CN112266017A - Method for preparing sodium vanadate from vanadium-phosphorus-containing solid waste - Google Patents
Method for preparing sodium vanadate from vanadium-phosphorus-containing solid waste Download PDFInfo
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- CN112266017A CN112266017A CN202010954177.0A CN202010954177A CN112266017A CN 112266017 A CN112266017 A CN 112266017A CN 202010954177 A CN202010954177 A CN 202010954177A CN 112266017 A CN112266017 A CN 112266017A
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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
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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
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- 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
Abstract
The invention provides a method for preparing sodium vanadate from solid waste containing vanadium and phosphorus, which comprises the following steps: adding vanadium-phosphorus-containing solid waste into a sodium hydroxide solution, uniformly mixing, heating, stirring and leaching in an oxidizing atmosphere, adding a precipitator step by step, carrying out solid-liquid separation, and crystallizing to obtain sodium vanadate. The method adopts the method of oxidizing and leaching vanadium-phosphorus-containing solid waste under the alkaline condition, is beneficial to fully oxidizing and converting vanadium into sodium vanadate, improves the leaching rate of vanadium, simultaneously adopts a mode of fractional precipitation and impurity removal, and improves the separation effect of vanadium and phosphorus, thereby ensuring the quality of the prepared sodium vanadate product, ensuring the recovery rate of vanadium to be more than 86 percent and the purity of the sodium vanadate product to be more than 98 percent.
Description
Technical Field
The invention relates to the technical field of sodium vanadate preparation, in particular to a method for preparing sodium vanadate from vanadium-phosphorus-containing solid waste.
Background
The low-grade vanadium titano-magnetite in China has large reserves, and the vanadium titano-magnetite is used in many industrial productions such as steel making, petroleum refining, alumina production, power generation of power stations and the like, so a large amount of vanadium-containing solid waste is generated every year. Wherein, VPO catalyst (also known as vanadyl pyrophosphate (VO)2P2O7) It is a tetravalent vanadium phosphate and is mainly used as a catalyst for preparing maleic anhydride by selective oxidation of C4 hydrocarbon in industry. Currently, the current practice is. The VPO catalyst which is invalid every year can reach thousands of tons, if the VPO catalyst is not processed, not only can the vanadium resource be greatly wasted, but also the vanadium has certain toxicity, and can bring great pollution to the environment and influence the human health. Therefore, it is very important to find a way to recycle vanadium in the VPO catalyst.
At present, the main process for recovering vanadium in a VPO catalyst in China is a sodium roasting method, and the method uses sodium salts such as carbonate, sodium chloride or sodium sulfate and the like, and the sodium salts and the VPO catalyst are jointly calcined under the air atmosphere to oxidize the vanadium into pentavalent vanadium, so that a mixture of sodium vanadate and sodium phosphate is formed, the mixture is leached by water, vanadium and phosphorus are separated and extracted, and a vanadium product is prepared. However, the VPO solid catalyst has poor contact with sodium salt, which results in poor reactivity of the VPO solid catalyst and sodium salt, and cannot sufficiently convert vanadium to form sodium vanadate. In addition, the process has the problems of high roasting energy consumption, large amount of tail gas and dust, serious pollution and the like. Therefore, it is important to find a green recycling method for resource utilization of the VPO catalyst, which can reduce the treatment energy consumption and has high vanadium utilization rate and is suitable for industrial production.
Disclosure of Invention
Aiming at the problems of high energy consumption, high vanadium loss rate and low purity of prepared vanadium products in the existing vanadium-phosphorus-containing solid waste treatment, the invention provides a method for preparing sodium vanadate by using vanadium-phosphorus-containing solid waste.
In order to solve the technical problems, the technical scheme provided by the invention is as follows:
a method for preparing sodium vanadate from vanadium-phosphorus-containing solid waste comprises the following steps:
adding vanadium-phosphorus-containing solid waste into a sodium hydroxide solution, uniformly mixing, heating, stirring and leaching in an oxidizing atmosphere, adding a precipitator step by step, carrying out solid-liquid separation, and crystallizing to obtain sodium vanadate.
Preferably, the method for preparing sodium vanadate by using the vanadium and phosphorus containing solid waste specifically comprises the following steps:
crushing vanadium and phosphorus-containing solid waste, adding the crushed vanadium and phosphorus-containing solid waste into a sodium hydroxide solution, and uniformly mixing to obtain mixed slurry; introducing oxidizing gas into the mixed slurry, heating, stirring and leaching, and carrying out solid-liquid separation to obtain vanadium-containing leaching solution;
step two, adding a first precipitator into the vanadium-containing leaching solution, heating for reaction, and carrying out solid-liquid separation to obtain a primary purified solution; adding a second precipitator into the primary purified liquid, heating for reaction, and carrying out solid-liquid separation to obtain a vanadium-containing purified liquid; wherein the first precipitator is a soluble magnesium salt and/or a soluble aluminum salt, and the second precipitator is an alkaline calcium compound;
and step three, cooling and crystallizing the vanadium-containing purified liquid, and carrying out solid-liquid separation to obtain sodium vanadate.
Compared with the prior art, the method adopts a mode of oxidizing and leaching the vanadium-phosphorus-containing solid waste in a sodium hydroxide solution, so that vanadium in the vanadium-phosphorus-containing solid waste is oxidized and leached under an alkaline condition, the reactivity of the vanadium is improved, the vanadium is favorably and fully oxidized and converted into sodium vanadate, the leaching rate of the vanadium is improved, and meanwhile, a mode of fractional precipitation and impurity removal is adopted, the separation effect of vanadium and phosphorus is improved, and the quality of a prepared sodium vanadate product is ensured. The method for preparing the sodium vanadate from the vanadium-phosphorus-containing solid waste can ensure that the recovery rate of vanadium is more than 86 percent, and the purity of the prepared sodium vanadate product is more than 98 percent.
Preferably, the vanadium-phosphorus-containing solid waste is VPO spent catalyst.
Preferably, in the first step, the vanadium-phosphorus-containing solid waste is crushed to 50-200 meshes.
The preferable crushing fineness is beneficial to the full oxidation leaching of vanadium in the vanadium-phosphorus-containing solid waste.
Preferably, in the first step, the oxidizing gas is oxygen or compressed air.
Preferably, in the step one, the flow rate of the oxidizing gas is 0.1-0.5 m3/h。
The preferred flow rate is favorable for fully oxidizing vanadium in the vanadium-phosphorus-containing solid waste.
Preferably, in the first step, the mass concentration of the sodium hydroxide solution is 5-15 wt%, and the mass-to-volume ratio of the vanadium-phosphorus-containing solid waste to the sodium hydroxide solution is 1: 3-6, wherein the unit of mass is g, and the unit of volume is ml.
The optimized concentration and addition of the sodium hydroxide solution are beneficial to improving the reactivity of vanadium, so that the vanadium is fully converted into sodium vanadate, and the leaching rate of the vanadium is improved.
Preferably, in the first step, the temperature for heating, stirring and leaching is 85-120 ℃, and the leaching time is 1-4 hours.
The optimal heating temperature is beneficial to fully oxidizing vanadium in the vanadium-phosphorus-containing solid waste, and is beneficial to improving the leaching rate and shortening the leaching time.
Preferably, in the second step, the first precipitator is at least one of magnesium sulfate, magnesium chloride, aluminum sulfate or aluminum chloride.
Preferably, in the second step, the second precipitator is one or both of calcium oxide and calcium hydroxide.
Preferably, in the second step, the addition amount of the first precipitator is 5-8 g/L, and the addition amount of the second precipitator is 0.5-2 g/L.
The preferable first precipitator and the second precipitator adopt a specific adding sequence, so that the separation effect of vanadium and phosphorus can be improved, and the loss of vanadium can be reduced.
Preferably, in the second step, the first precipitator is added and then the heating temperature is 80-95 ℃, and the reaction time is 0.5-1 h; and adding a second precipitator, and then heating at 80-95 ℃ for 0.5-1 h.
The optimized reaction temperature and time are favorable for fully removing impurities and improving the purity of the sodium vanadate product.
In the third step, the temperature for cooling and crystallizing is 0-40 ℃ and the time is 1-4 h.
The preferable temperature and time for cooling and crystallizing can improve the purity of the sodium vanadate product.
Preferably, the crystallization mother liquor obtained by solid-liquid separation after crystallization in the third step is used for preparing the sodium hydroxide solution in the first step.
The generated liquid phase is returned to the leaching procedure for recycling, no wastewater is discharged, the wastewater treatment components are reduced, and the economic and environmental benefits of the process are improved.
The method for preparing sodium vanadate by using vanadium-phosphorus-containing solid waste provided by the invention does not need high-temperature roasting, the reaction temperature of the whole process is low, the process is simple, the operation is easy, the vanadium extraction rate is high, the impurity removal efficiency is high, the impurity removal effect is good, the vanadium loss can be effectively reduced, the quality of a sodium vanadate product is improved, the energy consumption can be saved, dust and tail gas polluting the environment are not generated, and the method has remarkable economic benefit and environmental benefit and wide application prospect.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
In the following examples the vanadium content of the VPO spent catalyst was 27 wt% and the phosphorus content was 19 wt%.
Example 1
A method for preparing sodium vanadate by using a VPO spent catalyst comprises the following steps:
step one, crushing 100g of VPO spent catalyst to 50-200 meshes, adding 400mL of sodium hydroxide solution with the mass concentration of 10 wt%, uniformly mixing, adding the mixed material into a reaction kettle, and adding the mixed material into the reaction kettle by 0.1m3Introducing compressed air at the flow rate of/h, heating to 90 ℃, stirring and leaching for 3h, and filtering to obtain vanadium-containing leaching solution; 24.6g/L of vanadium, 18.2g/L of phosphorus and 95.9% of vanadium leaching rate in the vanadium-containing leaching solution;
step two, adding 7.5g/L of aluminum sulfate into the vanadium-containing leaching solution, heating to 95 ℃, reacting for 0.5h, filtering, adding 0.5g/L of calcium oxide into the filtrate, heating to 95 ℃, reacting for 0.5h, and filtering to obtain vanadium-containing purified liquid; the phosphorus content in the vanadium-containing purification liquid is 0.078g/L, the vanadium content is 23.8g/L, and the vanadium recovery rate is 88.1 percent;
and step three, cooling the vanadium-containing purified liquid to 0 ℃, crystallizing for 1h, and filtering to obtain sodium vanadate. The HPLC purity of sodium vanadate was 98.3%.
Example 2
A method for preparing sodium vanadate by using a VPO spent catalyst comprises the following steps:
step one, crushing 100g of VPO spent catalyst to 50-200 meshes, adding 300mL of sodium hydroxide solution with the mass concentration of 15 wt%, uniformly mixing, adding the mixed material into a reaction kettle, and adding the mixed material into the reaction kettle by 0.5m3Introducing oxygen at the flow rate of/h, heating to 85 ℃, stirring and leaching for 4h, and filtering to obtain vanadium-containing leaching solution; 26.8g/L of vanadium, 17.6g/L of phosphorus and 96.2% of vanadium leaching rate in the vanadium-containing leaching solution;
step two, adding 8g/L of mixture (mass ratio is 1: 1) of magnesium chloride and aluminum sulfate into the vanadium-containing leaching solution, heating to 90 ℃ for reaction for 1 hour, filtering, adding 1.5g/L of calcium hydroxide into the filtrate, heating to 80 ℃ for reaction for 1 hour, and filtering to obtain vanadium-containing purified liquid; the phosphorus content in the vanadium-containing purification liquid is 0.064g/L, the vanadium content is 26.1g/L, and the vanadium recovery rate is 86.9 percent;
and step three, cooling the vanadium-containing purified liquid to 10 ℃, crystallizing for 2 hours, and filtering to obtain sodium vanadate. The HPLC purity of sodium vanadate was 98.8%.
Example 3
A method for preparing sodium vanadate by using a VPO spent catalyst comprises the following steps:
step one, crushing 100g of VPO spent catalyst to 50-200 meshes, adding 600mL of sodium hydroxide solution with the mass concentration of 5 wt%, uniformly mixing, adding the mixed material into a reaction kettle, and adding the mixed material into the reaction kettle by 0.3m3Introducing oxygen at the flow rate of/h, heating to 120 ℃, stirring and leaching for 1h, and filtering to obtain vanadium-containing leaching solution; the vanadium content in the vanadium-containing leaching solution is 25.7g/L, the phosphorus content is 18.5g/L, and the vanadium leaching rate is 95.9 percent;
adding 5g/L magnesium sulfate into the vanadium-containing leaching solution, heating to 80 ℃, reacting for 1h, filtering, adding 2g/L calcium oxide into the filtrate, heating to 90 ℃, reacting for 1h, and filtering to obtain vanadium-containing purified liquid; the phosphorus content in the vanadium-containing purification liquid is 0.067g/L, the vanadium content is 24.5g/L, and the vanadium recovery rate is 87.5 percent;
and step three, cooling the vanadium-containing purified liquid to 40 ℃, crystallizing for 4 hours, and filtering to obtain sodium vanadate. The HPLC purity of sodium vanadate was 98.5%.
In examples 1 to 3, the mother liquid of crystallization obtained by solid-liquid separation after the crystallization in step three can be used for the preparation of the sodium hydroxide solution in step one.
In conclusion, the method for preparing sodium vanadate from the vanadium-phosphorus-containing solid waste provided by the invention has the advantages that through controlling various process parameters, impurities in the leachate are effectively removed on the premise of ensuring that vanadium in the vanadium-phosphorus-containing solid waste is fully leached, the quality of a subsequent sodium vanadate product is ensured, high-temperature roasting is not needed, the process operation is simple and convenient, the cost is reduced, and the method has a wide application prospect.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents or improvements made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (10)
1. A method for preparing sodium vanadate from vanadium-phosphorus-containing solid waste is characterized by comprising the following steps: adding vanadium-phosphorus-containing solid waste into a sodium hydroxide solution, uniformly mixing, heating, stirring and leaching in an oxidizing atmosphere, adding a precipitator step by step, carrying out solid-liquid separation, and crystallizing to obtain sodium vanadate.
2. The method for preparing sodium vanadate from solid waste containing vanadium and phosphorus according to claim 1, which comprises the following steps:
crushing vanadium and phosphorus-containing solid waste, adding the crushed vanadium and phosphorus-containing solid waste into a sodium hydroxide solution, and uniformly mixing to obtain mixed slurry; introducing oxidizing gas into the mixed slurry, heating, stirring and leaching, and carrying out solid-liquid separation to obtain vanadium-containing leaching solution;
step two, adding a first precipitator into the vanadium-containing leaching solution, heating for reaction, and carrying out solid-liquid separation to obtain a primary purified solution; adding a second precipitator into the primary purified liquid, heating for reaction, and carrying out solid-liquid separation to obtain a vanadium-containing purified liquid; wherein the first precipitator is a soluble magnesium salt and/or a soluble aluminum salt, and the second precipitator is an alkaline calcium compound;
and step three, cooling and crystallizing the vanadium-containing purified liquid, and carrying out solid-liquid separation to obtain sodium vanadate.
3. The method for preparing sodium vanadate from the vanadium-phosphorus-containing solid waste as claimed in claim 2, wherein the vanadium-phosphorus-containing solid waste is a VPO spent catalyst.
4. The method for preparing sodium vanadate from solid waste containing vanadium and phosphorus as claimed in claim 3, wherein in the first step, the solid waste containing vanadium and phosphorus is crushed to 50-200 meshes; and/or
In the first step, the oxidizing gas is oxygen or compressed air.
5. The method for preparing sodium vanadate from vanadium-phosphorus-containing solid waste as claimed in claim 3, wherein in the first step, the mass concentration of the sodium hydroxide solution is 5-15 wt%, and the mass-to-volume ratio of the vanadium-phosphorus-containing solid waste to the sodium hydroxide solution is 1: 3-6, wherein the unit of mass is g, and the unit of volume is ml; and/or
In the first step, the flow rate of the oxidizing gas is 0.1-0.5 m3/h。
6. The method for preparing sodium vanadate from solid waste containing vanadium and phosphorus according to claim 3, wherein in the first step, the temperature for heating, stirring and leaching is 85-120 ℃, and the leaching time is 1-4 h.
7. The method for preparing sodium vanadate from solid waste containing vanadium and phosphorus according to claim 3, wherein in the second step, the first precipitator is at least one of magnesium sulfate, magnesium chloride, aluminum sulfate or aluminum chloride; and/or
In the second step, the second precipitator is one or two of calcium oxide or calcium hydroxide.
8. The method for preparing sodium vanadate from the vanadium-phosphorus containing solid waste as claimed in claim 7, wherein in the second step, the addition amount of the first precipitator is 5-8 g/L, and the addition amount of the second precipitator is 0.5-2 g/L.
9. The method for preparing sodium vanadate from the vanadium-phosphorus-containing solid waste as claimed in claim 7, wherein in the second step, the first precipitant is added and then the heating temperature is 80-95 ℃, and the reaction time is 0.5-1 h; and adding a second precipitator, and then heating at 80-95 ℃ for 0.5-1 h.
10. The method for preparing sodium vanadate from solid waste containing vanadium and phosphorus according to claim 3, wherein in the third step, the temperature for cooling crystallization is 0-40 ℃ and the time is 1-4 h.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115417392A (en) * | 2022-08-29 | 2022-12-02 | 广东邦普循环科技有限公司 | Method for recovering sodium phosphovanadate anode material |
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Cited By (2)
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