CN111484076A - Method for recovering high-purity vanadium from failure vanadium electrolyte - Google Patents
Method for recovering high-purity vanadium from failure vanadium electrolyte Download PDFInfo
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- CN111484076A CN111484076A CN202010320249.6A CN202010320249A CN111484076A CN 111484076 A CN111484076 A CN 111484076A CN 202010320249 A CN202010320249 A CN 202010320249A CN 111484076 A CN111484076 A CN 111484076A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G31/00—Compounds of vanadium
- C01G31/02—Oxides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G31/00—Compounds of vanadium
- C01G31/003—Preparation involving a liquid-liquid extraction, an adsorption or an ion-exchange
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Abstract
The invention discloses a method for recovering high-purity vanadium from spent vanadium electrolyte, which comprises the steps of adding an oxidant into the spent vanadium electrolyte, oxidizing vanadium ions in the electrolyte into pentavalent ions, wherein the oxidant is formed by mixing sodium persulfate and potassium permanganate with the mass ratio of 1: 1.9-2.8; then adjusting the pH value of the electrolyte to 2-5; eluting the filtrate with ion exchange resin; adding a vanadium precipitation agent into the electrolyte after the elution treatment to obtain a solid precipitate, wherein the vanadium precipitation agent is (NH) with the mass ratio of 1-5:24)2S2O8And (NH)4)2SO4Forming; and finally, washing the obtained solid precipitate by sequentially adopting a vanadium precipitation agent aqueous solution and deionized water, drying, and then carrying out high-temperature roasting treatment to obtain vanadium pentoxide solid with the purity of more than 95%. The recovery process has strong operability, does not need large-scale equipment and has low recovery cost.
Description
Technical Field
The invention relates to the technical field of metal resource recovery processing, in particular to a method for recovering high-purity vanadium from a spent vanadium electrolyte.
Background
A vanadium redox battery (i.e. an all vanadium redox flow battery, abbreviated as VRB) is a redox battery in which the active material is in a liquid state of circulating flow. The VRB has the advantages of high reversible charge-discharge rate, long cycle life, high energy conversion efficiency, no cross contamination of positive and negative electrolytes, easy scale production and the like. The method has the advantages of high cost, short construction period, low system operation and maintenance cost, and especially has the characteristics of safe operation and environmental friendliness.
The vanadium battery system can be widely applied to the aspects of energy storage equipment for solar energy and wind energy power generation, large-scale emergency power supply systems, power station energy storage, peak clipping and valley filling of power systems, load leveling and the like. At present, vanadium batteries are built on a large scale and stably run.
The electric energy of the vanadium battery is stored in sulfuric acid electrolytic cells of vanadium ions with different valence states in a chemical energy mode, the electrolytic cells are pressed into a battery stack body through an external pump, the electrolytic cells circularly flow in different liquid storage tanks and closed loops of half batteries under the action of mechanical power, a proton exchange membrane is adopted as a diaphragm of a battery pack, an electrolyte solution parallelly flows on the surface of an electrode and generates electrochemical reaction, and current is collected and conducted through double electrode plates, so that the chemical energy stored in the solution is converted into the electric energy.
With the rapid growth of the application of the vanadium battery, the electrolyte of the waste vanadium battery is more and more, the electrolyte of the waste vanadium battery is a sulfuric acid solution of vanadium ions with different valence states, and the total vanadium content reaches 2 mol/L.
In chinese patent CN2012105140786, a method for preparing vanadyl sulfate from spent electrolyte for vanadium batteries is disclosed, which solves the problem of waste liquid treatment in the prior art that vanadium electrolyte is unbalanced in energy and cannot be used after being used for many times. The method takes the failure vanadium electrolyte as a raw material, the valence state of vanadium in the electrolyte is increased to pentavalent through battery charging, a proper amount of vanadium precipitation agent is added to precipitate the pentavalent vanadium, then an organic reducing agent is added, and the vanadyl sulfate crystal is prepared by normal temperature culture. But the recovery rate of vanadium in the process is low and can only reach about 80 percent.
In chinese patent CN2016109926029, a method for recycling spent electrolyte of vanadium battery is disclosed, which comprises the steps of: adding solid vanadium sulfate, sulfuric acid and water into the failed electrolyte in batches to obtain the electrolyte with certain electrolytic efficiency again. Although this process allows the reuse of spent electrolytes, the properties of the electrolytes obtained by reuse still have certain drawbacks, among whichThe main reason is that the failure electrolyte contains a large amount of Fe3+、SiO3 2-、Al3+、Mg2+And impurity ions are generated and the valence ratio of vanadium ions in the electrolyte is unstable.
The discharge amount of the electrolyte of the failed vanadium battery is very large, so that the recovery of high-purity vanadium metal from the waste liquid has a certain economic value, but the recovery cost is relatively high at present, the recovery rate is low, the impurity content in the recovered vanadium pentoxide is high, the quality of the recovered product is low, and the popularization and the use of the recovery process are also restricted.
Disclosure of Invention
Based on the above problems, the object of the present invention is to provide a method for recovering high purity vanadium from spent vanadium electrolytes. Because the metal impurities in the failure vanadium electrolyte are relatively more, the purity of the recovered vanadium is very easy to be lower in the recovery process of the metal vanadium. The invention adopts the following technical scheme for recovering and obtaining high-purity vanadium:
the recovery method of the invention comprises the following steps:
s1, adding an oxidant into the spent vanadium electrolyte, fully stirring for 30-60min at the temperature of 35-70 ℃, oxidizing vanadium ions in the electrolyte into pentavalent ions, wherein the molar ratio of the added oxidant to the vanadium ions in the electrolyte is 1.2-2:1, and the oxidant is formed by mixing sodium persulfate and potassium permanganate with the mass ratio of 1: 1.9-2.8;
s2, adjusting the pH value of the electrolyte to 2-5, fully stirring and filtering;
s3, eluting the filtrate by ion exchange resin;
s4, adding a vanadium precipitation agent accounting for 10-20% of the mass of the electrolyte into the electrolyte after elution treatment, and stirring for 1-2h at the temperature of 50-60 ℃ to obtain solid precipitates, wherein the vanadium precipitation agent is (NH) with the mass ratio of 1-5:24)2S2O8And (NH)4)2SO4Forming;
and S5, washing the solid precipitate obtained in the step S5 by using a vanadium precipitation agent aqueous solution and deionized water in sequence, drying, and then performing high-temperature roasting treatment to obtain high-purity vanadium pentoxide solid.
Specifically, in step S2 of the present invention, the oxidized electrolyte is concentrated before the pH is adjusted, so that the vanadium concentration in the electrolyte is 50-60 g/L.
Specifically, in step S2 of the present invention, the pH of the electrolyte solution is adjusted to 3.
Specifically, the eluent used in step S3 of the present invention is a polyion aqueous solution, and V is contained in the eluent5+43.52 g/L of Al3+The concentration is 4.36 mg/L, Ca2+The concentration is 1.58 mg/L, Fe3+The concentration is 5.73 Mg/L, Mg2+Ti at a concentration of 0.76 mg/L2+The concentration was 0.68 mg/L.
Specifically, the vanadium precipitation agent aqueous solution used in step S5 of the present invention is (NH) with a mass ratio of 1-5:24)2S2O8And (NH)4)2SO4Mixing, adding water, and dissolving to obtain precipitant with mass concentration of 10-20%.
Specifically, the washed precipitate is dried at 50-80 ℃ for 20-50min in step S5.
Specifically, the calcination temperature in step S5 is 550-700 ℃, and the calcination time is 3-5 h.
The recovery mechanism of the present invention is as follows: the method comprises the following steps of adding an oxidant into the failure vanadium electrolyte, and oxidizing all vanadium ions in a low valence state into pentavalent vanadium, wherein the vanadium recovery rate in the electrolyte is reduced because the conversion of the low valence vanadium into the high valence vanadium is not thorough enough in the existing electrolyte, and the oxidation of vanadium in the electrolyte can be realized by using a mixture of sodium persulfate and potassium permanganate with the mass ratio of 1:1.9-2.8 as the oxidant, and the vanadium in the electrolyte is oxidized into the pentavalent vanadium; then adjusting the pH value of the electrolyte to be acidic so that pentavalent vanadium ions exist in the electrolyte in the form of metavanadate, and further removing metal impurities in the electrolyte through ion exchange resin after filtering so as to enrich the vanadium ions in the electrolyte; and finally, adding a precipitator to obtain a vanadium precipitate, washing, drying and roasting at high temperature to obtain a high-purity vanadium pentoxide product.
Compared with the prior art, the invention has the following beneficial effects: the recovery process can completely recover vanadium ions in the electrolyte and obtain vanadium pentoxide solid with the purity of more than 95%. The recovery process has strong operability, does not need large-scale equipment and has low recovery cost.
Detailed Description
The present invention will be further described with reference to the following specific examples.
Example 1
A method for recovering high-purity vanadium from a spent vanadium electrolyte comprises the following steps:
s1, adding an oxidant into the spent vanadium electrolyte, fully stirring for 30min at the temperature of 70 ℃, oxidizing vanadium ions in the electrolyte into pentavalent ions, wherein the molar ratio of the added oxidant to the vanadium ions in the electrolyte is 1.5:1, and the oxidant is formed by mixing sodium persulfate and potassium permanganate in a mass ratio of 1: 2;
s2, concentrating the oxidized electrolyte to enable the concentration of vanadium in the electrolyte to be 50 g/L, adjusting the pH value of the electrolyte to be 3, fully stirring and filtering;
s3, eluting the filtrate with ion exchange resin to obtain an eluate V which is polyion water solution5+43.52 g/L of Al3+The concentration is 4.36 mg/L, Ca2+The concentration is 1.58 mg/L, Fe3+The concentration is 5.73 Mg/L, Mg2+Ti at a concentration of 0.76 mg/L2+The concentration is 0.68 mg/L;
s4, adding a vanadium precipitation agent accounting for 15% of the mass of the electrolyte into the electrolyte after the elution treatment, and stirring for 2h at the temperature of 60 ℃ to obtain a solid precipitate, wherein the vanadium precipitation agent is (NH) with the mass ratio of 3:24)2S2O8And (NH)4)2SO4Forming;
and S5, washing the solid precipitate obtained in the step S5 by sequentially adopting an aqueous solution with a vanadium precipitation agent with the mass concentration of 20% and deionized water, drying at 50 ℃ for 30min, and then carrying out high-temperature roasting treatment, wherein the roasting temperature is 550 ℃, and the roasting time is 4h, so that vanadium pentoxide solid with the purity of 99.7% is obtained.
Example 2
A method for recovering high-purity vanadium from a spent vanadium electrolyte comprises the following steps:
s1, adding an oxidant into the spent vanadium electrolyte, fully stirring for 30min at the temperature of 50 ℃, oxidizing vanadium ions in the electrolyte into pentavalent ions, wherein the molar ratio of the added oxidant to the vanadium ions in the electrolyte is 1.2:1, and the oxidant is formed by mixing sodium persulfate and potassium permanganate with the mass ratio of 1: 2.5;
s2, concentrating the oxidized electrolyte to enable the concentration of vanadium in the electrolyte to be 50 g/L, adjusting the pH value of the electrolyte to be 3, fully stirring and filtering;
s3, eluting the filtrate with ion exchange resin to obtain an eluate V which is polyion water solution5+43.52 g/L of Al3+The concentration is 4.36 mg/L, Ca2+The concentration is 1.58 mg/L, Fe3+The concentration is 5.73 Mg/L, Mg2+Ti at a concentration of 0.76 mg/L2+The concentration is 0.68 mg/L;
s4, adding a vanadium precipitation agent which accounts for 20% of the mass of the electrolyte into the electrolyte after the elution treatment, and stirring for 2h at the temperature of 60 ℃ to obtain solid precipitate, wherein the vanadium precipitation agent is (NH) with the mass ratio of 1:24)2S2O8And (NH)4)2SO4Forming;
and S5, washing the solid precipitate obtained in the step S5 by sequentially adopting an aqueous solution with a vanadium precipitation agent with the mass concentration of 20% and deionized water, drying at the temperature of 50 ℃ for 30min, and then carrying out high-temperature roasting treatment, wherein the roasting temperature is 600 ℃, and the roasting time is 3h, so that vanadium pentoxide solid with the purity of 97.5% is obtained.
Example 3
A method for recovering high-purity vanadium from a spent vanadium electrolyte comprises the following steps:
s1, adding an oxidant into the spent vanadium electrolyte, fully stirring for 30min at the temperature of 50 ℃, oxidizing vanadium ions in the electrolyte into pentavalent ions, wherein the molar ratio of the added oxidant to the vanadium ions in the electrolyte is 1.2:1, and the oxidant is formed by mixing sodium persulfate and potassium permanganate with the mass ratio of 1: 2.8;
s2, concentrating the oxidized electrolyte to enable the concentration of vanadium in the electrolyte to be 50 g/L, adjusting the pH value of the electrolyte to be 3, fully stirring and filtering;
s3, eluting the filtrate with ion exchange resin to obtain an eluate V which is polyion water solution5+43.52 g/L of Al3+The concentration is 4.36 mg/L, Ca2+The concentration is 1.58 mg/L, Fe3+The concentration is 5.73 Mg/L, Mg2+Ti at a concentration of 0.76 mg/L2+The concentration is 0.68 mg/L;
s4, adding a vanadium precipitation agent which accounts for 20% of the mass of the electrolyte into the electrolyte after the elution treatment, and stirring for 2h at the temperature of 60 ℃ to obtain a solid precipitate, wherein the vanadium precipitation agent is (NH) with the mass ratio of 5:24)2S2O8And (NH)4)2SO4Forming;
and S5, washing the solid precipitate obtained in the step S5 by sequentially adopting an aqueous solution with a vanadium precipitation agent mass concentration of 10-20% and deionized water, drying at 50-80 ℃ for 20-50min, and then carrying out high-temperature roasting treatment at 600 ℃ for 3h to obtain vanadium pentoxide solid with the purity of 98.4%.
Example 4
A method for recovering high-purity vanadium from a spent vanadium electrolyte comprises the following steps:
s1, adding an oxidant into the spent vanadium electrolyte, fully stirring for 30min at the temperature of 35 ℃, oxidizing vanadium ions in the electrolyte into pentavalent ions, wherein the molar ratio of the added oxidant to the vanadium ions in the electrolyte is 1.8:1, and the oxidant is formed by mixing sodium persulfate and potassium permanganate with the mass ratio of 1: 1.9;
s2, concentrating the oxidized electrolyte to enable the concentration of vanadium in the electrolyte to be 50 g/L, adjusting the pH value of the electrolyte to be 3, fully stirring and filtering;
s3, eluting the filtrate by using ion exchange resinThe eluent is a polyion water solution, and V in the eluent5+43.52 g/L of Al3+The concentration is 4.36 mg/L, Ca2+The concentration is 1.58 mg/L, Fe3+The concentration is 5.73 Mg/L, Mg2+Ti at a concentration of 0.76 mg/L2+The concentration is 0.68 mg/L;
s4, adding a vanadium precipitation agent accounting for 10% of the mass of the electrolyte into the electrolyte after the elution treatment, and stirring for 2h at the temperature of 60 ℃ to obtain a solid precipitate, wherein the vanadium precipitation agent is (NH) with the mass ratio of 2:14)2S2O8And (NH)4)2SO4Forming;
and S5, washing the solid precipitate obtained in the step S5 by sequentially adopting an aqueous solution with a vanadium precipitation agent with the mass concentration of 20% and deionized water, drying at the temperature of 80 ℃ for 50min, and then carrying out high-temperature roasting treatment, wherein the roasting temperature is 700 ℃, and the roasting time is 5h, so as to obtain vanadium pentoxide solid with the purity of 96.3%.
Comparative example 1
The treatment process described in example 1 was followed to treat spent electrolyte with sodium persulfate as the only oxidizing agent, the remainder being different, wherein the molar ratio of the sodium persulfate oxidizing agent added to the vanadium ions in the spent electrolyte was 1.5: 1. Finally, vanadium pentoxide solid with the purity of 83.5 percent is obtained by recovery.
Comparative example 2
According to the treatment process described in example 1, the spent electrolyte is treated by only using potassium permanganate as an oxidizing agent, and the rest processes are different, wherein the molar ratio of the addition amount of the sodium persulfate oxidizing agent to the vanadium ions in the spent electrolyte is 1.5: 1. Finally, vanadium pentoxide solid with the purity of 80.9 percent is obtained by recovery.
Comparative example 3
According to the treatment process described in example 1, the step of eluting with the ion exchange resin of step S3 was omitted, and the remaining steps were not changed, and finally, vanadium pentoxide solid having a purity of 75.4% was recovered.
Comparative example 4
The treatment process described in example 1 was followed to modify the vanadium precipitation agent to (NH)4)2S2O8Or (NH)4)2SO4The addition amount of one of the vanadium precipitating agents and other processes are the same as those in example 1, and finally, vanadium pentoxide solids with the purity of 79.1% and 82.7% are obtained by recovery.
The principles and embodiments of the present invention have been described herein using specific examples, which are provided only to help understand the method and the core concept of the present invention; meanwhile, for a person skilled in the art, according to the idea of the present invention, the specific embodiments and the application range may be changed. In view of the above, the present disclosure should not be construed as limiting the invention.
Claims (7)
1. A method for recovering high-purity vanadium from spent vanadium electrolyte is characterized by comprising the following steps:
s1, adding an oxidant into the spent vanadium electrolyte, fully stirring for 30-60min at the temperature of 35-70 ℃, oxidizing vanadium ions in the electrolyte into pentavalent ions, wherein the molar ratio of the added oxidant to the vanadium ions in the electrolyte is 1.2-2:1, and the oxidant is formed by mixing sodium persulfate and potassium permanganate with the mass ratio of 1: 1.9-2.8;
s2, adjusting the pH value of the electrolyte to 2-5, fully stirring and filtering;
s3, eluting the filtrate by ion exchange resin;
s4, adding a vanadium precipitation agent accounting for 10-20 wt% of the electrolyte into the electrolyte after elution treatment, and stirring for 1-2h at 50-60 ℃ to obtain solid precipitate, wherein the vanadium precipitation agent is (NH) with the mass ratio of 1-5:24)2S2O8And (NH)4)2SO4Forming;
and S5, washing the solid precipitate obtained in the step S5 by using a vanadium precipitation agent aqueous solution and deionized water in sequence, drying, and then performing high-temperature roasting treatment to obtain high-purity vanadium pentoxide solid.
2. The method for recovering high purity vanadium from spent vanadium electrolyte according to claim 1, wherein the oxidized electrolyte is concentrated before the pH is adjusted in step S2 so that the vanadium concentration in the electrolyte is 50-60 g/L.
3. The method for recovering high purity vanadium from spent vanadium electrolyte according to claim 1, wherein step S2 adjusts the pH of the electrolyte to 3.
4. The method of claim 1, wherein the eluent used in step S3 is a polyionic aqueous solution, and V is the eluent5+43.52 g/L of Al3+The concentration is 4.36 mg/L, Ca2+The concentration is 1.58 mg/L, Fe3+The concentration is 5.73 Mg/L, Mg2+Ti at a concentration of 0.76 mg/L2+The concentration was 0.68 mg/L.
5. The method for recovering high-purity vanadium from spent vanadium electrolyte according to claim 1, wherein the vanadium precipitation agent aqueous solution used in the step S5 is (NH) with the mass ratio of 1-5:24)2S2O8And (NH)4)2SO4Mixing, adding water, and dissolving to obtain precipitant with mass concentration of 10-20%.
6. The method for recovering high purity vanadium from spent vanadium electrolyte according to claim 1, wherein the step S5 is to dry the washed precipitate at a temperature of 50 to 80 ℃ for 20 to 50 min.
7. The method for recovering high-purity vanadium from spent vanadium electrolyte according to claim 1, wherein the roasting temperature in the step S5 is 550-700 ℃, and the roasting time is 3-5 h.
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