is, 1- octyls -3- methylimidazoles-bromide.
In this step, vanadium is combined prior to ammonium ion generates ammonium metavanadate or ammonium poly-vanadate precipitation.
S3, it the ammonium metavanadate or ammonium poly-vanadate that are obtained in step S2 is deposited at 550 DEG C -600 DEG C calcining obtains vanadium oxygen
Compound.
In this step, different calcination conditions produces 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 to ensure that Cr VI is reduced completely, and stirring to pH value of solution is tieed up under room temperature
It holds in 2 or so, i.e. Cr6+Reduction generates Cr completely3+, chromium is precipitated with precipitation form after adjusting chromium pH=8.0, is calcined up to Cr2O3,
As shown in figure 4, recyclable trivalent chromium, final vanadium recovery are 73.34% in turn, chromium 75.67%.
Cr2O7 2-+3HSO3-+5H+→2Cr3++3SO4 2-+4H2O(1.8<pH<2.2)
Fig. 4 is the X-ray diffraction detected using school's special detection XRD equipment, by carrying out X-ray diffraction to material,
Its diffracting spectrum is analyzed, the research means of the information such as the ingredient of material, the structure of material internal atom or molecule or form are obtained.
X-ray diffraction spectrum is X-ray diffractometer with the entire diffraction region of the angle scanning of 2 θ, as angle change, as X-ray diffraction
The abscissa of spectrum exists.Different angle of diffraction (being 2 θ, be not θ) diffraction maximum intensity as ordinate, constitute XRD in this way
Spectrum.In the present embodiment, after test sample, data are handled, sample is chrome green.
Embodiment 2
The present embodiment uses sodium roasting vanadium chromium slag pickle liquor extraction and separation vanadium chromium.Method includes：
The good vanadium chromium slag pickle liquor of S0,100.0ml pre-oxidation (2.5g/L containing vanadium, contain chromium 0.16g/L), using 10~
The sulfuric acid of 50wt% adjusts the pH value of leachate, and it is 4 to make pH value.
120.0ml extract liquors, the pentavalent vanadium that will be obtained in step S0 under room temperature are added in S1, the pickle liquor into step S0
It is extracted into Cr VI separated from the water after organic phase, obtains the organic phase of load vanadium chromium, the extraction yield of vanadium single-stage is
88.59%, the extraction yield of chromium single-stage is 90.48%.
Extract liquor is to be prepared for n-amyl alcohol with organic solvent using 1- decyl -3- methyl-imidazoles tetrafluoroborates as extractant
At ionic liquid-amyl alcohol solution of the 45.0g/L containing extractant.
S2, the organic phase of the load vanadium chromium in step S1 is stripped using 1.0mol/L ammonium bromide solutions, is stripped
After, obtain lower layer's back extraction extraction raffinate containing chromium (aqueous solution), ammonium metavanadate or ammonium poly-vanadate precipitation and regeneration of ionic liquid i.e. 1-
Octyl -3- methylimidazoles-bromide.
S3, it the ammonium metavanadate or ammonium poly-vanadate that are obtained in step S2 is deposited at 550 DEG C calcining obtains 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 scanning electron microscope equipment, is all the data that equipment provides, and table is also machine
Measure providing later as a result, 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 to ensure that Cr VI is reduced completely, and stirring to pH value of solution is tieed up under room temperature
It holds in 2 or so, i.e. Cr6+Reduction generates Cr completely3+, chromium is precipitated with precipitation form after adjusting chromium pH=8.0, is calcined up to Cr2O3,
And then recyclable trivalent chromium, final vanadium recovery are 78.68%, chromium 82.95%.
Embodiment 3
The present embodiment uses sodium roasting vanadium chromium slag pickle liquor extraction and separation vanadium chromium.Method includes：
The good pickle liquor of S0,100.0ml pre-oxidation (2.5g/L containing vanadium contains 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.
150.0ml extract liquors, the pentavalent vanadium that will be obtained in step S0 under room temperature are added in S1, the pickle liquor into step S0
It is extracted into Cr VI separated from the water after organic phase, obtains the organic phase of load vanadium chromium, the extraction yield of vanadium single-stage is
90.02%, the extraction yield of chromium single-stage is 92.84%.
Extract liquor is using 1- dodecyl -3- methyl-imidazoles tetrafluoroborates as extractant, is n-amyl alcohol with organic solvent
It is configured to ionic liquid-amyl alcohol solution of the 50.0g/L containing extractant.
S2, the organic phase of the load vanadium chromium in step S1 is stripped using 1.25mol/L ammonium bromide solutions, is stripped
After, obtain lower layer's back extraction extraction raffinate containing chromium (aqueous solution), ammonium metavanadate or ammonium poly-vanadate precipitation and regeneration of ionic liquid i.e. 1-
Octyl -3- methylimidazoles-bromide；
S3, it the ammonium metavanadate or ammonium poly-vanadate that are obtained in step S2 is deposited at 580 DEG C calcining obtains 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 to ensure that Cr VI is reduced completely, and stirring to pH value of solution is tieed up under room temperature
It holds in 2 or so, i.e. Cr6+Reduction generates Cr completely3+, chromium is precipitated with precipitation form after adjusting chromium pH=8.0, and calcining obtains Cr2O3,
And then recyclable trivalent chromium, final vanadium recovery are 80.05%, chromium 85.78%.
In traditional technology, extraction separation method is to instigate leachate and another not miscible solvent close contact, is allowed molten
Certain or several solutes in liquid enter in solvent, to the process for making them be detached with other interfering components in solution.Mesh
It is preceding existing using extraction and separation vanadium/chromium research, for example, by using amine extractant system, three phase extraction system, aqueous two-phase extraction body
System etc. achievees the purpose that vanadium/chromium separation.Extraction and separation have vanadium/chromium separation it is big, technological process is short, it is easy to operate, at
This low advantage.Therefore, vanadium/chromium extraction isolation technics must be one of the main method that the following vanadium chromium slag develops and uses, and open
Research related to this is opened up to be of great significance.
In metal ion extraction system, ionic liquid is only acted only as into " supporting role " as " green solvent " application and is made
With, but since its is expensive, so the possibility of industrial applications is minimum.It can be seen that using ionic liquid as extractant,
It is applied to vanadium/chromium extraction separation with 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 be all with existing for free state, and the zwitterion of ionic liquid is also to exist with free state
, therefore vanadium/chromium extraction separation is applied to " leading role " identity of " extractant " for ionic liquid and provides environmental basis.With new
Science, probe into the application in a manner of " leading role " in vanadium/chromium separation system using ionic liquid as extractant, achieve
By " green solvent " " supporting role " identity to " extractant " " leading role " identity big counteroffensive.
Ionic liquid is expensive in the prior art, is usually all to be used as green solvent, it is therefore desirable to quantity of solvent
It steeply rises, it is of high cost, it is to be dissolved in n-amyl alcohol as extractant and form extract liquor in the embodiment of the present invention, changes
It is applied to vanadium chromium slag by traditional supporting role role of " green solvent " of ionic liquid with " leading role " new role of " extractant "
Recycling, the cost " bottleneck " for breaking through Industrialization of Ionic Liquids application restrict, and expand 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 cannot 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 specific implementation modes of the present invention, these modes fall within this hair
Within bright protection domain.
Claims (10)
1. a kind of method of extraction and separation vanadium and chromium in chromium slag pickle liquor from vanadium, which is characterized in that including：
S1, using extract liquor by vanadium chromium slag pickle liquor pentavalent vanadium and Cr VI be extracted into separated from the water after organic phase, obtain
To the organic phase of load vanadium chromium, wherein the extract liquor is ionic liquid-amyl alcohol solution；S2, using back washing agent in step S1
The organic phase of load vanadium chromium be stripped, after back extraction, obtain lower layer containing chromium back extraction extraction raffinate, ammonium metavanadate or more vanadic acid
Ammonia-sinking shallow lake and regeneration of ionic liquid；
S3, it the ammonium metavanadate or ammonium poly-vanadate that are obtained in step S2 is deposited at 550 DEG C -600 DEG C calcining obtains barium oxide；
S4, the Cr that will be stripped in step S2 in extraction raffinate6+Reduction generates Cr3+, chromium is precipitated with precipitation form after adjusting chromium pH, is calcined
Obtain Cr2O3Powder.
2. according to the method described in claim 1, it is characterized in that, before step S1, the method further includes：
S0, the pH value for adjusting pretreated vanadium chromium slag pickle liquor, it is 2~5 to make pH value；
Correspondingly, S1, using extract liquor by the immersion liquid obtained in step S0 pentavalent vanadium and after Cr VI is extracted into organic phase
It is separated from the water, obtain the organic phase of load vanadium chromium.
3. according to the method described in claim 2, it is characterized in that, step S0 includes：
Inorganic acid and ammonium hydroxide are added in the good vanadium chromium slag pickle liquor of pre-oxidation, the pH value of leachate is made to be located at 2~5 sections；
Wherein, the inorganic acid is one kind in sulfuric acid, hydrochloric acid or phosphoric acid.
4. method according to claim 1 or 2, which is characterized in that extract liquor in the step S1 is by by extractant
It is dissolved in diluent acquisition；
The diluent is the alcohol that carbon atom number is 5.
5. according to the method described in claim 4, it is characterized in that, extractant is 1- octyl -3- methyl-imidazoles tetrafluoroborates
[Omim]BF4；
Alternatively,
Extractant is 1- decyl -3- methyl-imidazoles Si Fupengsuanyans [Deim]BF4；
Or
Extractant is 1- dodecyl -3- Jia Jimizuosifupengsuanyans [Domim]BF4。
6. method according to claim 1 or 2, which is characterized in that the back washing agent in step S2 is 0.5~1.25mol/L
NH4Br solution.
7. according to the method described in claim 2, it is characterized in that, using level-one extraction mode or multitple extraction side in step S1
Pentavalent vanadium in the immersion liquid obtained in formula extraction step S0 and Cr VI.
8. method according to claim 1 or 2, which is characterized in that using level-one 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, which is characterized in that the extract liquor be 10.0g/L -50.0g/L from
Sub- liquid-amyl alcohol solution.
10. according to the method described in claim 9, it is characterized in that, the extract liquor is 1- octyl -3- methyl-imidazoles tetrafluoros
Ionic liquid-organic phase solution that borate is configured to amylalcohol；
Alternatively,
The extract liquor is 1- decyl -3- methyl-imidazoles Si Fupengsuanyans [Deim]BF4The ionic liquid-being configured to amylalcohol has
Machine phase solution；
Alternatively,
The extract liquor is 1- dodecyl -3- Jia Jimizuosifupengsuanyans [Domim]BF4The ionic liquid being configured to amylalcohol
Body-organic phase solution.
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| CN201710537785.XA CN107312942B (en) | 2017-07-04 | 2017-07-04 | The method of extraction and separation vanadium and chromium from vanadium chromium slag pickle liquor |
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| CN107312942B true CN107312942B (en) | 2018-10-23 |
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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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| 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 |
| CN109207724B (en) * | 2018-09-12 | 2020-12-29 | 哈尔滨工业大学（威海） | Extraction solvent and extraction method for simultaneously extracting and separating vanadium and chromium from vanadium and chromium-containing solution |
| 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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| 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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| 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 |
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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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