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CN105803198A - Method of extracting high-purity V2O5 in dilute sulfuric acid leaching solution of stone coal vanadium ore calcine by adopting normal-temperature direct precipitation method - Google Patents

Method of extracting high-purity V2O5 in dilute sulfuric acid leaching solution of stone coal vanadium ore calcine by adopting normal-temperature direct precipitation method Download PDF

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Publication number
CN105803198A
CN105803198A CN201610156580.2A CN201610156580A CN105803198A CN 105803198 A CN105803198 A CN 105803198A CN 201610156580 A CN201610156580 A CN 201610156580A CN 105803198 A CN105803198 A CN 105803198A
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vanadium
sulfuric acid
dilute sulfuric
purity
calcining
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杨道印
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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
    • C22B3/44—Treatment or purification of solutions, e.g. obtained by leaching by chemical processes
    • 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
    • C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
    • C22B3/06—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic acid solutions, e.g. with acids generated in situ; in inorganic salt solutions other than ammonium salt solutions
    • C22B3/08—Sulfuric acid, other sulfurated acids or salts thereof
    • 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
    • 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)
  • Manufacturing & Machinery (AREA)
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  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • General Life Sciences & Earth Sciences (AREA)
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  • Inorganic Compounds Of Heavy Metals (AREA)

Abstract

The invention provides a method of extracting high-purity V2O5 in a dilute sulfuric acid leaching solution of stone coal vanadium ore calcine by adopting a normal-temperature direct precipitation method. The technological process comprises the following steps of (1) crushing, grinding and roasting stone coal vanadium ores; (2) carrying out circulation trickle leaching or multi-segment stirring leaching of the stone coal vanadium ore calcine with the dilute sulfuric acid; (3) filtering to obtain a leaching solution with the vanadium concentration to be larger than 6.0g/L; (4) directly adding a complex depositing agent into the dilute sulfuric acid leaching solution under the ambient temperature condition without removing impurities, and obtaining precipitates, wherein the vanadium precipitation rate is larger than or equal to 95 percent; (5) dissolving the precipitates with alkali, separating vanadium from the impurities through filtering, and leaving the vanadium in a filtrate, wherein the vanadium dissolution rate is larger than or equal to 95 percent; (6) enabling the cooled filtrate to react with an ammonium salt to produce ammonium metavanadate, wherein the vanadium precipitation rate is larger than or equal to 99 percent; (7) washing the ammonium metavanadate so as to improve the quality of the vanadium; and (8) calcining the ammonium metavanadate to prepare the high-purity vanadium pentoxide, wherein the quality of the V2O5 is larger than 99 percent. The method has the advantages of short technological process, simpleness and convenience in procedure, simpleness in operation, higher work efficiency, lower production cost, further lowering environmental pollution and the like.

Description

Bone coal navajoite calcining dilute sulfuric acid leachate room temperature direct precipitation method extracts high-purity V2O5
Technical field
The present invention relates to a kind of employing room temperature direct precipitation method high-purity V of extraction from bone coal navajoite calcining dilute sulfuric acid leachate2O5Method.Belong to field of hydrometallurgy.
Background technology
For bone coal navajoite sulphuric leachate, generally after pretreatment in commercial production, adopt multi-stage counter current extraction or the physical method Vanadium Concentrationin such as ion-exchange absorption is attached, be then hydrolyzed precipitation again.Hydrolysis precipitation is typically in 90 DEG C and carries out to fluidized state, gained V2O5Purity is not high, and sewage quantity is big.
When being enriched with chemical method, that generally to pass through complexity removes the cleaning procedure such as silicon, dephosphorization, and requires that precipitation temperature controls at 95 DEG C to fluidized state.
At present, under normal temperature condition, direct precipitation technique is used for stone coal sodium roasting infusion, but vanadium recovery is relatively low, and quality is not high.
The problem such as above method all exists technological process length, complex procedures, technical parameter is wayward, energy consumption is high, work efficiency is low, product quality is not high, wastewater treatment capacity is big and benefit is low.
The present invention is directed to bone coal navajoite calcining dilute sulfuric acid leachate, at normal temperatures, directly (without remove impurity) leaching liquid, add compound precipitants and also adjust pH, it is thus achieved that polyoxovanadate (includes the impurity such as part aluminium salt, phosphate) precipitate；With alkaline matter dissolution precipitation thing and adjust pH, it is separated by filtration impurity；Ammonium metavanadate is obtained by ammonium salt precipitation containing vanadium filtrate；Washing ammonium metavanadate；In oxidizing atmosphere, calcinations of ammonium metavanadate prepares high purity vanadic anhydride, V2O5Quality > 99%.
Summary of the invention
It is an object of the invention to provide a kind of employing room temperature direct precipitation method high-purity V of extraction from bone coal navajoite calcining dilute sulfuric acid leachate2O5Method, its technological process is short, operation is easy, simple to operate, can improve work efficiency, reduces energy consumption, improve product quality and reduce environmental pollution.
Present invention room temperature direct precipitation method from bone coal navajoite calcining dilute sulfuric acid leachate extracts high-purity V2O5Method, it is characterised in that comprise the steps of successively
(1) undertaken bone coal navajoite crushing, grinding, grinding particle size > 60 order；
(2) roasting bone coal navajoite in oxidizing atmosphere, temperature 750 DEG C～900 DEG C；
(3) calcining dilute sulfuric acid leaches, and sulfuric acid dosage is the 1～8% of stone coal mine quality, liquid-solid ratio=3: 1～1: 1, and leaching or multistage leaching, leaching time 2～8h are drenched in room temperature circulation；
(4) acquisition dilute sulfuric acid leachate, leachate vanadium concentration > 6.0g/L are filtered；
(5) under normal temperature condition, without remove impurity, for obtaining higher vanadium rate of deposition, in step (4) leachate, directly add ammonium salt class compound precipitants, adjusting and controlling pH is 3.0～6.5, it is thus achieved that polyoxovanadate (includes the impurity such as part aluminium salt, phosphate) precipitate.Wherein compound precipitants is (NH4)2SO4、NH4HSO4、NH4Cl、NH4NO3、(NH4)2HPO4、(NH4)3PO4、NH4HCO3、(NH4)2CO3、NH4Two kinds in F and ammonia combine.Effective reaction time 1～5h, vanadium rate of deposition >=95%.
(6) according to content of vanadium in step (5) precipitate, calculating amount of water, make solution vanadium concentration > 20g/L, and heated by solution to 40～80 DEG C, adding alkaline matter adjustment pH is 8～9, effective reaction time 0.5～3h.Wherein alkaline matter is ammonia, Ca(OH)2、NaOH, KOH and Na2CO3In one.
(7) aqueous slkali is filtered, by vanadium and magazins' layout, it is thus achieved that alkalescence metavanadate filtrate, molten yield >=95% of vanadium；
(8) after filtrate cooling in step (7), ammonium metavanadate, precipitation rate >=99% are generated with ammonium salt effect.Wherein ammonium salt is the one in ammonium chloride, ammonium sulfate.
(9) washing ammonium metavanadate is to improve vanadium quality.Wherein cleaning mixture is the one in industrial process waters, pure water, 1～3% ammonium chloride solution and 1～3% ammonium sulfate.
(10) oxidizing atmosphere calcination ammonium metavanadate prepares high purity vanadic anhydride, calcination temperature 400 DEG C～600 DEG C, V2O5Quality > 99%.
Present invention have the advantage that
1, room temperature direct precipitation method Vanadium Concentrationin.Under normal temperature condition, do not need complicated remove impurity operation, Direct precipitation Vanadium Concentrationin for bone coal calcining dilute sulfuric acid leachate.
2, can effectively vanadium in polyoxovanadate precipitate be separated with impurity etc..
3、V2O5Quality > 99%.
4, technological process is short, and operation is easy, and effective reaction time is short, and work efficiency is high.
5, technical parameter is reliable and stable, workable, it is easy to realize industrial automation.
6, producing equipment simple, except the broken mill of bone coal navajoite, roasting, leaching and calcination ammonium metavanadate, all the other respectively walk capital equipment and have only to settling tank and pressure filter.
7, reagent material is cheap, and production cost is relatively low.
8, environmental friendliness.In industrialized production of the present invention, water consumption is few and can recycle；Slag is relative " totally " after extracting useful element, can as building materials or for mining area backfill second ploughing；Reduce environmental pollution further.
Accompanying drawing: bone coal navajoite calcining dilute sulfuric acid leachate room temperature direct precipitation method extracts high-purity V2O5Flow chart
Detailed description of the invention
Below in conjunction with embodiment, the invention will be further described, and following example are intended to illustrate the present invention rather than limitation of the invention further.
Embodiment 1
Take containing V2O58.56g/L、Si0.11g/L、Fe< 0.05g/L, Al1.92g/L, P2.13g/L and pH1.5 bone coal calcining dilute sulfuric acid leachate 500ml, under normal temperature condition, be directly added into compound precipitants, adjusting pH value of solution is 6.5, effective reaction time 5h, vanadium rate of deposition 95.7%.According to content of vanadium in precipitate, calculating amount of water, making solution vanadium concentration is 30g/L.Being heated by solution to 80 DEG C, adding alkaline matter adjustment pH is 8～9, effective reaction time 3h.Filtering aqueous slkali, vanadium is stayed in filtrate, the molten yield 95.8% of vanadium；After filtrate cools down, add ammonium salt generate ammonium metavanadate, precipitation rate 99.5%；Washing ammonium metavanadate；Oxidizing atmosphere is calcined ammonium metavanadate and prepares high purity vanadic anhydride, V2O5Quality 99.89%.
Embodiment 2
Take containing V2O516.26g/L、Si0.12g/L、Fe< 0.05g/L, Al2.27g/L, P2.98g/L and pH1.3 bone coal calcining two-stage nitration dilute sulfuric acid leachate 1000ml, under normal temperature condition, being directly added into compound precipitants, adjusting pH value of solution is 6.0, effective reaction time 3h, vanadium rate of deposition is 97.3%.According to content of vanadium in precipitate, calculating amount of water, making solution vanadium concentration is 45g/L.Being heated by solution to 70 DEG C, adding alkaline matter adjustment pH is 8～9, effective reaction time 3h.Filtering aqueous slkali, vanadium is stayed in filtrate, and the molten yield of vanadium is 96.8%；After filtrate cools down, add ammonium salt generate ammonium metavanadate, precipitation rate 99.7%；Washing ammonium metavanadate；Oxidizing atmosphere is calcined ammonium metavanadate and prepares high purity vanadic anhydride, V2O5Quality 99.92%.
Embodiment 3
Take containing V2O525.55g/L、Si0.12g/L、Fe< 0.05g/L, Al3.35g/L, P4.37g/L and pH1.0 three sections of dilute sulfuric acid leachate 1000ml of bone coal calcining, under normal temperature condition, being directly added into compound precipitants, adjusting pH value of solution is 5.5, effective reaction time 3h, vanadium rate of deposition is 99.4%.According to content of vanadium in precipitate, calculating amount of water, making solution vanadium concentration is 35g/L.Being heated by solution to 50 DEG C, adding alkaline matter adjustment pH is 8～9, effective reaction time 3h.Filtering aqueous slkali, vanadium is stayed in filtrate, and the molten yield of vanadium is 97.4%；After filtrate cools down, add ammonium salt generate ammonium metavanadate, precipitation rate 99.8%；Washing ammonium metavanadate；Oxidizing atmosphere is calcined ammonium metavanadate and prepares high purity vanadic anhydride, V2O5Quality 99.87%.
Embodiment 4
Take containing V2O58.98g/L、Si0.15g/L、Fe< 0.05g/L, Al2.28g/L, P2.35g/L and pH1.33 bone coal calcining dilute sulfuric acid circulation drench immersion 19m3, under normal temperature condition, it is directly added into compound precipitants, adjusting pH value of solution is 6.5, and effective reaction time 3h, vanadium rate of deposition is 96.5%.According to content of vanadium in precipitate, calculating amount of water, making solution vanadium concentration is 42g/L.Being heated by solution to 70 DEG C, adding alkaline matter adjustment pH is 8～9, effective reaction time 3h.Filtering aqueous slkali, vanadium is stayed in filtrate, and the molten yield of vanadium is 95.6%；After filtrate cools down, add ammonium salt generate ammonium metavanadate, precipitation rate 99.6%；Washing ammonium metavanadate；Oxidizing atmosphere is calcined ammonium metavanadate and prepares high purity vanadic anhydride, V2O5Quality 99.87%.
The invention is not restricted to above-described embodiment, for persons skilled in the art, any apparent change under the premise without departing substantially from the principle of the invention, it done, broadly fall into the protection domain of claims of the present invention.

Claims (9)

1. the high-purity V of room temperature direct precipitation method extraction from bone coal navajoite calcining dilute sulfuric acid leachate2O5Method, it is characterised in that comprise the steps of successively
(1) undertaken bone coal navajoite crushing, grinding, grinding particle size > 60 order；
(2) roasting bone coal navajoite in oxidizing atmosphere；
(3) calcining dilute sulfuric acid leaches；
(4) acquisition dilute sulfuric acid leachate, leachate vanadium concentration > 6.0g/L are filtered；
(5) under normal temperature condition, it is not necessary to remove impurity, for obtaining higher vanadium rate of deposition, directly adding compound precipitants in step (4) dilute sulfuric acid leachate, adjusting and controlling pH is 3.0～6.5, it is thus achieved that precipitate.Vanadium rate of deposition >=95%.
(6) according to content of vanadium in step (5) precipitate, calculating amount of water, make solution vanadium concentration > 20g/L, and heated by solution to 40～80 DEG C, adding alkaline matter adjustment pH is 8～9.
(7) filtering aqueous slkali, by vanadium and magazins' layout, vanadium is stayed in filtrate, molten yield >=95% of vanadium；
(8) after filtrate cooling in step (7), ammonium metavanadate, precipitation rate >=99% are generated with ammonium salt effect.
(9) washing ammonium metavanadate is to improve vanadium quality.
(10) oxidizing atmosphere calcination ammonium metavanadate prepares high purity vanadic anhydride, V2O5Quality > 99%.
2. one according to claim 1 room temperature direct precipitation method from bone coal navajoite calcining dilute sulfuric acid leachate extracts high-purity V2O5Method, it is characterised in that: bone coal navajoite torrefaction temperature 650 DEG C～900 DEG C in (2).
3. one according to claim 1 room temperature direct precipitation method from bone coal navajoite calcining dilute sulfuric acid leachate extracts high-purity V2O5Method, it is characterised in that: in (3) calcining with dilute sulfuric acid room temperature circulation drench leaching or multistage leaching, sulfuric acid dosage is the 1～8% of bone coal navajoite quality.
4. one according to claim 1 room temperature direct precipitation method from bone coal navajoite calcining dilute sulfuric acid leachate extracts high-purity V2O5Method, it is characterised in that: in (5), compound precipitants is (NH4)2SO4、NH4HSO4、NH4Cl、NH4NO3、(NH4)2HPO4、(NH4)3PO4、NH4HCO3、(NH4)2CO3、NH4Two kinds in F and ammonia combine.
5. one according to claim 1 room temperature direct precipitation method from bone coal navajoite calcining dilute sulfuric acid leachate extracts high-purity V2O5Method, it is characterised in that: (6) neutral and alkali material is ammonia, Ca(OH)2、NaOH, KOH and Na2CO3In one as pH adjusting agent.
6. one according to claim 1 room temperature direct precipitation method from bone coal navajoite calcining dilute sulfuric acid leachate extracts high-purity V2O5Method, it is characterised in that: filtering aqueous slkali in (7), by vanadium and magazins' layout, vanadium is stayed in filtrate.
7. one according to claim 1 room temperature direct precipitation method from bone coal navajoite calcining dilute sulfuric acid leachate extracts high-purity V2O5Method, it is characterised in that: in (8), ammonium salt is the one in ammonium chloride, ammonium sulfate.
8. one according to claim 1 room temperature direct precipitation method from bone coal navajoite calcining dilute sulfuric acid leachate extracts high-purity V2O5Method, it is characterised in that: in (9), cleaning mixture is the one in industrial process waters, pure water, 1～3% ammonium chloride solution and 1～3% ammonium sulfate.
9. one according to claim 1 room temperature direct precipitation method from bone coal navajoite calcining dilute sulfuric acid leachate extracts high-purity V2O5Method, it is characterised in that: in (10) prepare high purity vanadic anhydride, quality > 99%.
CN201610156580.2A 2016-03-21 2016-03-21 Method of extracting high-purity V2O5 in dilute sulfuric acid leaching solution of stone coal vanadium ore calcine by adopting normal-temperature direct precipitation method Pending CN105803198A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109022829A (en) * 2018-08-10 2018-12-18 南阳汉鼎高新材料有限公司 A kind of device of increasingly automated clean manufacturing high purity vanadium
CN112457037A (en) * 2019-09-09 2021-03-09 天津大学 Performance and application of mullite fiber whisker porous reinforcement reinforced silica aerogel composite material prepared based on liquid phase method
CN115286038A (en) * 2022-08-08 2022-11-04 吉林吉恩镍业股份有限公司 Method for producing ammonium metavanadate by taking phosphorus removal slag as raw material

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109022829A (en) * 2018-08-10 2018-12-18 南阳汉鼎高新材料有限公司 A kind of device of increasingly automated clean manufacturing high purity vanadium
CN109022829B (en) * 2018-08-10 2021-02-19 南阳汉鼎高新材料有限公司 Device for highly automatically and cleanly producing high-purity vanadium
CN112457037A (en) * 2019-09-09 2021-03-09 天津大学 Performance and application of mullite fiber whisker porous reinforcement reinforced silica aerogel composite material prepared based on liquid phase method
CN112457037B (en) * 2019-09-09 2022-02-11 天津大学 Performance and application of mullite fiber whisker porous reinforcement reinforced silica aerogel composite material prepared based on liquid phase method
CN115286038A (en) * 2022-08-08 2022-11-04 吉林吉恩镍业股份有限公司 Method for producing ammonium metavanadate by taking phosphorus removal slag as raw material
CN115286038B (en) * 2022-08-08 2023-10-10 吉林吉恩镍业股份有限公司 Method for producing ammonium metavanadate by taking dephosphorization slag as raw material

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