CN106086441A - The method of Vanadium fluidization vanadium extraction - Google Patents

The method of Vanadium fluidization vanadium extraction Download PDF

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Publication number
CN106086441A
CN106086441A CN201610659452.XA CN201610659452A CN106086441A CN 106086441 A CN106086441 A CN 106086441A CN 201610659452 A CN201610659452 A CN 201610659452A CN 106086441 A CN106086441 A CN 106086441A
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vanadium
fluidization
extraction
passed
reaction column
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CN106086441B (en
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郭继科
付自碧
殷兆迁
李明
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Pangang Group Panzhihua Iron and Steel Research Institute Co Ltd
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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
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B34/00—Obtaining refractory metals
    • C22B34/20—Obtaining niobium, tantalum or vanadium
    • C22B34/22—Obtaining vanadium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
    • C22B7/006—Wet processes
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/20—Recycling

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Metallurgy (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Organic Chemistry (AREA)
  • Geology (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Manufacture And Refinement Of Metals (AREA)
  • Processing Of Solid Wastes (AREA)

Abstract

The invention belongs to vanadium extraction chemical technology field, a kind of method being specifically related to Vanadium fluidization vanadium extraction.For silicon, sodium content height in Vanadium, during vanadium extraction, the floccule in solid phase or jelly are too much, cause filtration, washing difficulty, and after washing, the total content of vanadium of residue and soluble vanadium content are the highest, the problems such as V leaching rate is low, the present invention provides a kind of method of Vanadium fluidization vanadium extraction.Vanadium is added in reaction column by the inventive method, and the hot water and air being passed through 90～100 DEG C carries out extraction reaction, stands, thus floccule, leachate and vanadium slag are effectively separated after extraction.The method of the present invention efficiently separates floccule or jelly in solution, and solution leaching residue TV and SV content is higher, filtration time is longer, Leaching Vanadium liquid concentration is limited etc. produces problem, and leaching rate is high, and technique simply, easily operates, saving production cost.

Description

The method of Vanadium fluidization vanadium extraction
Technical field
The invention belongs to vanadium extraction chemical technology field, a kind of method relating to Vanadium fluidization vanadium extraction.
Background technology
At present, from vanadium slag, the method for vanadium extraction mainly has: sodium roasting-water logging or alkali leaching；Calcification baking-acidleach；Directly The techniques such as acidleach, its objective is the vanadium existence changed in solid phase, so that it discharges from Spinel and goes forward side by side one Step oxidation, is converted into the vanadate dissolved in acid solution, alkali liquor or aqueous solution, separates with vanadium slag system impurity realizing vanadium. During vanadium slag sodium roasting, because its temperature is higher, sodium salt addition is more, and the impurity such as silicon in vanadium slag, chromium, phosphorus, ferrum is also led To enter in solution with sodium-salt form；In leaching process, pH value of solution is higher, and general pH is about 10, vanadium concentration in leachate During lifting, Na ion concentration is with certain proportion Synchronous lifting, and solution viscosity increases, concurrently form based on silicate Floccule or jelly increase, be mainly scattered in slag mutually among, during filtration, easily blocking cake filtration layer micropore and filter cloth Hole, causes strainability, scourability to be deteriorated；Additionally, due to the dissolving of vanadate raises with temperature and increases, industrial needs Use about 90 DEG C hot water to carry out leaching, laundry operation, high temperature increases solution viscosity coefficient further, thus deteriorates further Solution filtration, scourability, cause grog leaching effect, the residual washing-out effect to be deteriorated.Leach using tradition slot type, wash During equipment, the bed of material is thick, and duty cycle is long, only washs and just needs about 60min, and in residue, TV content and SV content are the highest, point It is not 1.20% and about 0.20%；Use band filter to carry out leaching, laundry operation time, duty cycle is shorter, and residue is washed Washing effect the most limited, in residue, TV content is in about 1.30%, and SV content is in about 0.30%.
Vanadium slag is after sodium roasting, and silicon in grog, sodium content are the highest, the floccule in solid phase or jelly during vanadium extraction Too much, it is not easy to filter and wash, the washing total content of vanadium of residue and soluble vanadium content are the highest, and V leaching rate is low.
The present invention intends providing a kind of Vanadium extraction vanadium method, carries out vanadium extraction by fluidization technology, solves above-mentioned asking Topic.
Summary of the invention
The technical problem to be solved in the present invention is silicon in Vanadium, sodium content height, the floccule in solid phase during vanadium extraction Or jelly is too much, it is not easy to filter and wash, after washing, the total content of vanadium of residue and soluble vanadium content are the highest, V leaching rate Low.
The present invention solve technical problem technical scheme be provide a kind of Vanadium fluidization vanadium extraction method, including with Lower step:
A, Vanadium is added in reaction column；
B, it is passed through the water of 90～100 DEG C from reaction column lower end inlet；
C, after b step terminates, from reaction column lower end, air inlet is passed through air；
D, after step c terminates, stand, siphon obtains floccule and leachate, filters floccule and leachate respectively；
E, after Step d terminates, pour out slip in reaction column, with in step d filter after filtering residue mix, wash, filter, Vanadium slag after being extracted.
Wherein, in the method for above-mentioned fluidization vanadium extraction, vanadium slag described in step a is SiO2Content 13～20wt%, Na2O content The vanadium slag of 6～10wt%.
Wherein, in the method for above-mentioned fluidization vanadium extraction, vanadium slag addition described in step a is that vanadium slag height accounts for reaction column height 5～15%.
Wherein, in the method for above-mentioned fluidization vanadium extraction, vanadium slag granularity described in step a be 240 mesh siftage account for 70～ 90wt%.
Wherein, in the method for above-mentioned fluidization vanadium extraction, the volume being passed through water described in step b is as the criterion to fill reaction column.
Wherein, in the method for above-mentioned fluidization vanadium extraction, being slowly introducing when being passed through water described in step b, the flow velocity being passed through water is 0.18～0.50m/s.
Wherein, in the method for above-mentioned fluidization vanadium extraction, step a and step b are carried out simultaneously.
Wherein, in the method for above-mentioned fluidization vanadium extraction, step c is passed through air themperature >=90 DEG C of reaction column, makes Air Temperature The method spending >=90 DEG C is: the air of reaction column first passes through a there-necked flask, and flask is built with the boiling warm of 2/3 volume Water.
Wherein, in the method for above-mentioned fluidization vanadium extraction, it is 21.37～28.49m/ that step c is passed through the air velocity of reaction column S, is passed through air time 5～10min.
Wherein, in the method for above-mentioned fluidization vanadium extraction, time of repose described in step d is 0.5～3min.
Wherein, in the method for above-mentioned fluidization vanadium extraction, before step e, first it is passed through 90～100 DEG C of water washs, be passed through Water flow velocity is 0.57～1.78m/s, and the volume being passed through water is as the criterion to fill reaction column.
Wherein, in the method for above-mentioned fluidization vanadium extraction, the liquid after filtering described in step e and washing returns in step b Recycle.
Wherein, in the method for above-mentioned fluidization vanadium extraction, can implement with the series connection of multiple reaction columns.
The invention have the benefit that the present invention uses fluidization principle, vanadium slag sodium grog leached, filter, wash, Utilize the absorption between gas rolling action, floccule or jelly and material difference of specific gravity, floccule or jelly, reunion etc. Principle, efficiently separates floccule or jelly in solution, solves to leach residue TV and SV content is higher, filtration time is longer, leaching Go out vanadium liquid concentration production problem such as limited grade.The inventive method vanadium extraction concentration is high, vanadium concentration ＞ in the sodium vanadium liquid after vanadium slag leaching During 30g/L the most applicable.And extraction time is short, it is not necessary to mechanical agitation；The rate of filtration is fast, residual washing-out ratio more thoroughly, in residue TV≤1.00%, SV≤0.10%；Leaching rate is high, and V leaching rate reaches more than 98%；The inventive method technique is simply, easily grasp Making, cleaning mixture can recycle in system, reduces water consumption.
Detailed description of the invention
The present invention provides a kind of method of Vanadium fluidization vanadium extraction, comprises the following steps:
A, Vanadium is added in reaction column；
B, it is passed through the water of 90～100 DEG C from reaction column lower end inlet；
C, after b step terminates, from reaction column lower end, air inlet is passed through air；
D, after step c terminates, stand, siphon obtains floccule and leachate, filters floccule and leachate respectively；
E, after Step d terminates, pour out slip in reaction column, with in step d filter after filtering residue mix, wash, filter, Vanadium slag after being extracted.
The present invention by sodium grog is leached, filters, washs, utilize gas rolling action, floccule or jelly with Absorption between material difference of specific gravity, floccule or jelly, reunion, efficiently separate floccule or jelly in solution, solves Leaching residue TV and SV content is higher, filtration time is longer, Leaching Vanadium liquid concentration is limited etc. produces problem.
The method of the present invention is applicable to SiO2Content 13～20wt%, Na2The vanadium slag of O content 6～10wt%, in order to make leaching Going out rate to improve, the granularity requirements of vanadium slag is relatively thin, and inventor finds through lot of experiments, when vanadium slag 240 mesh siftage account for 70～ When 90%, extraction rate is the highest.Meanwhile, the addition of vanadium slag also has influence on extracting effect, and addition should not mistake when extraction for vanadium slag Many, when addition is too much, it can not effectively be stirred by water and air, forms solid liquid phase three-phase flow, and leaching effect is bad, To this end, the vanadium slag height that vanadium slag addition is set in reaction column by inventor accounts for the 5～15% of reaction column height.
The present invention is passed through water and air in vanadium slag, and requires the temperature of water and air all more than 90 DEG C, and material needs Full and uniform with aqueous solution mix, and ensure certain stirring condition, could realize leaching chemical reaction.Leach reaction needs one Fixed temperature, effectively provides heat source for reaction with the hot water of more than 90 DEG C, is passed through 90 DEG C of air above and on the one hand provides reaction Thermal source, on the one hand can also add strong mixing, makes leaching reaction more thorough.For avoiding the occurrence of channel, bed material shifting on the whole etc., Being passed through of hot water and air is desirable that control speed, and the flow velocity being passed through water in step b is 0.18～0.50m/s, and step c is passed through instead The air velocity of Ying Zhu is 21.37～28.49m/s, when washing before step e, be passed through the flow velocity of water be 0.57～ 1.78m/s；The flow being passed through water and air varies in size according to reaction column and different, is passed through the flow of water and air equal to flow velocity Product with reaction column sectional area.
Being passed through after hot water and air carries out leaching reaction, need to stand a period of time, during standing, residue density is big, About 1.4g/cm3, can first be deposited in bottom；Floccule density is little, after a period of time reunites mutually, adsorbs formed lamellar or Bulk floccule, density about 0.2g/cm3, then it is deposited in residue surface；So, foot is residue, and middle part is floccule, Top is leachate, thus floccule, residue and lixiviating solution is efficiently separated, and uses siphon to discharge floccule and leaching Go out liquid, individually filter floccule and leachate, thus avoid floccule to residue when filtration washing residue and leachate filtering residue Filtration and washing impact, save the filtration washing time, saved Financial cost.
Below in conjunction with embodiment, the detailed description of the invention of the present invention is further described, the most therefore the present invention is limited System is among described example ranges.
Grog used by embodiment and comparative example is vanadium slag product after sodium roasting, and its component content and particle diameter see table 1；In embodiment, separator used is conventional liquid-solid fluidization reactor, and reaction column internal diameter is 4.0～4.1cm.
The composition of table 1 grog and content and particle diameter
Embodiment 1 technical solution of the present invention carries out fluidization vanadium extraction
Take 250g grog to add in reaction column, be passed through 400mL temperature >=90 DEG C hot water, air-blowing 5min in 5min, control sky About throughput 7L/min；Stand 1min, use siphon mode to obtain floccule, leachate, filter respectively；To reaction in 2min 500mL temperature >=90 DEG C hot water it is passed through in post；In reaction column, slip is crossed after filtering residue mixes with leachate and is filtered, and uses hot water Washing, water temperature controls at about 90 DEG C, leaching requirement 400mL.
After vanadium extraction terminates, it is thus achieved that leachate 350mL, TV are 29.28g/L, residue (dry weight) 215g, TV are 0.85%, SV Being 0.086%, floccule (dry weight) 0.097g, TV are 1.52%, and calculating leaching rate is 98.21%.
Embodiment 2 technical solution of the present invention carries out fluidization vanadium extraction
Take 250g grog to add in reaction column, be passed through 400mL temperature >=90 DEG C mixing vanadium liquid in 3min (in Example 1 Cleaning solution for removing residue mix with leachate, TV is 25.00g/L), air-blowing 8min, control about air mass flow 7L/min；Stand 30s, uses siphon mode to obtain floccule, leachate, filters respectively；In reaction column, 500mL temperature >=90 it are passed through in 2min DEG C hot water；In reaction column, slip is crossed after filtering residue mixes with leachate and is filtered, and uses hot water to wash, and water temperature controls 90 About DEG C, leaching requirement 400mL.
After vanadium extraction terminates, it is thus achieved that leachate 345mL, TV are 56.69g/L, residue (dry weight) 220g, TV are 0.89%, SV Being 0.091%, floccule (dry weight) 0.121g, TV are 2.03%, and calculating leaching rate is 99.02%.
Embodiment 3 technical solution of the present invention carries out fluidization vanadium extraction
Take 250g grog to add in reaction column, be passed through 400mL temperature >=90 DEG C hot water, air-blowing 7min in 5min, control sky About throughput 7L/min；Stand 55s, use siphon mode to obtain floccule；Filter after row outside slip in reaction column, adopt Washing with hot water, water temperature controls at about 90 DEG C, leaching requirement 400mL.
After vanadium extraction terminates, it is thus achieved that leachate 362mL, TV are 28.30g/L, residue (dry weight) 209g, TV are 0.91%, SV Being 0.088%, floccule (dry weight) 0.105g, TV are 1.61%, and calculating leaching rate is 98.22%.
Comparative example 4 carries out Leaching of Vanadium from Vanadium slag without fluidization process
Take 250g grog and put in beaker, add 400mL temperature >=90 DEG C hot water, be stirred leaching, control water temperature steady Fixed >=90 DEG C, leach 30min, with 500mL temperature >=90 DEG C hot water repeatedly washing by soaking, it is thus achieved that leachate 355mL, TV are 28.31g/L, residue (dry weight) 212g, TV are 1.13%, and SV is 0.120%, and calculating leaching rate is 97.54%.
Compliance test result
Filter the time difference of leachate and filtered wash solution for contrast, embodiment 1～3 was carried out after being siphoned off floccule Filter, washing, compare with comparative example 4, it is ensured that slag blanket thickness is 1.10cm, and leachate volume is 300mL, cleaning mixture volume Being 400mL, by gas diverter, control sucking filtration machine pressure and be-0.05MPa, comparing result is shown in Table 2.
Table 2 filters the timetable of leachate and cleaning mixture
Filter leachate time/s Filtered wash solution time/s
Embodiment 1 35 40
Embodiment 2 61 75
Embodiment 3 50 60
Comparative example 4 110 130
From embodiment 1～3 and comparative example 4, carrying out the fluidization vanadium extraction of vanadium slag by technical solution of the present invention, vanadium extraction is soaked Going out rate high, can reach about 99%, and use conventional methods vanadium extraction, leaching rate is less than the present invention；Leach simultaneously as conventional For leaching, the floccule produced in leaching process is dispersed in leachate and residue, easily blocking filter course micropore and filter Paper micropore, filter, clean result poor, filtration time is long, and the present invention can be previously isolated from floccule, then refilters, washs, mistake The filter time is greatly decreased, and improves production efficiency, has saved production cost greatly.

Claims (10)

1. the method for Vanadium fluidization vanadium extraction, it is characterised in that comprise the following steps:
A, Vanadium is added in reaction column；
B, it is passed through the water of 90～100 DEG C from reaction column lower end inlet；
C, after b step terminates, from reaction column lower end, air inlet is passed through air；
D, after step c terminates, stand, siphon obtains floccule and leachate, filters floccule and leachate respectively；
E, after Step d terminates, pour out slip in reaction column, with in step d filter after filtering residue mix, wash, filter, obtain Vanadium slag after extraction.
The method of Vanadium fluidization vanadium extraction the most according to claim 1, it is characterised in that: vanadium slag described in step a is SiO2Content 13～20wt%, Na2The vanadium slag of O content 6～10wt%.
The method of Vanadium fluidization vanadium extraction the most according to claim 1 and 2, it is characterised in that: vanadium slag described in step a Addition is that vanadium slag height accounts for the 5～15% of reaction column height.
4. according to the method for the Vanadium fluidization vanadium extraction described in any one of claims 1 to 3, it is characterised in that: step a institute Stating vanadium slag granularity is that 240 mesh siftage account for 70～90wt%.
5. according to the method for the Vanadium fluidization vanadium extraction described in any one of Claims 1 to 4, it is characterised in that: step b institute Stating the volume being passed through water to be as the criterion to fill reaction column, the flow velocity being passed through water is 0.18～0.50m/s.
6. according to the method for the Vanadium fluidization vanadium extraction described in any one of Claims 1 to 5, it is characterised in that: step c is led to Entering air themperature >=90 DEG C of reaction column, being passed through air velocity is 21.37～28.49m/s, is passed through air time 5～10min.
7. according to the method for the Vanadium fluidization vanadium extraction described in any one of claim 1～6, it is characterised in that: step d institute Stating time of repose is 0.5～3min.
8. according to the method for the Vanadium fluidization vanadium extraction described in any one of claim 1～7, it is characterised in that: in step e First being passed through 90～100 DEG C of water from lower end inlet to wash, the flow velocity being passed through water is 0.57～1.78m/s, is passed through water before Volume be as the criterion to fill reaction column.
9. according to the method for the Vanadium fluidization vanadium extraction described in any one of claim 1～8, it is characterised in that: step e institute Using 90～100 DEG C of water washings when stating slip washing, leaching requirement is with step b institute water consumption.
10. according to the method for the Vanadium fluidization vanadium extraction described in any one of claim 1～9, it is characterised in that: step e Described in filter and wash after liquid return in step b and recycle.
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109913661A (en) * 2019-04-25 2019-06-21 河钢股份有限公司承德分公司 A method of from extraction sulphur and vanadium in desulfurization slag containing vanadium
CN114291879A (en) * 2021-11-23 2022-04-08 攀钢集团研究院有限公司 Preparation method of aluminum silicate

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Publication number Priority date Publication date Assignee Title
RU2096510C1 (en) * 1996-06-07 1997-11-20 Гусейн Бахлул Садыхов Method of recovering vanadium from titanium-containing slags
CN1235201A (en) * 1998-05-08 1999-11-17 湖南省煤炭科学研究所 Method for adsorption of vanadium by resin
CN103710552A (en) * 2013-12-26 2014-04-09 中信锦州金属股份有限公司 Leaching technique and system for preparing vanadium solution by quenching vanadium slag roasting clinker
CN105671306A (en) * 2016-03-21 2016-06-15 攀钢集团攀枝花钢铁研究院有限公司 Method for separating iron, vanadium and titanium in vanadic titanomagnetite

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
RU2096510C1 (en) * 1996-06-07 1997-11-20 Гусейн Бахлул Садыхов Method of recovering vanadium from titanium-containing slags
CN1235201A (en) * 1998-05-08 1999-11-17 湖南省煤炭科学研究所 Method for adsorption of vanadium by resin
CN103710552A (en) * 2013-12-26 2014-04-09 中信锦州金属股份有限公司 Leaching technique and system for preparing vanadium solution by quenching vanadium slag roasting clinker
CN105671306A (en) * 2016-03-21 2016-06-15 攀钢集团攀枝花钢铁研究院有限公司 Method for separating iron, vanadium and titanium in vanadic titanomagnetite

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109913661A (en) * 2019-04-25 2019-06-21 河钢股份有限公司承德分公司 A method of from extraction sulphur and vanadium in desulfurization slag containing vanadium
CN114291879A (en) * 2021-11-23 2022-04-08 攀钢集团研究院有限公司 Preparation method of aluminum silicate
CN114291879B (en) * 2021-11-23 2023-09-05 攀钢集团研究院有限公司 Preparation method of aluminum silicate

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