EP4077751A1 - Récupération de vanadium à partir de matériaux de scories - Google Patents

Récupération de vanadium à partir de matériaux de scories

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Publication number
EP4077751A1
EP4077751A1 EP20901538.7A EP20901538A EP4077751A1 EP 4077751 A1 EP4077751 A1 EP 4077751A1 EP 20901538 A EP20901538 A EP 20901538A EP 4077751 A1 EP4077751 A1 EP 4077751A1
Authority
EP
European Patent Office
Prior art keywords
vanadium
solution
leach
product
feed stream
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
EP20901538.7A
Other languages
German (de)
English (en)
Other versions
EP4077751A4 (fr
Inventor
David Robinson
Mark Daniel Urbani
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Avanti Materials Ltd
Original Assignee
Avanti Materials Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Priority claimed from AU2019904837A external-priority patent/AU2019904837A0/en
Application filed by Avanti Materials Ltd filed Critical Avanti Materials Ltd
Publication of EP4077751A1 publication Critical patent/EP4077751A1/fr
Publication of EP4077751A4 publication Critical patent/EP4077751A4/fr
Pending legal-status Critical Current

Links

Classifications

    • 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
    • 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
    • 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
    • C22B7/04—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
    • 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
    • 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
    • C22B34/10—Obtaining titanium, zirconium or hafnium
    • C22B34/12—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08
    • C22B34/1236—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08 obtaining titanium or titanium compounds from ores or scrap by wet processes, e.g. by leaching
    • C22B34/124—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08 obtaining titanium or titanium compounds from ores or scrap by wet processes, e.g. by leaching using acidic solutions or liquors
    • 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

Definitions

  • the present invention relates to a method for the recovery of vanadium from slag materials.
  • the method of the present invention is adapted to recover vanadium from steel slag through hydrometallurgical processing.
  • Vanadium is most prominently found within magnetite iron ore deposits and is typically present in slags generated during iron recovery processes.
  • the slags are typically processed with the so-called ‘salt roast process’.
  • the salt roast process the vanadium slag is mixed with alkali salts and subjected to a roast to produce sodium metavanadate. These vanadium values are subsequently leached with water. Vanadate values are then precipitated from the leach solution as ammonium metavanadate or ammonium polyvanadate.
  • the high temperature roast step is highly energy intensive and so the vanadium tenor in the slag needs to be at a particular level to make the process economical.
  • a number of different hydrometallurgical process have been employed to process the slags for the recovery of vanadium. Such processes typically comprise an acid leach step in order to extract vanadium into solution.
  • the main issue faced with the recovery of vanadium by hydrometallurgical means is that other metals species such as iron and titanium are typically co-extracted with the vanadium during the acid leach step.
  • the separation of vanadium from a leach solution that also comprises dissolved iron species poses a significant challenge. Most processes by which this can be achieved are uneconomical. Both vanadium and iron can be found in multiple oxidation states and degrees of coordination with varying leach systems and the mixture of species containing these elements alone can be quite complex.
  • a method for the recovery of vanadium from a vanadium containing feed stream comprises: subjecting the vanadium containing feed stream to an acid leach step to form a slurry including a pregnant leach solution that comprises dissolved vanadium and a solid residue; passing the product of the leach step to a solid/liquid separation step to produce a pregnant leach solution that comprises dissolved vanadium; contacting the pregnant leach solution with a reducing agent to reduce one or more species in the pregnant leach solution; passing the pregnant leach solution to a precipitation step in which the solution pH is increased to precipitate a vanadium product; and recovering the vanadium product from the solution.
  • the method further comprises the step of: directing the vanadium product to a purification circuit to product a purified vanadium product.
  • the method of the present invention is preferably adapted to recover vanadium products from slag materials that result from the steel industry. In addition to vanadium, such materials will contain iron, along with other species such as titanium.
  • the method of the present invention allows for a vanadium product to be directly precipitated from the pregnant leach solution without the need to first remove iron species from the pregnant leach solution. This is advantageous where the vanadium recovery is targeted as the separate impurity removal steps are not required prior to the recovery of vanadium.
  • the vanadium containing feed stream comprises a steel slag.
  • steel slag will be understood to refer to the slag byproduct of a steel manufacturing process.
  • impurities or gangue material are separated from the molten metal and are removed as a slag. This slag is subsequently cooled and a solid material is formed.
  • the leach step the leachate used in the acid leach step is sulphuric acid, hydrochloric acid or carbonic acid.
  • the method further comprises the step of: subjecting the feed stream to a pretreatment process. prior to the step of subjecting the feed stream to the leach step.
  • the pre-treatment process comprises a screening step to remove oversize particles.
  • the pre-treatment process comprises one or more size reduction steps. More preferably, the one or more size reduction steps comprise one or more of a crushing step, a grinding step and a milling step.
  • the pre-treatment process comprises one or more beneficiation steps.
  • the one or more beneficiation steps include one or more of a gravity classification step, a magnetic classification step and a floatation step.
  • the feed stream is subjected to a pre-leach step, prior to the leach step.
  • the preleach step comprises the contact of the feed stream with water to produce a preleach slurry. More preferably, the preleach slurry is subjected to a thickening step to increase the solid concentration.
  • the step of: subjecting the feed stream to a leach step to form a slurry including a pregnant leach solution that comprises dissolved vanadium and a solid residue more specifically comprises subjecting the feed stream to a leach step in one or more leach reactors.
  • the step comprises subjecting the feed stream to a leach step in two or more leach reactors. More preferably, the step comprises subjecting the feed stream to a leach step in three or more leach reactors. More preferably, the step comprises subjecting the feed stream to a leach step in four or more leach reactors. More preferably, the step comprises subjecting the feed stream to a leach step in five or more leach reactors.
  • the step of subjecting the feed stream to a leach step is conducted at atmospheric pressure.
  • the step of subjecting the feed stream to a leach step is conducted at elevated temperature.
  • the solid/liquid separation step comprises the treatment of the slurry in a counter current decantation (CCD) circuit.
  • the CCD circuit comprises two or more thickeners arranged in series.
  • the CCD circuit comprises three or more thickeners arranged in series.
  • the CCD circuit comprises four or more thickeners arranged in series.
  • the CCD circuit comprises five or more thickeners arranged in series.
  • the CCD circuit comprises six or more thickeners arranged in series.
  • the CCD circuit comprises seven or more thickeners arranged in series.
  • the solid/liquid separation step comprises the treatment of the slurry in a filtration device.
  • the filtration device is a belt filter.
  • the step of contacting the pregnant leach solution with a reducing agent will reduce substantial proportion of ferric ions present in the pregnant leach solution to ferrous ions.
  • at least 95% of the ferric ions present in solution are reduced to ferrous ions.
  • at least 96% of the ferric ions present in solution are reduced to ferrous ions.
  • at least 97% of the ferric ions present in solution are reduced to ferrous ions.
  • at least 98% of the ferric ions present in solution are reduced to ferrous ions.
  • at least 99% of the ferric ions present in solution are reduced to ferrous ions.
  • the step of contacting the pregnant leach solution with a reducing agent will target a solution Eh of ⁇ 250 mV against a Ag/AgCI reference electrode.
  • the precipitation step comprises contacting the pregnant leach solution with a pH modifier to increase the pH of the solution.
  • the pH modifier is an alkaline substance. More preferably, the pH modifier is selected from one or more of magnesium carbonate, sodium bicarbonate and sodium carbonate.
  • the precipitation step comprises increasing the solution pH to at least 4. In one form of the present invention, the precipitation step comprises increasing the solution pH to at least 4.1. In one form of the present invention, the precipitation step comprises increasing the solution pH to at least 4.2. In one form of the present invention, the precipitation step comprises increasing the solution pH to at least 4.3. In one form of the present invention, the precipitation step comprises increasing the solution pH to at least 4.4. In one form of the present invention, the precipitation step comprises increasing the solution pH to at least 4.5.
  • the precipitation step comprises increasing the solution pH to between 4 and 5. In one form of the present invention, the precipitation step comprises increasing the solution pH to between 4.1 and 5. In one form of the present invention, the precipitation step comprises increasing the solution pH to between 4.2 and 5. In one form of the present invention, the precipitation step comprises increasing the solution pH to between 4.3 and 5. In one form of the present invention, the precipitation step comprises increasing the solution pH to between 4.4 and 5. In one form of the present invention, the precipitation step comprises increasing the solution pH to between 4.5 and 5.
  • the precipitation step is conducted prior to the recovery of iron values from the pregnant leach solution.
  • the precipitation step is conducted prior to the recovery of titanium values from the pregnant leach solution.
  • the step of recovering the vanadium product comprises passing the slurry formed in the precipitation step to solid liquid separation step to produce a solid vanadium product and a barren solution.
  • the solid vanadium product is washed prior to further processing.
  • the purification circuit more specifically comprises a salt roast step, a leach step and an ammonium metavanadate precipitation step.
  • the purification circuit further comprises a V2O5 production step.
  • the purification circuit more specifically comprises an acid leach step and a vanadium solvent extraction step.
  • the vanadium solvent extraction step will recover vanadium as a vanadyl sulphate solution.
  • the purification circuit more specifically comprises an ammoniacal leach step, a vanadyl product precipitation step and calcination step.
  • Figure 1 is a flowsheet of the process to recover a vanadium product
  • Figure 2 is flowsheet of various purification routes that may be utilised to purify the vanadium product produced in Figure 1 .
  • the method of the present invention relates to the recovery of vanadium from a vanadium containing feed stream.
  • the method comprises the steps of: subjecting the vanadium containing feed stream to a leach step step to form a slurry including a pregnant leach solution that comprises dissolved vanadium and a solid residue; passing the product of the leach step to a solid/liquid separation step to produce a pregnant leach solution that comprises dissolved vanadium; contacting the pregnant leach solution with a reducing agent to reduce one or more species in the pregnant leach solution; passing the pregnant leach solution to a precipitation step in which the solution pH is increased to precipitate a vanadium product; and recovering the vanadium product from the solution.
  • the recovered vanadium product comprises a fairly high V2O5 component amongst other precipitated solids. In one embodiment, the recovered vanadium product comprises at least 10% vanadium.
  • the method the present invention is suitable to recover vanadium from steel slags.
  • steel slags comprise a large proportion of iron species. These iron species, along with other metal impurities, will be co-extracted into the leach solution during the leach step. These impurities will need to be considered in the recovery process.
  • the process of the present invention provides a method by which a vanadium product can be selectively precipitated over iron species present in the pregnant leach solution, thereby permitting the recovery of vanadium directly from the pregnant leach solution without the need to first remove/recover iron.
  • FIG. 1 there is shown a method for the recovery of vanadium 10 in accordance with an embodiment of the present invention.
  • a feed stream 12 is subjected to a pre-treatment process 14 to render the feed stream suitable for further processing.
  • the feed stream 12 is first directed to a primary crusher 16 to break up large pieces of the feed stream 12 for further processing.
  • the resulting material from the primary crusher is directed to a primary grinder 18 to reduce the particle size of the feed stream 12.
  • the material resulting material is directed to screen 20 and any oversize material 22 is directed to a tertiary crusher 24 before being redirected to the primary grinder 18.
  • the screen has a mesh size of between 75 pm and 500 pm.
  • the ground material 26 is directed to secondary grinding stage 28 to further reduce the particle size.
  • the resulting material is directed to a cyclonic separator 30 and any oversize particles 32 are recycled back to the secondary grinding stage 28.
  • the cyclonic separator 30 could be replaced with other particle size separation devices, such as for example a screen.
  • the secondary grinding stage will reduce the particle size of the feed stream to the below 150 pm. In one embodiment, the secondary grinding stage will reduce the particle size of the feed stream to the below 140 pm. In one embodiment, the secondary grinding stage will reduce the particle size of the feed stream to the below 130 pm. In one embodiment, the secondary grinding stage will reduce the particle size of the feed stream to the below 120 pm. In one embodiment, the secondary grinding stage will reduce the particle size of the feed stream to the below 110 pm. In one embodiment, the secondary grinding stage will reduce the particle size of the feed stream to the below 100 pm. In one embodiment, the secondary grinding stage will reduce the particle size of the feed stream to the below 90 pm. In one embodiment, the secondary grinding stage will reduce the particle size of the feed stream to the below 80 pm.
  • the processed feed stream is directed to a pre-leach step (not shown) where it is contacted with water to produce a pre-leach slurry 34.
  • the slurry 34 is then directed to a thickening step 36 to remove excess water and produce a concentrated leach feed stream 38.
  • the inventors have found that the pre-leach step will help remove excess lime and other water soluble materials from the feed stream and consequently reduce leachate consumption in the later leach step.
  • the solids content of the leach feed stream is controlled to a target solids content.
  • the target solids content is dependent on the grade of the feed material and is manipulated such that sufficient water is present in the discharge from the leach to maintain all soluble salts in solution.
  • the target solids content in the leach feed stream is between 5% and 40% by weight. More preferably, the target solids content in the leach feed stream is between 20% and 30% by weight.
  • the inventors have found that the preferred target solids content in the leach feed stream is depended on the grade of the feedstock. Generally speaking, the higher the feedstock grade, the lower the target solids content.
  • the concentrated leach feed stream is directed to a leach circuit 40 where it is contacted with a leachate to leach vanadium and other metals into solution.
  • the leach step is an acid leach step and the leachate is sulfuric acid 42.
  • the leach circuit 40 comprises a number of leach reactors arranged in series. Sulfuric acid 42 is added to the leach reactors in sufficient excess to maintain a free acid concentration.
  • the concentration of the sulphuric acid is in the range of the range of 10% to 60% (w/w). In one embodiment, the concentration of the sulphuric acid is in the range of the range of 20% to 50% (w/w).
  • the leach can be exothermic and is typically operated at elevated temperature of 45-105°C with or without the addition of heat.
  • the leach step will produce a leach slurry 44 that comprises a pregnant leach solution containing dissolved vanadium and other soluble metals, together with a residue of undissolved material.
  • the leach step 40 will also result in the precipitation of calcium sulfate with varying degrees of hydration and this will form part of the slurry 44.
  • the amount of calcium in the feed stream 12 will determine the amount of calcium sulfate that is produced.
  • the leach slurry 44 is directed to a solid liquid separation step to separate any solids from the pregnant leach solution.
  • the slurry 44 is directed to a counter current decantation (CCD) circuit 46.
  • CCD counter current decantation
  • the slurry 44 is washed in a series of thickeners until the majority of the dissolved metals are removed.
  • the slurry 44 is directed into the first thickener and the wash solution is directed to the final thickener.
  • the underflow and overflow flow counter current to one another.
  • a flocculent 48 may be added to one or more of the thickeners to aid in the separation process.
  • the overflow 49 from the first thickener is directed to further processing to recover metals.
  • the underflow 50 of the final thickener contains a high calcium sulfate content which can be recovered for sale.
  • the inventors have found that the use of the CCD circuit 46 is advantageous as it involves multiple solid washing stages. This will ensure that a significant amount of the soluble metals will be separated from the solids that are produced during the leach step. As discussed above, calcium sulfate will be produced during the leach reaction. The use of the CCD circuit 46 will substantially clean this solid, allowing for the possibility of subsequent use.
  • the slurry may be directed to a filtration step, using a belt filter or other filtration devices.
  • the filtration step would preferably also include a wash step.
  • the pregnant leach solution 49 is directed to a reduction step 52 where it is contact with a reducing agent 54.
  • the step of contacting the pregnant leach solution 49 with a reducing agent 54 will reduce substantial proportion of ferric ions present in the pregnant leach solution to ferrous ions.
  • any reducing agent which will act to reduce a substantial portion of the ferric ions present in the pregnant leach solution to ferrous will be suitable for use.
  • the reducing agent is a metal powder.
  • the metal power is iron.
  • the reducing agent is selected from sodium sulfite, sodium metabisulphite and sulphur dioxide.
  • sufficient reducing agent is added to reduce the solution Eh of ⁇ 250 mV against a Ag/AgCI reference electrode.
  • the pregnant leach solution is directed to a precipitation step 56, where the pH of the solution is increased to precipitate a vanadium product.
  • the reduction step 52 reduces the ferric species to ferrous ion, the increase in pH will precipitate vanadium products with a high degree of selectivity over iron and other impurity metal ions in the solution.
  • the pH of the solution is increased by the addition of a pH modifier 58.
  • the pH modifier 58 is an alkaline substance.
  • the pH modifier 58 is selected from one or more of sodium bicarbonate and sodium carbonate.
  • the pH is increased to above 3. In one embodiment of the present invention, the pH is increased to above 3.5. In one embodiment of the present invention, the pH is increased to above 4.
  • the pH is increased to between 3 and 4.5. In one embodiment of the present invention, the pH is increased to between 3.5 and 4.5. In one embodiment of the present invention, the pH is increased to between 4 and 4.5.
  • the resulting slurry 60 is directed to a solid liquid separation step 62 to recover the precipitated vanadium products 64.
  • the solid liquid separation 62 step comprises a filtration step to recover the vanadium product 64.
  • the recovered vanadium product 64 is washed to remove and entrained iron other impurities.
  • the filtrate 66 from the solid liquid separation step 62 is a ferrous sulfate solution comprising dissolved impurity metals.
  • the filtrate 66 is directed to a neutralisation circuit 68 where it is contacted with a neutralising agent, such as lime 70, to increase the solution pH and precipitate an iron rich calcium sulfate residue and an aqueous effluent.
  • a neutralising agent such as lime 70
  • the residue 72 is recovered in solid liquid separations step 74 and directed to disposal.
  • the vanadium product 64 contains mixture of vanadium oxides and hydroxides with varying degrees of hydration. In one embodiment, the vanadium product 64 contains approximately 10% to 40% V2O5 equivalent.
  • the vanadium product 64 may be dried and sold as a final product. Alternatively, the vanadium product 64 can be directed to a purification circuit to increase the vanadium purity.
  • the purification circuit is more specifically comprises a salt roast step 78, a leach step 80 and a precipitation step 82.
  • the salt roast step 78 the vanadium product 64 is roasted at elevated temperature in the presence of a salt 84.
  • the salt is an alkaline or alkaline earth salt, preferably sodium carbonate.
  • the amount of salt in the roast step is dependent on the vanadium content.
  • at least 5% w/w salt is added to the vanadium product 64.
  • the vanadium product 64 comprises approximately 18% vanadium
  • approximately 7-8% w/w salt is added to the vanadium product 64.
  • the roast step 78 is conducted at a temperature of at least 1 ,000 °C.
  • the residence time of the roast step 78 is at least 1 hour.
  • the roasted product is directed to the leach step 80 to dissolve vanadium species.
  • the leach step comprises to contact of the roasted product with water.
  • the leach step is conducted at a temperature of at least 70°C.
  • the leach step is conducted for a residence time of at least 1 hour.
  • the vanadium-containing aqueous solution can be treated by known processes to recover vanadium.
  • aluminium sulfate is first added to the warm vanadium solution to facilitate silica (and alumina) removal.
  • the purified vanadium solution is treated with ammonium sulfate in precipitation step 82 to precipitate ammonium metavanadate 86.
  • the ammonium metavanadate may then be separated and subjected to a calcination step to produce solid V2O5.
  • the purification circuit comprises an acid leach step 90 to leach vanadium into solution.
  • the pregnant leach solution is directed to a solvent extraction step 92 to recover vanadium.
  • a solvent extraction step 92 For most efficient separation of vanadium from iron the higher oxidation states of vanadium and iron are preferred in solution.
  • Optimisation of acid strength and oxidant addition is required to economically effect this oxidation and phosphine oxides (e.g. Cyanex 923) or amine reagents (e.g. Alamine 336) can be used to selectively extract vanadium.
  • the vanadium solvent extraction step will recover vanadium as a vanadyl sulphate solution 94.
  • the purification circuit comprises an ammoniacal leach step 98 where it is contacted with an alkaline leachant to leach vanadium into solution.
  • the alkaline leachant is selected from NaHCC>3 or NFUOH.
  • the pregnant leach solution is directed to a precipitation step 100 where is contacted with an ammonium species to precipitate NH4VO3.
  • the resulting precipitate can be recovered and directed to a calcination step 102 to produce a V2O5 product 104.
  • a steel slag sample was sourced from a steel production plant.
  • a chemical assay of the material was conducted and the material was shown to contain 2.46% V, 17.9% Fe and 0.72% Ti.
  • the material was subjected to a sulphuric acid leach step using 50% sulfuric acid and 22% solids (1800 kg/t acid addition).
  • the leach was conducted at a temperature of 100 °C.
  • the leach curve is provided in Figure 3.
  • the leach kinetics were rapid and extractions high (>99% V).
  • the resulting leach solution was separated from the solids and a chemical analysis was performed on each.
  • the leach liquor contained 10.4 g/L V, 78 g/L Fe and 2.8 g/L Ti.
  • the final residue contained 25.8% Ca, 4.0% Si, 100 ppm V, 1000 ppm Fe and 200 ppm Ti.
  • Example 2 A sample of composite steel slag (400g) was added to 400gpl sodium carbonate (made up in Perth scheme water) at a pulp density of 15% solids by weight and agitated in a glass reactor. Hydrogen peroxide was added periodically to maintain an Eh close to zero. The test was maintained at 90°C for twelve hours. No kinetic samples were taken. The test was terminated after twelve hours and the pulp filtered, assayed and stored. The results are shown in Table 1 :
  • a steel slag sample was subjected to a sulphuric acid leach and the filtrate was separated. Iron powder was added to the leach liquor. An Eh ⁇ 250mV Ag/AgCI was targeted. The solution pH was increased to 4 with the addition lime to precipitate a vanadium product. Essentially complete vanadium precipitation was achieved (99.6%) to a high-grade precipitate (18.3% V).
  • Example 3 The vanadium product from Example 3 was subjected to a salt roast process to determine the effectiveness of this method to purify the vanadium product.
  • the head sample was 16% V (details below) and in a first pass at SRL 10% w/w Na2C03 was used as the salt addition and the test performed as follows:
  • a vanadium product was subjected to an alkaline leach process to determine the effectiveness of this method to purify the vanadium product.
  • This V PLS can be processed through ammonium metavanadate precipitation and V2O5 production using standard methods.

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  • Engineering & Computer Science (AREA)
  • Metallurgy (AREA)
  • Mechanical Engineering (AREA)
  • Organic Chemistry (AREA)
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  • Environmental & Geological Engineering (AREA)
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  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Manufacture And Refinement Of Metals (AREA)

Abstract

L'invention concerne également un procédé de récupération de vanadium à partir d'un flux d'alimentation contenant du vanadium, le procédé comprenant les étapes consistant : à soumettre le flux d'alimentation contenant du vanadium à une étape de lixiviation acide pour former une bouillie comprenant une solution de lixiviation enrichie qui comprend du vanadium dissous et un résidu solide ; à faire passer le produit de l'étape de lixiviation à une étape de séparation solide/liquide pour produire une solution de lixiviation enrichie qui comprend du vanadium dissous ; à mettre en contact la solution de lixiviation enrichie avec un agent réducteur pour réduire une ou plusieurs espèces dans la solution de lixiviation enrichie ; à faire passer la solution de lixiviation enrichie à une étape de précipitation dans laquelle le pH de la solution est augmenté pour précipiter un produit de vanadium ; et à récupérer le produit de vanadium à partir de la solution.
EP20901538.7A 2019-12-19 2020-12-08 Récupération de vanadium à partir de matériaux de scories Pending EP4077751A4 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
AU2019904837A AU2019904837A0 (en) 2019-12-19 Recovery of Vanadium from Slag Materials
PCT/AU2020/051337 WO2021119728A1 (fr) 2019-12-19 2020-12-08 Récupération de vanadium à partir de matériaux de scories

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