Method for recovering vanadium pentoxide from vanadium electrolyte
By adding surfactants and initiators to the vanadium electrolyte, combined with ultraviolet irradiation and back-extraction treatment, the problem of low recovery efficiency of vanadium electrolyte was solved, and high-purity vanadium pentoxide was efficiently recovered.
Patent Information
- Application Number
- CN202311661507.7
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2023-12-05
- Publication Date
- 2025-12-26
- Estimated Expiration
- 2043-12-05
AI Technical Summary
Existing technologies for vanadium electrolyte recovery are complex and inefficient, making it difficult to effectively recover vanadium pentoxide, which limits the promotion of all-vanadium redox flow batteries.
High-purity vanadium pentoxide product is obtained by adding surfactants and initiators to vanadium electrolyte, combined with ultraviolet light irradiation, and then undergoing one-stage and two-stage back-extraction treatments, including ultrasonic treatment and calcination.
It achieves efficient vanadium recovery with simple operation and low cost, with high recovery efficiency and purity reaching 99% and 95%, and is suitable for large-scale recovery of vanadium waste electrolyte.
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Figure CN117585718B_ABST
Abstract
Description
TECHNICAL FIELD
[0001] The application belongs to the technical field of vanadium recovery, and particularly relates to a method for recovering vanadium pentoxide in vanadium electrolyte. BACKGROUND
[0002] In view of the accelerated growth of the share of renewable energy in global energy production, the demand for large-scale energy storage has also been increasing. The standard features required for a successful energy storage system are fast response time, long life, ability to withstand a large number of charge and discharge life cycles, flexible design capacity to meet the needs of power generation and demand sides, and low cost. Although pumped storage power stations account for a much larger proportion of global energy production, they are gradually being limited in the field of modern energy and being replaced by some chemical energy due to geographical limitations and the requirement for a large amount of water. Lithium ion batteries, fuel cells, supercapacitors and redox flow batteries are widely entering the energy storage market. Compared with pumped storage, they have unique characteristics such as independent power design, easy expansion, long life, high safety and low maintenance. The all-vanadium redox flow (VFB) battery is in the leading position in the long-term and large-load energy demand. However, the problem of difficult recovery of vanadium waste electrolyte after use also limits its further promotion in the field of energy storage.
[0003] In VFB, the electrolyte is pumped through the electrode, and a better electrode will have a higher utilization rate of vanadium electrolyte, and a poor electrode will have a relatively poor utilization rate of vanadium electrolyte. However, despite this, vanadium ions will still exist in the electrolyte after the vanadium battery is used up. At the same time, since the cost of the vanadium battery is mostly derived from the electrolyte. Therefore, it is crucial to recover vanadium ions. However, the recovery process in the prior art has problems such as complex process and low recovery efficiency. SUMMARY
[0004] In view of the above deficiencies in the prior art, the application provides a method for recovering vanadium pentoxide in vanadium electrolyte, which has the advantages of simple operation, low cost, high recovery efficiency, and can effectively solve the problems existing in the prior art method.
[0005] To achieve the above-mentioned purpose, the technical solution adopted by the application to solve its technical problems is:
[0006] A method for recovering vanadium pentoxide in vanadium electrolyte, comprising the following steps:
[0007] (1) adding a surfactant and an initiator to the vanadium electrolyte, and then irradiating the solution with ultraviolet light;
[0008] (2) One-stage stripping treatment: adding ammonium chloride to the solution after ultraviolet irradiation and performing ultrasonic treatment, and collecting the precipitate; two-stage stripping treatment: then continuing to add sodium hydroxide and sodium chloride and performing ultrasonic treatment, and collecting the precipitate;
[0009] (3) Calcining the precipitates produced in the two stripping processes respectively to obtain two kinds of vanadium pentoxide products with different purities.
[0010] In the above scheme, the surface active agent is added to the vanadium electrolyte to increase the surface activation effect, promote the polymerization of vanadium ions in the solution, and make the vanadium ions complex with the acid ions in the solution to produce high acid vanadium ions, which is convenient for subsequent stripping to form a precipitate. The addition of ammonium persulfate can reduce the reaction energy, and under the condition of ultraviolet irradiation, it can further improve the combination of vanadium ions and acid ions, increase the precipitation effect in the subsequent stripping process, and improve the extraction efficiency and extraction rate of vanadium.
[0011] Further, the surface active agent in step (1) includes at least one of sodium dodecyl sulfonate, cetyltrimethylammonium bromide, and potassium lauryl ether phosphate, and the concentration of the surface active agent in the vanadium pentoxide solution is 0.5-2 mol / L.
[0012] In the above scheme, the concentration of the surface active agent is too small to promote the complexation of vanadium ions and acid ions, and the amount is too large, resulting in resource waste.
[0013] Further, the initiator in step (1) includes at least one of ammonium persulfate, cumene peroxide, and dibenzoyl peroxide, and the concentration of the initiator in the vanadium pentoxide solution is 0.5-2 mol / L.
[0014] In the above scheme, the concentration of the initiator is too small to sufficiently reduce the reaction energy and achieve the complexation effect, and the amount is too large, resulting in resource waste.
[0015] Further, the ultraviolet light irradiation power in step (1) is 10-50 W, and the irradiation time is 10-20 min.
[0016] In the above scheme, the ultraviolet irradiation power and time both affect the combination of vanadium ions and acid ions, and the ultraviolet irradiation power that is too large or too small cannot meet the requirements.
[0017] Further, the concentration of ammonium chloride in the solution in step (2) is 0.5-2 mol / L.
[0018] In the above scheme, high vanadate ions are produced in the pretreated solution, which can combine with ammonium ions to form a vanadium-containing precipitate. The concentration of ammonium chloride is too small to sufficiently complex vanadate ions, and the concentration is too large, resulting in waste.
[0019] Further, in the step (2) one-stage stripping process, the ultrasonic power is 500-700 W, the ultrasonic frequency is 25-100 kHz, and the ultrasonic time is 1-10 min.
[0020] In the above scheme, the ultrasonic treatment can increase the combination effect of vanadate and ammonium ions, and shorten the treatment time.
[0021] Further, in the step (2), the concentration of sodium hydroxide in the solution is 0.5-2 mol / L, and the concentration of sodium chloride is 0.5-2 mol / L.
[0022] In the above scheme, ammonium chloride is added to the vanadium electrolyte, and high vanadate ions are combined with ammonium ions to generate vanadium-containing precipitates in the solution, and then the vanadium ions are calcined and recovered. After the combination with the ammonium ions, the concentration of vanadium ions in the solution is reduced, and a more active sodium-based substance is needed to better combine the high vanadate ions to produce a precipitate, and sodium hydroxide and sodium chloride are added to the remaining solution to produce a vanadium-containing precipitate with slightly lower purity, and then calcined and recovered.
[0023] Further, in the step (2) two-stage stripping process, the ultrasonic power is 500-700 W, the ultrasonic frequency is 25-100 kHz, and the ultrasonic time is 1-10 min.
[0024] Further, in the step (3), the calcination temperature is 400-600 DEG C, and the calcination time is 1-3 h.
[0025] The beneficial effects of the present application are:
[0026] 1. The method in the present application adds a surfactant to the vanadium electrolyte to increase the surface activation effect, promote the polymerization of vanadium ions in the solution, and make the vanadium ions complex with the acid ions in the solution to produce high acid vanadium ions, which is convenient for subsequent stripping to form a precipitate. The addition of ammonium persulfate can reduce the reaction energy, and under the condition of ultraviolet irradiation, it can further improve the combination of vanadium ions and acid ions, increase the precipitation effect in the subsequent stripping process, greatly improve the leaching efficiency of vanadium, shorten the leaching time, and improve the extraction rate. This method is suitable for large-scale recovery of vanadium waste electrolyte.
[0027] 2. The method in the present application has the advantages of simple operation and low cost.
[0028] 3. The method in the present application can recover high-purity vanadium pentoxide products with a purity of more than 99% and vanadium pentoxide products with a purity of more than 95%, and has the advantages of high vanadium pentoxide recovery efficiency and high purity. BRIEF DESCRIPTION OF DRAWINGS
[0029] Figure 1A physical map of the vanadium pentoxide with purity greater than 99%;
[0030] Figure 2 A physical map of the vanadium pentoxide with purity greater than 95%. DETAILED DESCRIPTION
[0031] In order to make the objectives, technical solutions and advantages of the present application clearer, the present application will be further described in detail below with reference to the embodiments. It should be understood that the specific embodiments described herein are only used to explain the present application and not to limit the present application, i.e., the described embodiments are only a part of the embodiments of the present application, but not all the embodiments.
[0032] Therefore, the detailed description of the embodiments of the present application provided below is not intended to limit the scope of the claimed present application, but only represents selected embodiments of the present application. Based on the embodiments of the present application, all other embodiments obtained by those skilled in the art without making creative efforts fall within the scope of the present application.
[0033] It should be noted that the relational terms such as "first" and "second" and the like are used only to distinguish one entity or operation from another entity or operation, and do not necessarily require or imply that there is any such actual relationship or order between these entities or operations. Moreover, the terms "comprising", "including" or any other variant thereof are intended to cover non-exclusive inclusion, so that a process, method, article or apparatus including a series of elements includes not only those elements, but also other elements not explicitly listed, or other elements inherent to such a process, method, article or apparatus. Without more limitations, the element defined by the statement "comprising a" does not exclude the presence of additional identical elements in the process, method, article or apparatus including the element.
[0034] The features and performances of the present application will be further described in detail below with reference to the embodiments and the accompanying drawings.
[0035] Example 1
[0036] A method for recycling vanadium pentoxide in a vanadium electrolyte, comprising the following steps:
[0037] (1) adding a surfactant sodium dodecyl sulfonate and an initiator ammonium persulfate to a vanadium electrolyte with a concentration of 1.65M, the concentration of sodium dodecyl sulfonate in the solution is 0.5mol / L, and the concentration of ammonium persulfate is 0.5mol / L, then using ultraviolet light to irradiate the solution, the irradiation power is 10W, and the irradiation time is 10min;
[0038] (2) adding ammonium chloride to the solution after ultraviolet irradiation and performing ultrasonic treatment to carry out one-stage stripping treatment, and collecting the precipitate, wherein the concentration of ammonium chloride in the solution is 0.5 mol / L, the ultrasonic power is 500 W, the ultrasonic frequency is 25 Khz, and the ultrasonic time is 1 min; then continuing to add sodium hydroxide and sodium chloride to the solution and performing ultrasonic treatment to carry out two-stage stripping treatment, and collecting the precipitate, wherein the concentration of sodium hydroxide in the solution is 0.5 mol / L, the concentration of sodium chloride is 0.5 mol / L, the ultrasonic power is 500 W, the ultrasonic frequency is 25 Khz, and the ultrasonic time is 1 min;
[0039] (3) using a muffle furnace to calcine the precipitates produced in the two stripping processes respectively, the calcination temperature is 400 DEG C, the calcination time is 1 h, and two kinds of vanadium pentoxide products with different purities are prepared.
[0040] Example 2
[0041] A method for recovering vanadium pentoxide in a vanadium electrolyte, comprising the following steps:
[0042] (1) adding a surfactant sodium dodecyl sulfonate and an initiator ammonium persulfate to a vanadium electrolyte with a concentration of 1.65 M, the concentration of sodium dodecyl sulfonate in the solution is 0.5 mol / L, the concentration of ammonium persulfate is 1.0 mol / L, then using ultraviolet light to irradiate the solution, the irradiation power is 10 W, and the irradiation time is 15 min;
[0043] (2) adding ammonium chloride to the solution after ultraviolet irradiation and performing ultrasonic treatment to carry out one-stage stripping treatment, and collecting the precipitate, wherein the concentration of ammonium chloride in the solution is 0.5 mol / L, the ultrasonic power is 500 W, the ultrasonic frequency is 25 Khz, and the ultrasonic time is 1 min; then continuing to add sodium hydroxide and sodium chloride to the solution and performing ultrasonic treatment to carry out two-stage stripping treatment, and collecting the precipitate, wherein the concentration of sodium hydroxide in the solution is 0.5 mol / L, the concentration of sodium chloride is 0.5 mol / L, the ultrasonic power is 500 W, the ultrasonic frequency is 25 Khz, and the ultrasonic time is 1 min;
[0044] (3) using a muffle furnace to calcine the precipitates produced in the two stripping processes respectively, the calcination temperature is 400 DEG C, the calcination time is 1 h, and two kinds of vanadium pentoxide products with different purities are prepared.
[0045] Example 3
[0046] A method for recovering vanadium pentoxide in a vanadium electrolyte, comprising the following steps:
[0047] (1) adding a surfactant sodium dodecyl sulfonate and an initiator ammonium persulfate into a vanadium electrolyte with a concentration of 1.65M, the concentration of sodium dodecyl sulfonate in the solution is 0.5mol / L, the concentration of ammonium persulfate is 0.5mol / L, then irradiating the solution with ultraviolet light, the irradiation power is 50W, and the irradiation time is 20min;
[0048] (2) adding ammonium chloride to the solution after ultraviolet irradiation and performing ultrasonic treatment, performing one-stage stripping treatment, and collecting the precipitate, wherein the concentration of ammonium chloride in the solution is 2mol / L, the ultrasonic power is 700W, the ultrasonic frequency is 100Khz, and the ultrasonic time is 10min; then continuing to add sodium hydroxide and sodium chloride to it and performing ultrasonic treatment, performing two-stage stripping treatment, and collecting the precipitate, wherein the concentration of sodium hydroxide in the solution is 2mol / L, the concentration of sodium chloride is 2mol / L, the ultrasonic power is 700W, the ultrasonic frequency is 100Khz, and the ultrasonic time is 10min;
[0049] (3) using a muffle furnace to calcine the precipitates produced in the two stripping processes respectively, the calcination temperature is 400℃, the calcination time is 1h, and two kinds of vanadium pentoxide products with different purities are prepared.
[0050] Example 4
[0051] A method for recovering vanadium pentoxide in a vanadium electrolyte, comprising the following steps:
[0052] (1) adding a surfactant sodium dodecyl sulfonate and an initiator ammonium persulfate into a vanadium electrolyte with a concentration of 1.65M, the concentration of sodium dodecyl sulfonate in the solution is 1mol / L, the concentration of ammonium persulfate is 2mol / L, then irradiating the solution with ultraviolet light, the irradiation power is 10W, and the irradiation time is 20min;
[0053] (2) adding ammonium chloride to the solution after ultraviolet irradiation and performing ultrasonic treatment, performing one-stage stripping treatment, and collecting the precipitate, wherein the concentration of ammonium chloride in the solution is 2mol / L, the ultrasonic power is 700W, the ultrasonic frequency is 100Khz, and the ultrasonic time is 10min; then continuing to add sodium hydroxide and sodium chloride to it and performing ultrasonic treatment, performing two-stage stripping treatment, and collecting the precipitate, wherein the concentration of sodium hydroxide in the solution is 2mol / L, the concentration of sodium chloride is 2mol / L, the ultrasonic power is 700W, the ultrasonic frequency is 100Khz, and the ultrasonic time is 10min;
[0054] (3) using a muffle furnace to calcine the precipitates produced in the two stripping processes respectively, the calcination temperature is 600℃, the calcination time is 3h, and two kinds of vanadium pentoxide products with different purities are prepared.
[0055] Example 5
[0056] A method for recovering vanadium pentoxide in a vanadium electrolyte, comprising the following steps:
[0057] (1) adding a surfactant sodium dodecyl sulfonate and an initiator ammonium persulfate to a vanadium electrolyte with a concentration of 1.65M, the concentration of sodium dodecyl sulfonate in the solution being 1mol / L and the concentration of ammonium persulfate being 0.5mol / L, then irradiating the solution with ultraviolet light, the irradiation power being 50W and the irradiation time being 10min;
[0058] (2) adding ammonium chloride to the solution after ultraviolet irradiation and performing ultrasonic treatment, performing one-stage stripping treatment and collecting the precipitate, wherein the concentration of ammonium chloride in the solution is 2mol / L, the ultrasonic power is 700W, the ultrasonic frequency is 100Khz and the ultrasonic time is 10min; then continuing to add sodium hydroxide and sodium chloride to the solution and performing ultrasonic treatment, performing two-stage stripping treatment and collecting the precipitate, wherein the concentration of sodium hydroxide in the solution is 2mol / L, the concentration of sodium chloride is 2mol / L, the ultrasonic power is 700W, the ultrasonic frequency is 100Khz and the ultrasonic time is 10min;
[0059] (3) using a muffle furnace to calcine the precipitates produced in the two stripping processes respectively, the calcination temperature being 600℃ and the calcination time being 3h, to obtain two vanadium pentoxide products with different purities.
[0060] Example 6
[0061] A method for recovering vanadium pentoxide in a vanadium electrolyte, comprising the following steps:
[0062] (1) adding a surfactant sodium dodecyl sulfonate and an initiator ammonium persulfate to a vanadium electrolyte with a concentration of 1.65M, the concentration of sodium dodecyl sulfonate in the solution being 1mol / L and the concentration of ammonium persulfate being 0.5mol / L, then irradiating the solution with ultraviolet light, the irradiation power being 50W and the irradiation time being 10min;
[0063] (2) adding ammonium chloride to the solution after ultraviolet irradiation and performing ultrasonic treatment, performing one-stage stripping treatment and collecting the precipitate, wherein the concentration of ammonium chloride in the solution is 0.5mol / L, the ultrasonic power is 500W, the ultrasonic frequency is 25Khz and the ultrasonic time is 1min; then continuing to add sodium hydroxide and sodium chloride to the solution and performing ultrasonic treatment, performing two-stage stripping treatment and collecting the precipitate, wherein the concentration of sodium hydroxide in the solution is 0.5mol / L, the concentration of sodium chloride is 0.5mol / L, the ultrasonic power is 500W, the ultrasonic frequency is 25Khz and the ultrasonic time is 1min;
[0064] (3) Using a muffle furnace, the precipitates produced in the two stripping processes are calcined respectively, the calcination temperature is 400℃, and the calcination time is 1h, and two purity vanadium pentoxide products are prepared respectively.
[0065] Example 7
[0066] A method for recovering vanadium pentoxide in a vanadium electrolyte, comprising the following steps:
[0067] (1) adding a surfactant sodium dodecyl sulfonate and an initiator ammonium persulfate to a vanadium electrolyte with a concentration of 1.65M, the concentration of sodium dodecyl sulfonate in the solution is 1mol / L, the concentration of ammonium persulfate is 2mol / L, then the solution is irradiated with ultraviolet light, the irradiation power is 10W, and the irradiation time is 20min;
[0068] (2) adding ammonium chloride to the solution after ultraviolet irradiation and performing ultrasonic treatment, performing one-stage stripping treatment, and collecting the precipitate, wherein the concentration of ammonium chloride in the solution is 2mol / L, the ultrasonic power is 700W, the ultrasonic frequency is 100Khz, and the ultrasonic time is 10min; then continue to add sodium hydroxide and sodium chloride and perform ultrasonic treatment, perform two-stage stripping treatment, and collect the precipitate, wherein the concentration of sodium hydroxide in the solution is 2mol / L, the concentration of sodium chloride is 2mol / L, the ultrasonic power is 700W, the ultrasonic frequency is 100Khz, and the ultrasonic time is 10min;
[0069] (3) Using a muffle furnace, the precipitates produced in the two stripping processes are calcined respectively, the calcination temperature is 600℃, and the calcination time is 3h, and two purity vanadium pentoxide products are prepared respectively.
[0070] Example 8
[0071] A method for recovering vanadium pentoxide in a vanadium electrolyte, comprising the following steps:
[0072] (1) adding a surfactant sodium dodecyl sulfonate and an initiator ammonium persulfate to a vanadium electrolyte with a concentration of 1.65M, the concentration of sodium dodecyl sulfonate in the solution is 1mol / L, the concentration of ammonium persulfate is 1mol / L, then the solution is irradiated with ultraviolet light, the irradiation power is 10W, and the irradiation time is 10min;
[0073] (2) adding ammonium chloride to the solution after ultraviolet irradiation and performing ultrasonic treatment to carry out one-stage stripping treatment, and collecting the precipitate, wherein the concentration of ammonium chloride in the solution is 2 mol / L, the ultrasonic power is 700 W, the ultrasonic frequency is 100 Khz, and the ultrasonic time is 10 min; then continuing to add sodium hydroxide and sodium chloride to the solution and performing ultrasonic treatment to carry out two-stage stripping treatment, and collecting the precipitate, wherein the concentration of sodium hydroxide in the solution is 2 mol / L, the concentration of sodium chloride is 2 mol / L, the ultrasonic power is 700 W, the ultrasonic frequency is 100 Khz, and the ultrasonic time is 10 min;
[0074] (3) using a muffle furnace to calcine the precipitates produced in the two stripping processes respectively, the calcination temperature is 400 DEG C, the calcination time is 1 h, and two kinds of vanadium pentoxide products with different purities are prepared.
[0075] Example 9
[0076] A method for recovering vanadium pentoxide in a vanadium electrolyte, comprising the following steps:
[0077] (1) adding a surfactant sodium dodecyl sulfonate and an initiator ammonium persulfate to a vanadium electrolyte with a concentration of 1.65 M, the concentration of sodium dodecyl sulfonate in the solution is 0.5 mol / L, the concentration of ammonium persulfate is 1 mol / L, then using ultraviolet light to irradiate the solution, the irradiation power is 10 W, and the irradiation time is 10 min;
[0078] (2) adding ammonium chloride to the solution after ultraviolet irradiation and performing ultrasonic treatment to carry out one-stage stripping treatment, and collecting the precipitate, wherein the concentration of ammonium chloride in the solution is 2 mol / L, the ultrasonic power is 700 W, the ultrasonic frequency is 100 Khz, and the ultrasonic time is 10 min; then continuing to add sodium hydroxide and sodium chloride to the solution and performing ultrasonic treatment to carry out two-stage stripping treatment, and collecting the precipitate, wherein the concentration of sodium hydroxide in the solution is 2 mol / L, the concentration of sodium chloride is 2 mol / L, the ultrasonic power is 700 W, the ultrasonic frequency is 100 Khz, and the ultrasonic time is 10 min;
[0079] (3) using a muffle furnace to calcine the precipitates produced in the two stripping processes respectively, the calcination temperature is 400 DEG C, the calcination time is 1 h, and two kinds of vanadium pentoxide products with different purities are prepared.
[0080] Example 10
[0081] A method for recovering vanadium pentoxide in a vanadium electrolyte, comprising the following steps:
[0082] (1) adding a surfactant sodium dodecyl sulfonate and an initiator ammonium persulfate to a vanadium electrolyte with a concentration of 1.65M, the concentration of sodium dodecyl sulfonate in the solution is 2mol / L, the concentration of ammonium persulfate is 2mol / L, then using ultraviolet light to irradiate the solution, the irradiation power is 10W, the irradiation time is 10min;
[0083] (2) adding ammonium chloride to the solution after ultraviolet irradiation and performing ultrasonic treatment, performing one-stage stripping treatment, collecting the precipitate, wherein the concentration of ammonium chloride in the solution is 0.5mol / L, the ultrasonic power is 500W, the ultrasonic frequency is 25Khz, and the ultrasonic time is 1min; then continue to add sodium hydroxide and sodium chloride and perform ultrasonic treatment, perform two-stage stripping treatment, collect the precipitate, wherein the concentration of sodium hydroxide in the solution is 0.5mol / L, the concentration of sodium chloride is 0.5mol / L, the ultrasonic power is 500W, the ultrasonic frequency is 25Khz, and the ultrasonic time is 1min;
[0084] (3) using a muffle furnace to calcine the precipitates produced in the two stripping processes respectively, the calcination temperature is 400℃, the calcination time is 1h, and two kinds of purity of vanadium pentoxide products are prepared respectively.
[0085] Comparative Example 1
[0086] A method for recovering vanadium pentoxide in a vanadium electrolyte, comprising the following steps:
[0087] (1) adding a surfactant sodium dodecyl sulfonate to a vanadium electrolyte with a concentration of 1.65M, the concentration of sodium dodecyl sulfonate in the solution is 1mol / L;
[0088] (2) adding ammonium chloride to the solution after ultraviolet irradiation and performing ultrasonic treatment, performing one-stage stripping treatment, collecting the precipitate, wherein the concentration of ammonium chloride in the solution is 2mol / L, the ultrasonic power is 700W, the ultrasonic frequency is 100Khz, and the ultrasonic time is 10min; then continue to add sodium hydroxide and sodium chloride and perform ultrasonic treatment, perform two-stage stripping treatment, collect the precipitate, wherein the concentration of sodium hydroxide in the solution is 2mol / L, the concentration of sodium chloride is 2mol / L, the ultrasonic power is 700W, the ultrasonic frequency is 100Khz, and the ultrasonic time is 10min;
[0089] (3) using a muffle furnace to calcine the precipitates produced in the two stripping processes respectively, the calcination temperature is 600℃, the calcination time is 3h, and two kinds of purity of vanadium pentoxide products are prepared respectively.
[0090] Comparative Example 2
[0091] A method for recovering vanadium pentoxide in a vanadium electrolyte, comprising the following steps:
[0092] (1) irradiating a vanadium electrolyte with a concentration of 1.65M using ultraviolet light, the irradiation power being 10W and the irradiation time being 20min;
[0093] (2) adding ammonium chloride to the solution after ultraviolet irradiation and performing ultrasonic treatment, performing one-stage stripping treatment and collecting the precipitate, wherein the concentration of ammonium chloride in the solution is 2mol / L, the ultrasonic power is 700W, the ultrasonic frequency is 100Khz, and the ultrasonic time is 10min; then continuing to add sodium hydroxide and sodium chloride and performing ultrasonic treatment, performing two-stage stripping treatment and collecting the precipitate, wherein the concentration of sodium hydroxide in the solution is 2mol / L, the concentration of sodium chloride is 2mol / L, the ultrasonic power is 700W, the ultrasonic frequency is 100Khz, and the ultrasonic time is 10min;
[0094] (3) using a muffle furnace to calcine the precipitates produced in the two stripping processes respectively, the calcination temperature being 600℃ and the calcination time being 3h, to obtain two vanadium pentoxide products with different purities.
[0095] Experimental Example
[0096] The purity of the vanadium pentoxide products collected by the method in the examples was detected, and the recovery rate of vanadium was detected, and the specific detection results are shown in Table 1.
[0097] Table 1: Purity of vanadium pentoxide
[0098]
[0099] As can be seen from the data in the above table, the method in the present application can effectively remove vanadium from the electrolyte. In Comparative Example 1, the initiator and ultraviolet irradiation operation were cancelled, and in Comparative Example 2, the addition of surfactant and initiator was cancelled. By comparing the purity and recovery rate of vanadium pentoxide in the examples, it was found that after cancelling part of the operation in Comparative Examples 1 and 2, the purity of vanadium pentoxide became worse and the recovery rate became smaller.
Claims
1. A method for recovering vanadium pentoxide from a vanadium electrolyte, characterized in that, The method comprises the following steps: (1) adding a surfactant and an initiator into a vanadium electrolyte, and then irradiating the solution with ultraviolet light; the surfactant is sodium dodecyl sulfonate, and the initiator is ammonium persulfate; (2) one-stage stripping treatment: adding ammonium chloride into the solution after ultraviolet irradiation and performing ultrasonic treatment, and collecting the precipitate; two-stage stripping treatment: then continuously adding sodium hydroxide and sodium chloride into the solution and performing ultrasonic treatment, and collecting the precipitate; (3) calcining the precipitates produced in the two stripping processes respectively, and obtaining two kinds of vanadium pentoxide products with different purities.
2. The method for recovering vanadium pentoxide from vanadium electrolyte according to claim 1, characterized in that, The concentration of the surfactant in the vanadium pentoxide solution is 0.5-2 mol / L.
3. The method for recovering vanadium pentoxide from vanadium electrolyte according to claim 1, characterized in that, The concentration of the initiator in the vanadium pentoxide solution is 0.5-2 mol / L.
4. The method for recovering vanadium pentoxide from vanadium electrolyte according to claim 1, characterized in that, The ultraviolet light irradiation power in step (1) is 10-50 W, and the irradiation time is 10-20 min.
5. The method of recovering vanadium pentoxide from vanadium electrolyte according to claim 1, characterized in that, The concentration of ammonium chloride in the solution in step (2) is 0.5-2 mol / L.
6. The method of recovering vanadium pentoxide from vanadium electrolyte according to claim 1, wherein the vanadium electrolyte is a vanadium electrolyte obtained by extracting vanadium from a vanadium-containing material. In the one-stage stripping process in step (2), the ultrasonic power is 500-700 W, the ultrasonic frequency is 25-100 Khz, and the ultrasonic time is 1-10 min.
7. The method of recovering vanadium pentoxide from vanadium electrolyte according to claim 1, wherein the vanadium electrolyte is a vanadium electrolyte obtained by extracting vanadium from a vanadium-containing material. The concentration of sodium hydroxide in the solution in step (2) is 0.5-2 mol / L, and the concentration of sodium chloride is 0.5-2 mol / L.
8. The method of recovering vanadium pentoxide from vanadium electrolyte according to claim 1, wherein In the two-stage stripping process in step (2), the ultrasonic power is 500-700 W, the ultrasonic frequency is 25-100 Khz, and the ultrasonic time is 1-10 min.
9. The method of recovering vanadium pentoxide from vanadium electrolyte according to claim 1, wherein The calcination temperature in step (3) is 400-600 ℃, and the calcination time is 1-3 h.
Citation Information
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