CN110117714A - A kind of method of room temperature saturated oxalic acid solution Anodic electrolysis Leaching Vanadium - Google Patents

A kind of method of room temperature saturated oxalic acid solution Anodic electrolysis Leaching Vanadium Download PDF

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CN110117714A
CN110117714A CN201910454934.5A CN201910454934A CN110117714A CN 110117714 A CN110117714 A CN 110117714A CN 201910454934 A CN201910454934 A CN 201910454934A CN 110117714 A CN110117714 A CN 110117714A
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vanadium
oxalic acid
acid solution
room temperature
concentrate
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CN110117714B (en
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闫柏军
陈学鑫
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University of Science and Technology Beijing USTB
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B1/00Preliminary treatment of ores or scrap
    • C22B1/02Roasting processes
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B1/00Preliminary treatment of ores or scrap
    • C22B1/14Agglomerating; Briquetting; Binding; Granulating
    • C22B1/24Binding; Briquetting ; Granulating
    • C22B1/242Binding; Briquetting ; Granulating with binders
    • C22B1/244Binding; Briquetting ; Granulating with binders organic
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B3/00Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/04Extraction of metal compounds from ores or concentrates by wet processes by leaching
    • C22B3/045Leaching using electrochemical processes
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B3/00Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/04Extraction of metal compounds from ores or concentrates by wet processes by leaching
    • C22B3/16Extraction of metal compounds from ores or concentrates by wet processes by leaching in organic solutions
    • C22B3/1608Leaching with acyclic or carbocyclic agents
    • C22B3/1616Leaching with acyclic or carbocyclic agents of a single type
    • C22B3/165Leaching with acyclic or carbocyclic agents of a single type with organic acids
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B34/00Obtaining refractory metals
    • C22B34/20Obtaining niobium, tantalum or vanadium
    • C22B34/22Obtaining vanadium
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
    • Y02P10/10Reduction of greenhouse gas [GHG] emissions
    • Y02P10/122Reduction of greenhouse gas [GHG] emissions by capturing or storing CO2
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
    • Y02P10/20Recycling

Abstract

A kind of method of room temperature saturated oxalic acid solution Anodic electrolysis Leaching Vanadium, anode is made in compression moulding, reduction roasting after binder mixing is added as initial feed using vanadium iron spinel-type concentrate containing vanadium.Cell reaction is carried out by electrolyte of saturated oxalic acid solution;Iron contained by electrolytic process Anodic and vanadium are oxidized to high valence ion, complex reaction occur with oxalate, finally with [Fe (C2O4)3]3‑, VO2+Or/and [VO (C2O4)2]3‑Form enters solution, [Fe (C2O4)3]3‑[VO (C2O4)2]3‑Promote the leaching of vanadium in vanadium concentrate, while anode surface has free of contamination carbon dioxide gas to be precipitated, cathode has hydrogen precipitation.It after cell reaction, is separated by solid-liquid separation, obtains and contain vanadium leachate.Anode is made using the electric conductivity of vanadium iron spinelle in the present invention, using oxalic acid solution as electrolyte, is electrolysed, and oxalate denominationby forms complex compound in conjunction with iron and vanadium, and the dissolution of vanadium concentrate and vanadium is promoted to be leached by efficient oxidation.The method of the present invention operating condition is mild, and normal temperature and pressure can carry out, and simple process is pollution-free, at low cost.

Description

A kind of method of room temperature saturated oxalic acid solution Anodic electrolysis Leaching Vanadium
Technical field
The invention belongs to electrochemical fields, are related to a kind of method of electrolysis method Leaching Vanadium from vanadium iron spinellid, Vanadium iron spinel-type concentrate containing vanadium is especially made into soluble anode Direct Electrolysis in oxalic acid electrolyte solution, is obtained containing vanadium Leachate.
Background technique
Vanadium is a kind of important alloying element, is widely used in the industries such as machinery, aviation, electronic technology, national defense industry, because This its production is concerned.Currently, the source of vanadium is mainly vanadium titano-magnetite and Rock coal containing alum.Vanadium titano-magnetite is through blast furnace process Enter molten iron afterwards, then by bessemerizing to obtain vanadium slag.Vanadium in Vanadium Residue hercynite is mutually the main phase of object containing vanadium.Vanadium product in bone coal The low and complicated occurrence state in position, in order to realize the enrichment and separation of vanadium in bone coal, Chinese patent CN106011456A and CN107641723A is using bone coal as initial feed, and di-iron trioxide is as additive, and under reducing atmosphere, temperature is 1200 DEG C of roastings It burns, obtaining after magnetic separation has vanadium iron spinel-type concentrate containing vanadium.In conclusion either vanadium titano-magnetite, or contain vanadium Bone coal can convert vanadium to vanadium iron spinelle object phase.Therefore, from vanadium iron spinel-type containing efficient green vanadium extraction in vanadium mineral There is extremely important meaning.
Currently, the prevailing technology from vanadium iron spinel-type containing vanadium extraction in vanadium mineral is sodium roasting, it is directly logical after roasting Water logging is crossed to obtain containing vanadium leachate.But product of roasting sodium metavanadate leads to material because forming a large amount of liquid phases since fusing point is low Sintering, to reduce the leaching rate of vanadium, and can generate HCl, Cl in roasting process2Equal pernicious gases, pollute environment.In order to Material sintering and noxious gas emission are avoided, metallargist proposes a kind of method of vanadium slag calcification baking, by lime and vanadium After slag mixing, direct high-temperature roasting obtains by sulfuric acid leaching after roasting and contains vanadium leachate.But maturing temperature is higher, most Up to 950 DEG C or so, consume energy larger, equipment loss is big.
The disadvantages of generating pernicious gas and high energy consumption high pollution in order to avoid roasting technique, metallurgists use acidleach Or alkali soaking technology carries out vanadium extraction from mineral containing vanadium resource, Xu Mengchun et al. carries out experimental study to tailings in vanadium extraction leaching behavior (experimental study [D] the Northeastern University of Xu Mengchun tailings in vanadium extraction leaching behavior, 2012.), the result shows that, tailings in vanadium extraction difference Using alkali extract technology and oxalic acid extract technology, the leaching effect of similar vanadium is obtained.Under the conditions of alkali extract technology, with alkali The increasing of concentration and liquid-solid ratio, the leaching of vanadium take the lead in increase after decline, as the temperature rises with the extension of extraction time, vanadium Leaching rate gradually rises.In oxalic acid extract technology, with the increase of oxalic acid additional amount and the extension of extraction time, the leaching of vanadium Rate gradually rises.But either alkali soaking technology or oxalic acid extract technology, the rate of recovery of vanadium is too low, and up to 66% is left It is right;The two technique extraction temperature is higher, and at 150 DEG C or more, therefore it is larger to consume energy, and needs high-tension apparatus, equipment investment is higher.This Outside, leachate impurity element is more, leaches in residue there are also the vanadium not being leached largely and chromium, cannot arbitrarily discharge, soaks Tailings processing is difficult out.
Contain vanadium mineral by electrochemical decomposition vanadium iron spinelle, is a kind of cleaning, efficient vanadium extracting new method.Chinese patent A kind of method that CN102134640A proposes electrocatalytic oxidation leaching Converter Vanadium-bearing Slag, by Converter Vanadium-bearing Slag and MnSO4、H2SO4It is tuned into mine Slurry leach without diaphragm electrocatalytic oxidation.But the rate of recovery of this method vanadium is low, and has additive to be added to electrolyte solution It is interior, difficulty is caused to the separation of subsequent vanadium.
Chinese patent CN103060843 and CN103421950A propose a kind of molten using potassium hydroxide solution as electrolyte Liquid, the synchronous method for extracting vanadium chromium of electrochemical decomposition vanadium slag.Mixed ingredients are made in vanadium slag and potassium hydroxide aqueous solution Hybrid Heating Slurry, is then added in normal pressure electrolytic cell, oxidizing gas is passed through into solution, is electrolysed to obtain reaction slurry, obtains and contain vanadium Leachate.But the method, there are still many deficiencies, electrolyte solution uses potassium hydroxide as electrolyte, improves and is produced into This, and concentration of potassium hydroxide is larger, and corrosivity is stronger;Before cell reaction, need mixed to vanadium slag and potassium hydroxide aqueous solution Heating is closed, to increase energy consumption;It in electrolytic process, needs continuously to be passed through oxidizing gas into reaction system, increases Production cost and bring security risk.
Summary of the invention
In view of the deficiencies of the prior art, one of the objects of the present invention is to provide a kind of room temperature saturated oxalic acid solution Anodics The method for being electrolysed Leaching Vanadium is made into anode Direct Electrolysis Leaching Vanadium with conductive vanadium iron spinel-type concentrate containing vanadium a kind of Method.It realizes in normal temperature and pressure, oxalic acid electrolyte solution, in the case where not adding any additive, obtains and soaked containing vanadium Liquid out.Iron contained by electrolytic process Anodic and vanadium are oxidized to high valence ion, with oxalate occur complex reaction, finally with [Fe(C2O4)3]3-, VO2+Or/and [VO (C2O4)2]3-Form enters solution, [Fe (C2O4)3]3-[VO (C2O4)2]3-Promote vanadium The leaching of vanadium in concentrate, while anode surface has free of contamination carbon dioxide gas to be precipitated.
A kind of method of room temperature saturated oxalic acid solution Anodic electrolysis Leaching Vanadium, it is characterised in that the following steps are included: with Vanadium iron spinel-type concentrate containing vanadium is initial feed, it is mixed in a certain ratio with binder, type is then pressed into, is restoring It is roasted under atmosphere, the anode of conductive energy is made;Using saturated oxalic acid solution as electrolyte, it is electrolysed at normal temperatures and pressures Reaction;Iron contained by electrolytic process Anodic and vanadium are oxidized to high valence ion, with oxalate occur complex reaction, finally with [Fe(C2O4)3]3-, VO2+Or/and [VO (C2O4)2]3-Form enters solution, [Fe (C2O4)3]3-[VO (C2O4)2]3-Promote vanadium The leaching of vanadium in concentrate, while anode surface has free of contamination carbon dioxide gas to be precipitated, cathode has hydrogen precipitation;Cell reaction After, it is separated by solid-liquid separation, obtains and contain vanadium leachate.
Further, vanadium iron spinel-type concentrate containing vanadium will carry out ball milling, until granularity is 0.074mm or less.
Further, the binder is the polyvinyl alcohol of mass fraction 5%, and vanadium concentrate and binder are 5 in mass ratio: 1~10:1 after evenly mixing, then with the pressure compression moulding of 200~300MPa;The round block suppressed is placed in high temperature furnace 6h is roasted under reducing atmosphere, and temperature is 800 DEG C~1000 DEG C.
Further, the mass ratio of vanadium concentrate and binder is preferably 8:1;Maturing temperature is preferably 800 under reducing atmosphere ℃。
Further, the electrolytic cell of the cell reaction is normal temperature and pressure electrolytic cell, and electrolyte is that grass is saturated under room temperature Acid solution selects metal material or carbon material for cathode using vanadium iron spinel-type concentrate containing vanadium as anode, and electrode shape is stick Shape.
Further, the cell reaction carries out under electromagnetic agitation, and the tank voltage of electrolysis is 5V~10V, cell reaction Time is 5h~10h.
Further, in the electrolytic process, the higher conducting wire of the electric conductivity connecting with vanadium concentrate cannot be molten with electrolyte Liquid contact, to ensure that anode electrolysis reaction occurs on vanadium iron spinelle.
Further, after cell reaction, anode and cathode deionized water is rinsed 3~5 times, solid-liquid is then carried out Separation obtains leached tailings and contains vanadium leachate.
Following reaction may occur during cell reaction:
H2C2O4-2e→2CO2+2H+
Fe2O4+7H2C2O4-2e→2[Fe(C2O4)3]3-+VOC2O4+3H2O+8H+
Fe2O4+8H2C2O4-2e→2[Fe(C2O4)3]3-+[VO(C2O4)2]2-+3H2O+10H+
2H++2e→H2
In the method for the present invention, iron contained by anode and vanadium are oxidized to high valence ion, complex reaction occur with oxalate, most Eventually with [Fe (C2O4)3]3-, VO2+Or/and [VO (C2O4)2]3-Form enters solution, [Fe (C2O4)3]3-[VO (C2O4)2]3-Promote Into the leaching of vanadium in vanadium concentrate, while anode surface has free of contamination carbon dioxide gas to be precipitated.This method is brilliant using vanadium iron point Vanadium iron spinel-type concentrate containing vanadium, is directly made into electrode, directly by the stronger complexing of electric conductivity and oxalate denominationby of stone Electrolysis, can carry out vanadium extraction at normal temperatures and pressures.To which in normal temperature and pressure, weak acid is sharp as vanadium iron is electrolysed under conditions of electrolyte Spar type concentrate containing vanadium, this technique relative to it is existing roasting, direct acidleach or alkali leaching and electrochemical oxidation leach process for extracting vanadium and Speech, in electrolytic process, the [Fe (C to be formed is complexed with oxalate denominationby2O4)3]3-[VO (C2O4)2]3-Promote the electricity of vanadium concentrate The leaching of solution and vanadium achievees the effect that vanadium is leached by efficient oxidation.In addition, production cost can be greatly lowered in this technique, drop Low energy consumption reduces environmental pollution.
The technical solution adopted by the present invention has the advantage that compared with prior art
1. the present invention provides a kind of method of room temperature saturated oxalic acid solution Anodic electrolysis Leaching Vanadium, vanadium iron spinelle is utilized Electric conductivity, vanadium iron spinel-type concentrate containing vanadium is directly made into anode, is contained by electrochemical means vanadium oxide hercynite type Vanadium concentrate.
2. the method compared with traditional handicraft, can be carried out in normal temperature and pressure, to reduce energy consumption, pollution is reduced;Nothing Any oxidant addition, ammonium acetate are simple.
3. in electrolytic process, the [Fe (C to be formed is complexed with oxalate denominationby in terms of reaction system2O4)3]3-[VO (C2O4)2]3-The leaching for promoting vanadium in vanadium concentrate, achievees the effect that vanadium is efficiently leached;The hydrogen that cathode generates is recovered, can be with It is used as clean energy resource, it is energy saving.
4. it is small to corrosivity such as electrolytic cell and electrodes since electrolyte oxalic acid solution belongs to weak acid, extend the use of equipment Service life.
Detailed description of the invention
Fig. 1 is vanadium iron spinel-type vanadium concentrate electrolysis unit figure,
Fig. 2 is electrolysed to pure vanadium iron spinelle, different tank voltages, the relationship of electric current and time, illustrate with The increase of tank voltage, curent change is violent, illustrates that anode metamorphosis is larger, and the leaching rate of vanadium increases.
Fig. 3 is that tank voltage is 10V, is fabricated to electrode to vanadium concentrate and is electrolysed, the relationship of electric current and time, Cong Tuzhong As can be seen that current fluctuation is larger, and cell reaction is violent before 6500s;After 6500s, electric current drops to the left side 0.006A suddenly The right side, since electric current is too small, the electrolysis of vanadium is leached slow.
Specific embodiment
In order to verify feasibility of the invention, below with reference to the example content that the present invention is further explained, but it is of the invention Content is not limited solely to following example.The simple modification that substantive content according to the present invention is made, should all cover in this hair Within bright protection scope.
Embodiment 1:
(1) using vanadium trioxide and di-iron trioxide as initial feed, under reducing atmosphere, temperature is to roast at 1200 DEG C 48h obtains Fe2VO4
(2) to obtain pure vanadium iron spinelle in step (1) as raw material, it is fabricated to anode, the diameter of the anode is 10mm, With a thickness of 3mm or so.
(3) cell reaction carries out in normal temperature and pressure electrolytic cell, and the cathode material of the electrolytic cell is the graphite of diameter 6mm Stick, away from for 5cm, electrolyte solution is saturated oxalic acid solution for center between anode and cathode.
(4) tank voltage is chosen for 1V, and electromagnetic agitation speed is 500r/min, and electrolysis temperature is room temperature, and cell reaction is chosen For 1h.
(5) it after cell reaction, is separated by solid-liquid separation, is finally by the concentration that ICP-AES measures vanadium in leachate 775.2mg/L。
Embodiment 2:
(1) using vanadium trioxide and di-iron trioxide as initial feed, under reducing atmosphere, temperature is to roast at 1200 DEG C 48h obtains Fe2VO4
(2) to obtain pure vanadium iron spinelle in step (1) as raw material, it is fabricated to anode, the diameter of the anode is 10mm, With a thickness of 3mm or so.
(3) cell reaction carries out in normal temperature and pressure electrolytic cell, and the cathode material of the electrolytic cell is the graphite of diameter 6mm Stick, away from for 5cm, electrolyte solution is saturated oxalic acid solution for center between anode and cathode.
(4) tank voltage is chosen for 5V, and electromagnetic agitation speed is 500r/min, and electrolysis temperature is room temperature, and cell reaction is chosen For 1h.
(5) it after cell reaction, is separated by solid-liquid separation, is finally by the concentration that ICP-AES measures vanadium in leachate 1887mg/L。
Embodiment 3:
(1) using vanadium trioxide and di-iron trioxide as initial feed, under reducing atmosphere, temperature is to roast at 1200 DEG C 48h obtains Fe2VO4
(2) to obtain pure vanadium iron spinelle in step (1) as raw material, it is fabricated to anode, the diameter of the anode is 10mm, With a thickness of 3mm or so.
(3) cell reaction carries out in normal temperature and pressure electrolytic cell, and the cathode material of the electrolytic cell is the graphite of diameter 6mm Stick, away from for 5cm, electrolyte solution is saturated oxalic acid solution for center between anode and cathode.
(4) tank voltage is chosen for 10V, and electromagnetic agitation speed is 500r/min, and electrolysis temperature is room temperature, and cell reaction is chosen For 1h.
(5) it after cell reaction, is separated by solid-liquid separation, is finally by the concentration that ICP-AES measures vanadium in leachate 2754mg/L。
Embodiment 4:
(1) using vanadium iron spinel-type vanadium concentrate as initial feed, by vanadium concentrate ball milling granularity to 0.074mm or less.
(2) vanadium concentrate is in agate mortar after weighing the ball milling of 0.8g, and the poly-vinyl alcohol solution of 3 drop 5% of addition is (about It 0.1g) is sufficiently mixed uniformly, the type of being then pressed into is that diameter is 10mm, with a thickness of the round block of 3mm or so.
(3) manufactured round block is placed in high temperature furnace, roasts 6h at 800 DEG C of temperature, reducing atmosphere, is made with one Determine the anode of intensity and conduction.
(4) cell reaction carries out in normal temperature and pressure electrolytic cell;The cathode material of the electrolytic cell is the graphite of diameter 6mm Stick, away from for 5cm, electrolyte is saturated oxalic acid solution under room temperature for center between anode and cathode.
(5) tank voltage is chosen for 10V, and electromagnetic agitation speed is 500r/min, and electrolysis temperature is room temperature.
(6) after cell reaction starts, the relationship of record current and time, as a result as shown in Figure 3: it can be seen from the figure that In the past, current fluctuation is larger by 6500s, and cell reaction is violent, and after 6500s, electric current drops to 0.006A or so suddenly, due to electricity Flow through small, the electrolysis of vanadium is leached slow.After cell reaction, it is separated by solid-liquid separation.Leachate is measured finally by ICP-AES In vanadium concentration be 999.6mg/L.

Claims (8)

1. a kind of method of room temperature saturated oxalic acid solution Anodic electrolysis Leaching Vanadium, it is characterised in that the following steps are included: with vanadium Hercynite type concentrate containing vanadium is initial feed, it is mixed in a certain ratio with binder, is then pressed into type, in also Primordial Qi It is roasted under atmosphere, the anode of conductive energy is made;Using saturated oxalic acid solution as electrolyte, carry out being electrolysed at normal temperatures and pressures anti- It answers;Iron contained by electrolytic process Anodic and vanadium are oxidized to high valence ion, complex reaction occur with oxalate, finally with [Fe (C2O4)3]3-, VO2+Or/and [VO (C2O4)2]3-Form enters solution, [Fe (C2O4)3]3-[VO (C2O4)2]3-Promote vanadium concentrate The leaching of middle vanadium, while anode surface has free of contamination carbon dioxide gas to be precipitated, cathode has hydrogen precipitation;Cell reaction terminates Afterwards, it is separated by solid-liquid separation, obtains and contain vanadium leachate.
2. the method for room temperature saturated oxalic acid solution Anodic electrolysis Leaching Vanadium as described in claim 1, which is characterized in that the vanadium Hercynite type concentrate containing vanadium will carry out ball milling, until granularity is 0.074mm or less.
3. the method for room temperature saturated oxalic acid solution Anodic electrolysis Leaching Vanadium as described in claim 1, which is characterized in that described viscous Tie the polyvinyl alcohol that agent is mass fraction 5%, vanadium concentrate and binder be in mass ratio 5:1~10:1 after evenly mixing, then With the pressure compression moulding of 200~300MPa;The round block suppressed is placed in high temperature furnace and roasts 6h under reducing atmosphere, temperature It is 800 DEG C~1000 DEG C.
4. the method for room temperature saturated oxalic acid solution Anodic electrolysis Leaching Vanadium as claimed in claim 1 or 3, which is characterized in that vanadium The mass ratio of concentrate and binder is 8:1;Maturing temperature is 800 DEG C under reducing atmosphere.
5. the method for room temperature saturated oxalic acid solution Anodic electrolysis Leaching Vanadium as described in claim 1, which is characterized in that the electricity The electrolytic cell of solution reaction is normal temperature and pressure electrolytic cell, and electrolyte is saturated oxalic acid solution under room temperature, is contained with vanadium iron spinel-type Vanadium concentrate is anode, selects metal material or carbon material for cathode, and electrode shape is rodlike.
6. the method for room temperature saturated oxalic acid solution Anodic electrolysis Leaching Vanadium as described in claim 1 or 5, which is characterized in that institute It states cell reaction to carry out under electromagnetic agitation, the tank voltage of electrolysis is 5V~10V, and the cell reaction time is 5h~10h.
7. the method for room temperature saturated oxalic acid solution Anodic electrolysis Leaching Vanadium as described in claim 1, which is characterized in that the electricity In solution preocess, the higher conducting wire of the electric conductivity being connect with vanadium concentrate cannot with electrolyte solution contacts, to ensure that anode electrolysis is anti- It should occur on vanadium iron spinelle.
8. the method for room temperature saturated oxalic acid solution Anodic electrolysis Leaching Vanadium as described in claim 1, which is characterized in that electrolysis is anti- After answering, anode and cathode deionized water is rinsed 3~5 times, is then separated by solid-liquid separation, obtains and contains vanadium leachate.
CN201910454934.5A 2019-05-29 2019-05-29 Method for leaching vanadium by anode electrolysis in normal-temperature saturated oxalic acid solution Expired - Fee Related CN110117714B (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111041200A (en) * 2019-11-18 2020-04-21 北京科技大学 Method for leaching vanadium, titanium and chromium from vanadium, titanium and chromium raw materials by organic acid through hydrothermal method

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102134640A (en) * 2011-03-01 2011-07-27 重庆大学 Method for leaching vanadium slag in converter by electro-catalytic oxidation
CN102168178A (en) * 2011-04-15 2011-08-31 重庆大学 Method for extracting vanadium again from tailing after extracting vanadium from vanadium tailing of converter
CN102534229A (en) * 2011-12-08 2012-07-04 重庆大学 Method for selectively leaching vanadium from vanadium-bearing converter slag
CN103436912A (en) * 2013-07-22 2013-12-11 彩虹集团公司 Synthetic method for preparing iron(II) acetate by electrolysis
CN106282563A (en) * 2016-08-31 2017-01-04 河北钢铁股份有限公司承德分公司 A kind of method utilizing solution containing vanadium directly to prepare barium oxide
CN107904613A (en) * 2017-11-27 2018-04-13 西北矿冶研究院 Method for recycling nickel-cobalt valuable metal from nickel-cobalt-iron high-temperature alloy

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102134640A (en) * 2011-03-01 2011-07-27 重庆大学 Method for leaching vanadium slag in converter by electro-catalytic oxidation
CN102168178A (en) * 2011-04-15 2011-08-31 重庆大学 Method for extracting vanadium again from tailing after extracting vanadium from vanadium tailing of converter
CN102534229A (en) * 2011-12-08 2012-07-04 重庆大学 Method for selectively leaching vanadium from vanadium-bearing converter slag
CN103436912A (en) * 2013-07-22 2013-12-11 彩虹集团公司 Synthetic method for preparing iron(II) acetate by electrolysis
CN106282563A (en) * 2016-08-31 2017-01-04 河北钢铁股份有限公司承德分公司 A kind of method utilizing solution containing vanadium directly to prepare barium oxide
CN107904613A (en) * 2017-11-27 2018-04-13 西北矿冶研究院 Method for recycling nickel-cobalt valuable metal from nickel-cobalt-iron high-temperature alloy

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
许孟春: "提钒尾渣浸出行为的实验研究", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111041200A (en) * 2019-11-18 2020-04-21 北京科技大学 Method for leaching vanadium, titanium and chromium from vanadium, titanium and chromium raw materials by organic acid through hydrothermal method
CN111041200B (en) * 2019-11-18 2021-02-19 北京科技大学 Method for leaching vanadium, titanium and chromium from vanadium, titanium and chromium raw materials by organic acid through hydrothermal method

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