CN109943734B - Method for improving stability of pentavalent vanadium leaching solution - Google Patents
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Abstract
The invention relates to a method for improving the stability of a pentavalent vanadium leaching solution, belonging to the technical field of vanadium metallurgy. The invention solves the technical problems that the solution system of pentavalent vanadium is unstable under the conditions of low pH value and high vanadium concentration of the leaching solution, and vanadium is easy to hydrolyze and precipitate to cause vanadium loss. The invention discloses a method for improving the stability of pentavalent vanadium leaching solution, which comprises the steps of mixing vanadium-containing material, phosphate and sulfuric acid, controlling the pH value of the mixed slurry to be 0.5-2.2, carrying out acid leaching, and carrying out solid-liquid separation to obtain high-concentration vanadium-containing leaching solution. The method can realize that the leachate solution system still keeps good stability under the conditions of higher pentavalent vanadium concentration and lower solution pH, and is favorable for deep extraction of vanadium-containing materials.
Description
Technical Field
The invention belongs to the technical field of vanadium metallurgy, and particularly relates to a method for improving the stability of a pentavalent vanadium leaching solution.
Background
Vanadium has wide application in the fields of metallurgy, chemical industry, aerospace and the like, and is an extremely important strategic resource. The main production raw material of the industrial vanadium product is vanadium-titanium magnetite, and the typical process flow is blast furnace ironmaking, vanadium extraction from vanadium-containing molten iron and vanadium slag production of vanadium oxide; in addition, part of vanadium products are derived from stone coal, vanadium ore and secondary vanadium-containing resources. In the production process of vanadium oxide, a vanadium-containing material blank or calcified roasting-acid leaching is a typical vanadium extraction process, and vanadium exists in a pentavalent vanadium form after the vanadium-containing material is roasted, so that a solution system is unstable under the conditions of low pH value of a leaching solution and high concentration of the pentavalent vanadium, and vanadium is easy to hydrolyze and precipitate to cause loss. In order to avoid adverse effects caused by vanadium hydrolysis, a mode of extracting vanadium by acid leaching twice is generally adopted in industry, namely, the pH value of acid leaching is controlled to be 2.8-3.5 for the first time, and high-concentration pentavalent vanadium can stably exist in the pH range; and controlling the pH value of acid leaching and the vanadium concentration of the leaching solution to be lower for the second time, so that vanadium is fully leached and is not hydrolyzed. However, the two-time acid leaching vanadium extraction mode has more operation processes and higher process cost. At present, no report related to leaching high-concentration pentavalent vanadium leachate from vanadium-containing materials by low pH is found, and a technology for controlling the pentavalent vanadium not to hydrolyze and precipitate under the condition of low pH needs to be developed.
Disclosure of Invention
The invention solves the technical problems that the solution system of pentavalent vanadium is unstable under the conditions of low pH value and high vanadium concentration of the leaching solution, and vanadium is easy to hydrolyze and precipitate to cause loss.
The technical scheme for solving the problems is to provide a method for improving the stability of the pentavalent vanadium leaching solution, which comprises the following steps:
mixing the vanadium-containing material, phosphate and sulfuric acid, carrying out acid leaching, and carrying out solid-liquid separation to obtain high-concentration vanadium-containing leachate.
Wherein the vanadium-containing material is V5+The vanadium-containing raw material with the mass content of more than 1 percent.
Wherein the phosphate is a phosphate which is soluble under a weakly acidic condition of pH 2.2-4.0.
Wherein the phosphate is at least one of sodium phosphate, potassium phosphate, ammonium phosphate, calcium phosphate, magnesium phosphate and their corresponding monohydrogen phosphate and dihydrogen phosphate.
Wherein the pH value of the mixed slurry is controlled to be 0.5-2.2 in the acid leaching process.
Wherein the addition amount of the phosphate is based on controlling the phosphorus concentration of the leachate to be 0.3-3 g/L.
Wherein the phosphorus concentration in the leaching solution is 0.3-3 g/L and V5+The concentration is 10-30 g/L.
Wherein the acid leaching temperature is 20-50 ℃, and the time is 30-90 min.
Wherein the acid leaching temperature is 25-35 ℃, and the time is 30-60 min.
Wherein the leaching solution is used for preparing vanadium oxide.
The invention has the beneficial effects that:
according to the invention, the phosphate is added in the acid leaching process, so that the hydrolytic precipitation of vanadium can be inhibited, and the vanadium loss is effectively reduced; according to the invention, the addition amount of phosphate and the acid leaching temperature and time are controlled, so that the good stability of the leachate solution system can be still maintained under the conditions of high pentavalent vanadium concentration and low solution pH, and the deep extraction of vanadium-containing materials is facilitated.
Detailed Description
The invention provides a method for deeply extracting vanadium from a vanadium-containing raw material, which specifically comprises the following steps:
mixing the vanadium-containing material, phosphate and sulfuric acid, carrying out acid leaching, and carrying out solid-liquid separation to obtain high-concentration vanadium-containing leachate.
The phosphate is added in the acid leaching process, so that the phosphorus concentration in the mixed slurry and the leachate is improved, vanadium and phosphorus form a vanadium-phosphorus heteropoly acid complex, and the loss of vanadium caused by vanadium hydrolysis precipitation is avoided.
The vanadium-containing material of the invention is especially for V5+The vanadium-containing raw material with the mass content of more than 1 percent is subjected to acid leaching to obtain leaching solution V5+≥10g/L。
In order to better inhibit the hydrolytic precipitation of vanadium, the invention selects phosphate which is soluble under the weak acidic condition that the pH value is 2.2-4.0.
Preferably, the phosphate of the present invention is selected from at least one of sodium phosphate, potassium phosphate, ammonium phosphate, calcium phosphate, magnesium phosphate and their corresponding monohydrogen phosphate and dihydrogen phosphate.
Furthermore, the pH value of the mixed slurry is controlled to be 0.5-2.2 in the acid leaching process. The lower pH value is beneficial to dissolving vanadium in the vanadium-containing material into the leaching solution, namely, the leaching rate of the vanadium is improved.
Wherein the addition amount of the phosphate is based on controlling the phosphorus concentration of the leachate to be 0.3-3 g/L.
Wherein the phosphorus concentration in the leaching solution is 0.3-3 g/L and V5+The concentration is 10-30 g/L.
Wherein the acid leaching temperature is 20-50 ℃, and the time is 30-90 min.
Preferably, the acid leaching temperature is 25-35 ℃, and the time is 30-60 min. Because the temperature is high, the hydrolysis and precipitation of pentavalent vanadium can be promoted more easily, energy is consumed, the stability of the pentavalent vanadium is better under the room temperature condition, and the acid leaching temperature is preferably 25-35 ℃ in consideration of the stability of the phosphapolyacid complex.
After the stable high-concentration vanadium-containing leaching solution is obtained, phosphorus is removed and vanadium is extracted according to the conventional method, so that the deep vanadium extraction of the high-vanadium material is realized.
Preferably, the stable high-concentration vanadium-containing leaching solution is obtained, the separation of vanadium and phosphorus can be further realized by utilizing a chemical phosphorus removal method, an ion exchange method and the like, and the vanadium-containing solution after dephosphorization is used for preparing vanadium oxide.
The invention is further illustrated and described by the following examples.
Example 1
Taking roasted vanadium-containing material (V)2O5 17.85%, P0.04%) 100g, and 3.78g of calcium phosphate were added to 350mL of tap water, the pH of the slurry was adjusted to 0.6 to 0.8 with sulfuric acid at room temperature, the mixture was stirred and reacted for 30min, solid-liquid separation was performed, and V was added to the acid leaching residue2O5The content is 0.75 percent, and the vanadium leaching rate is 96.0 percent; leachate V5+The concentration is 27.46g/L, the P concentration is 2.55g/L, and the solution system is stable.
Example 2
Taking roasted vanadium-containing material (V)2O517.85%, P0.04%) 100g, and 2.86g of magnesium phosphate were added to 450mL of tap water, the pH of the slurry was adjusted to 1.0 to 1.2 with sulfuric acid at room temperature, the mixture was stirred and reacted for 60min, solid-liquid separation was performed, and V was added to the acid leaching residue2O5The content is 0.83 percent, and the vanadium leaching rate is 95.7 percent; leachate V5+The concentration is 21.26g/L, the P concentration is 1.72g/L, and the solution system is stable.
Example 3
Taking roasted vanadium-containing material (V)2O517.85%, P0.04%) and 100g of the acid leaching residue, adding 5.46g of sodium phosphate into 350mL of tap water, adjusting the pH of the slurry to 1.3-1.5 with sulfuric acid at normal temperature, stirring and reacting for 70min, carrying out solid-liquid separation, and obtaining the V in the acid leaching residue2O5The content is 1.07 percent, and the vanadium leaching rate is 94.29 percent; leachate V5+The concentration is 26.94g/L, the P concentration is 2.95g/L, and the solution system is stable.
Example 4
Taking roasted vanadium-containing material (V)2O517.85%, P0.04%) and 100g of potassium phosphate, and 4.97g of potassium phosphate were added to 350mL of tap water, the pH of the slurry was adjusted to 1.7 to 1.9 with sulfuric acid at room temperature, the mixture was stirred and reacted for 80min, solid-liquid separation was performed, and V in the obtained acid leaching residue was performed2O5The content is 1.12 percent, and the vanadium leaching rate is 94.02 percent; leachate V5+The concentration is 26.86g/L, the P concentration is 2.08g/L, and the solution system is stable.
Example 5
Taking roasted vanadium-containing material (V)2O517.85%, P0.04%) and 100g of ammonium phosphate, and 4.64g of ammonium phosphate were added to 350mL of tap water, the pH of the slurry was adjusted to 2.0 to 2.2 with sulfuric acid at room temperature, the mixture was stirred and reacted for 90min, solid-liquid separation was performed, and the obtained acid-dipped solution was subjected to acid leachingV in the residue2O5The content is 1.24 percent, and the vanadium leaching rate is 93.38 percent; leachate V5+The concentration is 26.68g/L, the P concentration is 2.76g/L, and the solution system is stable.
Claims (17)
1. A method for improving the stability of a pentavalent vanadium leaching solution is characterized by comprising the following steps: the method comprises the following steps:
mixing vanadium-containing materials, phosphate and sulfuric acid, carrying out acid leaching, and carrying out solid-liquid separation to obtain high-concentration vanadium-containing leachate; the acid leaching process controls the pH of the mixed slurry to be 0.5-2.2; the addition amount of the phosphate is based on controlling the phosphorus concentration of the leachate to be 0.3-3 g/L; the acid leaching temperature is 20-50 ℃, and the time is 30-90 min.
2. The method for improving the stability of a pentavalent vanadium leaching solution according to claim 1, wherein: the vanadium-containing material is V5+The vanadium-containing raw material with the mass content of more than 1 percent.
3. The method for improving the stability of a pentavalent vanadium leaching solution according to claim 1 or 2, wherein: the phosphate is soluble under a weak acidic condition of pH = 2.2-4.0.
4. The method for improving the stability of a pentavalent vanadium leaching solution according to claim 1 or 2, wherein: the phosphate is at least one of sodium phosphate, potassium phosphate, ammonium phosphate, calcium phosphate, magnesium phosphate and their corresponding monohydrogen phosphate and dihydrogen phosphate.
5. The method for improving the stability of a pentavalent vanadium leaching solution according to claim 3, wherein: the phosphate is at least one of sodium phosphate, potassium phosphate, ammonium phosphate, calcium phosphate, magnesium phosphate and their corresponding monohydrogen phosphate and dihydrogen phosphate.
6. The method for improving the stability of a pentavalent vanadium leaching solution according to any one of claims 1, 2 or 5, wherein the method comprises the step of adding a catalyst to the pentavalent vanadium leaching solutionIs characterized in that: the phosphorus concentration in the leaching solution is 0.3-3 g/L and V5+The concentration is 10-30 g/L.
7. The method for improving the stability of a pentavalent vanadium leaching solution according to claim 3, wherein: the phosphorus concentration in the leaching solution is 0.3-3 g/L and V5+The concentration is 10-30 g/L.
8. The method for improving the stability of a pentavalent vanadium leaching solution according to claim 4, wherein: the phosphorus concentration in the leaching solution is 0.3-3 g/L and V5+The concentration is 10-30 g/L.
9. The method according to any one of claims 1 to 2, 5 or 7 to 8, wherein the method comprises the following steps: the acid leaching temperature is 25-35 ℃, and the time is 30-60 min.
10. The method for improving the stability of a pentavalent vanadium leaching solution according to claim 3, wherein: the acid leaching temperature is 25-35 ℃, and the time is 30-60 min.
11. The method for improving the stability of a pentavalent vanadium leaching solution according to claim 4, wherein: the acid leaching temperature is 25-35 ℃, and the time is 30-60 min.
12. The method for improving the stability of a pentavalent vanadium leaching solution according to claim 6, wherein: the acid leaching temperature is 25-35 ℃, and the time is 30-60 min.
13. The method for improving the stability of a pentavalent vanadium leaching solution according to any one of claims 1 to 2, 5, 7 to 8 or 10 to 12, wherein: the leachate is used for preparing vanadium oxide.
14. The method for improving the stability of a pentavalent vanadium leaching solution according to claim 3, wherein: the leachate is used for preparing vanadium oxide.
15. The method for improving the stability of a pentavalent vanadium leaching solution according to claim 4, wherein: the leachate is used for preparing vanadium oxide.
16. The method for improving the stability of a pentavalent vanadium leaching solution according to claim 6, wherein: the leachate is used for preparing vanadium oxide.
17. The method for improving the stability of a pentavalent vanadium leaching solution according to claim 9, wherein: the leachate is used for preparing vanadium oxide.
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| CN105671339A (en) * | 2016-03-03 | 2016-06-15 | 中国科学院过程工程研究所 | Method for extracting vanadium from ammonium phosphate leaching vanadium containing raw clinker |
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Effective date of registration: 20230922 Address after: 617000 Taoyuan street, East District, Panzhihua, Sichuan Province, No. 90 Patentee after: PANGANG GROUP PANZHIHUA IRON & STEEL RESEARCH INSTITUTE Co.,Ltd. Patentee after: Chengdu advanced metal material industry technology Research Institute Co.,Ltd. Address before: 617000 Taoyuan street, East District, Panzhihua, Sichuan Province, No. 90 Patentee before: PANGANG GROUP PANZHIHUA IRON & STEEL RESEARCH INSTITUTE Co.,Ltd. |