CN110306043B - Method for leaching vanadium in magnetic vanadium iron spinel type powder vanadium concentrate through normal-temperature electrooxidation - Google Patents

Method for leaching vanadium in magnetic vanadium iron spinel type powder vanadium concentrate through normal-temperature electrooxidation Download PDF

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CN110306043B
CN110306043B CN201910584546.9A CN201910584546A CN110306043B CN 110306043 B CN110306043 B CN 110306043B CN 201910584546 A CN201910584546 A CN 201910584546A CN 110306043 B CN110306043 B CN 110306043B
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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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    • 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
    • C22B3/045—Leaching using electrochemical 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
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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Abstract

A method for leaching vanadium in magnetic vanadium iron spinel type powder vanadium concentrate by electrooxidation at normal temperature. Taking vanadium-iron spinel type vanadium-containing concentrate as an initial raw material; sleeving the rod-shaped magnet by using an insulating sleeve, and adsorbing an iron sheet on the outer side of the bottom of the insulating sleeve to introduce current; evenly mixing vanadium concentrate and iron powder according to a certain proportion, and adsorbing the mixture on a conductive iron sheet; and immersing the adsorbed powder into an electrolyte solution for electrooxidation, and leaching vanadium in the electrolyte solution to obtain vanadium-containing leaching solution. The method adsorbs the powder together by the magnet, and omits the step of preparing a block electrode. The in-situ direct electro-oxidation leaching of the ferrovanadium spinel powder is realized by utilizing the conductivity of the ferrovanadium spinel and introducing current through the contact of an iron sheet and the powder. The reactant particles are directly connected with the electrodes, so that the conductive electrode is good in conductivity and easy to oxidize, and no oxidant is added or oxidizing gas is introduced; the electrolytic reaction rate is accelerated, and briquetting, roasting and forming are not needed, so that the energy consumption and the production cost are reduced.

Description

Method for leaching vanadium in magnetic vanadium iron spinel type powder vanadium concentrate through normal-temperature electrooxidation
Technical Field
The invention belongs to the field of vanadium leaching from vanadium-iron spinel type powder minerals by an electrooxidation method. In particular to a method for directly electro-oxidatively leaching vanadium in an electrolyte solution by adsorbing vanadium concentrate powder on an iron sheet with conductivity through a magnet without preparing a block electrode by utilizing the magnetism and the conductivity of vanadium-iron spinel type vanadium-containing concentrate.
Background
Vanadium is an indispensable metal element in modern industry, has a plurality of excellent physical properties and chemical properties, is widely applied to industries such as machinery, aviation, electronic technology, national defense industry and the like, and is called metal vitamin. The vanadium resources in China are rich, and the main vanadium-containing minerals are vanadium titano-magnetite and vanadium-containing stone coal. Vanadium in vanadium titano-magnetite or vanadium-containing stone coal can be converted into vanadium iron spinel with conductivity and magnetism by a metallurgical method. At present, in order to separate metal elements from minerals in a green and efficient manner, an ore pulp electrolysis process is favored by metallurgy workers due to the characteristics of short flow, low energy consumption, high metal separation efficiency, good ecological environment and the like. Therefore, there are many workers applying the ore pulp electrolysis method to the vanadium extraction field, for example, chinese patents CN104017988A, CN102534229A, CN102134640A, CN103060843, and CN103421950A all extract vanadium from vanadium-containing minerals by the ore pulp electrolysis method, and finally obtain vanadium-containing leachate.
When the vanadium-containing mineral is treated by traditional ore pulp electrolysis, on one hand, vanadium in the mineral can be leached by electrooxidation when mineral particles collide with the surface of an electrode, but the reaction has a much smaller occurrence probability. Therefore, in order to enhance leaching, an additive is added into the electrolyte solution, and the additive generates an oxidant with strong oxidizing property at the anode, so that the oxidative leaching of the vanadium-containing mineral is realized, and the vanadium-containing leaching solution is obtained. In essence, this is an indirect oxidation process, which results in increased production costs and difficulties in the purification of the subsequent leachate; chinese patent CN104017988A mentions that when chloride is used as an additive, chlorine is generated at the anode as an oxidant, but chlorine is a harmful gas and pollutes the environment. Therefore, the vanadium iron spinel used as a soluble anode is directly subjected to electro-oxidation in an electrolyte solution by utilizing the conductivity of the vanadium iron spinel so as to obtain a vanadium-containing leaching solution, wherein the defects caused by the indirect oxidation process of the ore pulp electrolysis process are overcome. For example, a method for anodically electrolyzing and leaching vanadium in strong base electrolyte solution (application number: 201910440720.2) and a method for anodically electrolyzing and leaching vanadium in normal temperature saturated oxalic acid solution (application number: 201910454934.5) mention that vanadium iron spinel vanadium-containing concentrate powder is made into a block electrode, vanadium concentrate can be directly electrolyzed at normal temperature and normal pressure without introducing any additive and oxidizing gas, and vanadium-containing leachate is obtained. However, the two methods require briquetting the powder for anode production, namely mixing vanadium iron spinel type vanadium concentrate powder and polyvinyl alcohol according to a certain proportion, briquetting, and roasting at a roasting temperature of more than or equal to 800 ℃ in a reducing atmosphere for forming. Therefore, the preparation process of the anode depends on high-temperature reduction conditions, and the aim of extracting vanadium at low cost is not achieved essentially.
In order to avoid the technical and economic problems brought by the preparation of the block electrode, the invention provides a method for preparing vanadium-containing leaching solution by utilizing the magnetic characteristic of vanadium-iron spinel, aggregating vanadium-containing concentrate powder of vanadium-iron spinel under the action of a magnetic field to prepare a powder electrode and directly carrying out electrooxidation reaction.
Disclosure of Invention
In view of the defects of the prior art, one of the purposes of the invention is to provide a method for leaching vanadium in magnetic ferrovanadium spinel type powder vanadium concentrate through normal-temperature electrooxidation, namely, ferrovanadium spinel type vanadium concentrate powder with magnetism and conductivity is used as an initial raw material; sleeving the rod-shaped magnet by using an insulating sleeve, and adsorbing an iron sheet on the outer side of the bottom of the insulating sleeve to introduce current; mixing vanadium concentrate and iron powder in certain proportion, adsorbing onto conductive iron sheet, soaking the adsorbed powder in electrolyte solution for electric oxidation to obtain vanadium-containing leaching solution.
Compared with the existing vanadium extraction process, the method utilizes the magnetism of vanadium iron spinel, and the powder is adsorbed together by the magnet, so that the step of preparing a block electrode is omitted. The method utilizes the conductivity of the vanadium iron spinel, and introduces current through the contact of an iron sheet and powder, thereby realizing the electro-oxidation leaching of the vanadium iron spinel. Compared with the traditional ore pulp electrolysis process, the method has the advantages that the reactant particles are directly connected with the electrodes, the conductivity is good, the in-situ electro-oxidation leaching is easy to realize, and no oxidizing additive is added or oxidizing gas is introduced; in addition, compared with the method for directly electrolytically leaching vanadium by using a block anode, the method increases the reaction interface, so that the electrolytic reaction rate is accelerated, briquetting roasting forming is not needed, the energy consumption and the production cost are reduced, and residues losing magnetism in electrolysis can be separated from the surface of vanadium concentrate and sink to the bottom of an electrolytic tank, so that the continuous oxidation leaching of unreacted vanadium concentrate is not hindered.
A method for leaching vanadium in magnetic vanadium iron spinel type powder vanadium concentrate through normal-temperature electrooxidation is characterized by comprising the following steps:
(1) taking vanadium-iron spinel type vanadium-containing concentrate as an initial raw material;
(2) sleeving the rod-shaped magnet by using an insulating sleeve, and adsorbing iron sheets on the outer side of the bottom of the rod-shaped magnet to lead out a lead; evenly mixing vanadium concentrate and iron powder according to a certain proportion, and adsorbing the mixture at the bottom of an iron sheet;
(3) soaking the adsorbed powder into an electrolyte solution, and carrying out electrooxidation leaching at normal temperature and normal pressure to leach vanadium;
(4) and after the electrolytic reaction is finished, cleaning the anode and the cathode by using deionized water for 3-5 times, and then carrying out solid-liquid separation to obtain the vanadium-containing leaching solution.
Further, the vanadium-iron spinel type vanadium-containing concentrate is subjected to ball milling in the step (1) until the particle size is below 0.074 mm.
Further, in the step (1), the mass ratio of the vanadium concentrate subjected to ball milling to the iron powder is 1: 1.
Further, in the step (2), the magnet is sleeved by an insulating sleeve, and a lead is led out from the bottom of the insulating sleeve through an iron sheet; the magnet is one of a permanent magnet and a non-permanent magnet, and is in the shape of a rod.
Further, the insulating sleeve used in step (2) is made of one of glass, plastic, and rubber, and is preferably in the form of a barrel, and more preferably, the insulating sleeve is a glass sleeve.
Further, in the step (2), vanadium concentrate and iron powder are uniformly mixed according to the mass ratio of 1:1 and then are adsorbed at the bottom of an iron sheet, and a conductive powder electrode is formed by utilizing the magnetism and the conductivity of the vanadium-iron spinel type vanadium-containing concentrate, so that the specific surface area is large, and the electrooxidation efficiency is high.
Further, the electrooxidation reaction in the step (3) is carried out in an electrolytic cell, and the electrolytic cell is preferably at normal temperature and normal pressure; the cathode material of the electrolytic cell is a metal material or a carbon material, and the electrode shape is preferably rod-shaped; the electrolyte is alkaline electrolyte or acidic electrolyte.
Further, the electrolytic reaction in the step (3) is carried out under mechanical stirring; the voltage of the electrolytic cell is 5-15V; the electrolysis time is more than 1h, preferably 1-3 h.
Further, during the electrolysis in step (3), the powder end portion is immersed in the electrolyte solution to ensure that anodic electrooxidation reaction occurs on the ferrovanadium spinel as much as possible.
Further, the method for leaching vanadium in the magnetic ferrovanadium spinel powder vanadium concentrate through normal-temperature electrooxidation is characterized in that in the step (4), after the electrolytic reaction is finished, the anode and the cathode are washed for 3-5 times by deionized water, and then solid-liquid separation is carried out to obtain a vanadium-containing leaching solution.
Compared with the prior art, the technical scheme adopted by the invention has the following advantages:
1. the invention provides a method for normal-temperature electro-oxidation leaching of vanadium in magnetic vanadium iron spinel type powder vanadium concentrate, which utilizes the magnetism of vanadium iron spinel, adsorbs the powder together through a magnet, omits the step of preparing a block electrode, and utilizes the conductivity of the vanadium iron spinel, and introduces current through the contact of an iron sheet and the powder, thereby realizing the in-situ electro-oxidation leaching of the vanadium iron spinel.
2. The method can be carried out at normal temperature and normal pressure, thereby reducing energy consumption and pollution; in addition, the equipment is simple, the operation is convenient, the investment cost is low, and the method is suitable for industrial popularization.
3. Compared with the traditional ore pulp electrolysis process, the method has the advantages that the reactant particles are directly connected with the electrodes, the conductivity is good, the oxidation is easy, and the addition of an oxidant and the introduction of oxidizing gas are not needed; in addition, the residue after the magnetic electrolysis leaching is removed from the surface of the vanadium concentrate under the action of stirring and is deposited at the bottom of the electrolytic cell, so that the continuous oxidation leaching of the unreacted vanadium concentrate is not hindered.
4. Compared with the method for directly electrolytically leaching vanadium by using the block anode, the method increases the reaction interface, thereby accelerating the electrolytic reaction rate, avoiding briquetting, roasting and forming, and reducing the energy consumption and the production cost.
Drawings
FIG. 1 is a diagram of a normal temperature direct electro-oxidation apparatus for magnetic powder.
FIG. 2 shows the electrolysis of pure vanadium ferrite with a current varying dramatically with time at different cell voltages, and the vanadium leaching rate can be increased by increasing the cell voltage.
FIG. 3 shows that when the bath voltage is 10V, the saturated oxalic acid solution is used as the electrolyte, and the magnetic vanadium concentrate powder and the iron powder are uniformly mixed in a ratio of 1:1, and then are electrolyzed, and the current and the time relation are that the current gradually decreases along with the progress of the electrolysis process.
FIG. 4 shows the relationship between the current and time of electrolysis of pure vanadic spinel with a cell voltage of 10V in 35% NaOH solution as electrolyte, the current gradually decreases as the anode dissolves.
FIG. 5 shows that the cell voltage is 10V, 35% NaOH solution is used as electrolyte, magnetic vanadium concentrate powder and iron powder are uniformly mixed in a ratio of 1:1, and then electrolysis is carried out, and the current is reduced gradually along with the progress of the electrolysis process.
Detailed Description
In order to verify the feasibility of the present invention, the following examples are further provided to illustrate the present invention, but the present invention is not limited to the following examples. All such modifications made in accordance with the spirit of the present invention are intended to be included within the scope of the present invention.
Example 1:
vanadium trioxide and ferric oxide are used as initial raw materials, and roasting is carried out for 48 hours at 1200 ℃ in a reducing atmosphere to obtain pure Fe2VO4. Weighing 0.5g of pure vanadium iron spinel, grinding to a particle size of below 0.074mm, and adsorbing the pure vanadium iron spinel on an iron sheet at the bottom of a glass sleeve provided with a magnet, wherein the diameter of the iron sheet is 12mm, and the thickness of the iron sheet is 3 mm. The electrolytic reaction is carried out in an electrolytic cell at normal temperature and normal pressure, the cathode of the electrolytic cell is made of a graphite rod with the diameter of 6mm, the center distance between the anode and the cathode is 7cm, and the electrolyte solution is saturated oxalic acid solution. The bath voltage is 5V, the mechanical stirring speed is 500r/min, the electrolysis temperature is room temperature, and the electrolysis reaction time is 3600 s. And after the electrolytic reaction is finished, carrying out solid-liquid separation, and finally measuring the concentration of vanadium in the leaching solution to be 265.2mg/L by ICP-AES.
Example 2:
vanadium trioxide and ferric oxide are used as initial raw materials, and roasting is carried out for 48 hours at 1200 ℃ in a reducing atmosphere to obtain pure Fe2VO4. Weighing 0.5g of pure vanadium iron spinel, grinding to a particle size of below 0.074mm, and adsorbing the pure vanadium iron spinel on an iron sheet at the bottom of a glass sleeve provided with a magnet, wherein the diameter of the iron sheet is 12mm, and the thickness of the iron sheet is 3 mm. The electrolytic reaction is carried out in an electrolytic cell at normal temperature and normal pressure, the cathode of the electrolytic cell is made of a graphite rod with the diameter of 6mm, the center distance between the anode and the cathode is 7cm, and the electrolyte solution is saturated oxalic acid solution. The bath voltage is 10V, the mechanical stirring speed is 500r/min, the electrolysis temperature is room temperature, and the electrolysis reaction time is 3600 s. And after the electrolytic reaction is finished, carrying out solid-liquid separation, and finally measuring the concentration of vanadium in the leaching solution to be 604.5mg/L by ICP-AES.
Example 3:
vanadium iron spinel type vanadium concentrate is used as an initial raw material, and the particle size of the vanadium concentrate is ball-milled to be less than 0.074 mm. 0.5g of the vanadium concentrate subjected to ball milling and 0.5g of iron powder are weighed and placed in an agate mortar to be fully and uniformly mixed. And adsorbing the mixed powder on an iron sheet at the bottom of a glass sleeve with a magnet, wherein the diameter of the iron sheet is 12mm, and the thickness of the iron sheet is 3 mm. The electrolytic reaction is carried out in an electrolytic cell at normal temperature and normal pressure, the cathode of the electrolytic cell is made of a graphite rod with the diameter of 6mm, the center distance between the anode and the cathode is 7cm, and the electrolyte solution is saturated oxalic acid solution. The cell voltage was 10V, the mechanical stirring speed was 500r/min, the electrolysis temperature was room temperature, and the electrolysis reaction was 4600 s. And after the electrolytic reaction is finished, carrying out solid-liquid separation, and finally measuring the concentration of vanadium in the leaching solution to be 344.3mg/L by ICP-AES.
Example 4:
vanadium trioxide and ferric oxide are used as initial raw materials, and roasting is carried out for 48 hours at 1200 ℃ in a reducing atmosphere to obtain pure Fe2VO4. Weighing 0.5g of pure vanadium iron spinel, grinding to a particle size of below 0.074mm, and adsorbing the pure vanadium iron spinel on an iron sheet at the bottom of a glass sleeve provided with a magnet, wherein the diameter of the iron sheet is 12mm, and the thickness of the iron sheet is 3 mm. The electrolytic reaction is carried out in an electrolytic cell at normal temperature and normal pressure, the cathode of the electrolytic cell is made of a graphite rod with the diameter of 6mm, the center distance between the anode and the cathode is 7cm, and the electrolyte solution is NaOH solution with the mass fraction of 35%. The bath voltage is 10V, the mechanical stirring speed is 500r/min, the electrolysis temperature is room temperature, and the electrolysis reaction time is 3600 s. And after the electrolytic reaction is finished, carrying out solid-liquid separation, and finally measuring the concentration of vanadium in the leaching solution to be 442mg/L by ICP-AES.
Example 5:
vanadium iron spinel type vanadium concentrate is used as an initial raw material, and the particle size of the vanadium concentrate is ball-milled to be less than 0.074 mm. 0.5g of the vanadium concentrate subjected to ball milling and 0.5g of iron powder are weighed and placed in an agate mortar to be fully and uniformly mixed. And adsorbing the mixed powder on an iron sheet at the bottom of a glass sleeve with a magnet, wherein the diameter of the iron sheet is 12mm, and the thickness of the iron sheet is 3 mm. The electrolytic reaction is carried out in an electrolytic cell at normal temperature and normal pressure, the cathode of the electrolytic cell is made of a graphite rod with the diameter of 6mm, the center distance between the anode and the cathode is 7cm, and the electrolyte solution is NaOH solution with the mass fraction of 35%. The bath voltage is 10V, the mechanical stirring speed is 500r/min, the electrolysis temperature is room temperature, and the electrolysis reaction is 10800 s. And after the electrolytic reaction is finished, carrying out solid-liquid separation, and finally measuring the concentration of vanadium in the leaching solution to be 214.2mg/L by ICP-AES.

Claims (7)

1. A method for leaching vanadium in magnetic vanadium iron spinel type powder vanadium concentrate through normal-temperature electrooxidation is characterized by comprising the following steps:
(1) taking vanadium-iron spinel type vanadium-containing concentrate as an initial raw material;
(2) sleeving the rod-shaped magnet by using an insulating sleeve, and adsorbing iron sheets on the outer side of the bottom of the rod-shaped magnet to lead out a lead; evenly mixing vanadium concentrate and iron powder according to a certain proportion, and adsorbing the mixture at the bottom of an iron sheet;
(3) soaking the adsorbed powder into an electrolyte solution, and carrying out electrooxidation leaching at normal temperature and normal pressure to leach vanadium;
(4) after the electrolytic reaction is finished, cleaning the anode and the cathode with deionized water for 3-5 times, and then carrying out solid-liquid separation to obtain vanadium-containing leachate;
ball milling vanadium-containing spinel concentrate until the particle size is below 0.074 mm;
in the step (2), the mass ratio of the vanadium concentrate subjected to ball milling to the iron powder is 1: 1.
2. The normal-temperature electro-oxidation leaching method of vanadium in magnetic vanadium iron spinel type powder vanadium concentrate as claimed in claim 1, wherein in the step (2), the magnet is sleeved with an insulating sleeve, and a lead is led out from the bottom of the insulating sleeve through an iron sheet; the magnet is one of a permanent magnet and a non-permanent magnet, and is in the shape of a rod.
3. The method for electro-oxidative leaching of vanadium from magnetic vanadium iron spinel type powder vanadium concentrate at normal temperature according to claim 1, wherein the insulating sleeve used in the step (2) is made of one of glass, plastic and rubber, and is in the shape of a barrel.
4. The method for leaching vanadium from magnetic vanadium iron spinel type powder vanadium concentrate through normal-temperature electrooxidation as claimed in claim 1, wherein in the step (2), vanadium concentrate and iron powder are uniformly mixed according to a mass ratio of 1:1 and then are adsorbed at the bottom of an iron sheet, and a conductive powder electrode is formed by utilizing the magnetism and the conductivity of the vanadium iron spinel type vanadium-containing concentrate, so that the specific surface area is large, and the electrooxidation efficiency is high.
5. The method for leaching vanadium from the magnetic vanadium iron spinel type powder vanadium concentrate through normal-temperature electro-oxidation as claimed in claim 1, wherein the electro-oxidation reaction in the step (3) is carried out in an electrolytic bath, and the electrolytic bath is a normal-temperature normal-pressure electrolytic bath; the cathode material of the electrolytic cell is a metal material or a carbon material, and the electrode is rod-shaped; the electrolyte is alkaline electrolyte or acidic electrolyte.
6. The normal-temperature electro-oxidation leaching method for vanadium in magnetic vanadium iron spinel type powder vanadium concentrate as claimed in claim 1, wherein the electrolysis reaction in the step (3) is carried out under mechanical stirring; the voltage of the electrolytic cell is 5-15V, and the time of electrolysis is 1-3 h.
7. The method for electro-oxidative leaching of vanadium from a magnetic ferrovanadium spinel-type powdered vanadium concentrate at ambient temperature as claimed in claim 1, wherein during the electrolysis in step (3), the end of the powder is partially immersed in the electrolyte solution to ensure that anodic electro-oxidation reaction occurs on the ferrovanadium spinel as much as possible.
CN201910584546.9A 2019-07-01 2019-07-01 Method for leaching vanadium in magnetic vanadium iron spinel type powder vanadium concentrate through normal-temperature electrooxidation Active CN110306043B (en)

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