CN110951970A - Method for recovering vanadium from vanadium-containing underflow slag - Google Patents
Method for recovering vanadium from vanadium-containing underflow slag Download PDFInfo
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- CN110951970A CN110951970A CN201911190799.4A CN201911190799A CN110951970A CN 110951970 A CN110951970 A CN 110951970A CN 201911190799 A CN201911190799 A CN 201911190799A CN 110951970 A CN110951970 A CN 110951970A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
- C22B7/007—Wet processes by acid leaching
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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
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B34/00—Obtaining refractory metals
- C22B34/20—Obtaining niobium, tantalum or vanadium
- C22B34/22—Obtaining vanadium
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Abstract
The invention relates to a method for recovering vanadium from vanadium-containing underflow slag, belonging to the technical field of vanadium recovery from vanadium-containing materials. The invention provides a method for recovering vanadium from vanadium-containing underflow slag, which comprises the following steps: collecting a liquid phase of the acid vanadium precipitation of the vanadium slag, and according to a liquid-solid ratio (2-4): 1 ml/g, adding vanadium-containing underflow slag into the liquid phase, fully leaching at 70-90 ℃, carrying out solid-liquid separation, and collecting leachate to obtain a vanadium-containing solution. The invention further provides a method for preparing a vanadium oxide product by using the vanadium-containing solution. The method utilizes the liquid phase of the acid vanadium precipitation of the vanadium slag to leach the vanadium-containing underflow slag, can prepare high-purity vanadium oxide products, has high vanadium recovery rate, and realizes the recycling of the acid vanadium precipitation waste liquid. Compared with the existing recovery method, the method has the advantages of low material consumption, short flow, low cost and the like.
Description
Technical Field
The invention relates to a method for recovering vanadium from vanadium-containing underflow slag, belonging to the technical field of vanadium recovery from vanadium-containing materials.
Background
The industrial vanadium extraction from vanadium slag mainly comprises the process flows of sodium roasting, water leaching, impurity removal and vanadium precipitation, wherein the impurity removal of the vanadium-containing leaching solution is mainly to remove silicon and phosphorus in the leaching solution, so that support is provided for obtaining high-quality vanadium products. Calcium chloride solution or aluminum sulfate solution is usually adopted when silicon and phosphorus are removed from the leachate, however, vanadium and calcium or aluminum form precipitates in the impurity removal process, the precipitates enter the underflow slag after impurity removal, and the vanadium content of the underflow slag can reach 10-20%. In order to improve the utilization rate of vanadium resources, the recovery of vanadium from underflow slag becomes a hotspot and difficulty of industrial research.
CN103911521 discloses a method for recovering vanadium from phosphorus removal underflow slag, wherein the phosphorus removal underflow slag is leached by oxalate solution to obtain alkaline vanadium-containing leachate, the pH value of the leachate is adjusted to 8-11, and ammonium metavanadate products are obtained by precipitating vanadium.
CN106048227 discloses a method for efficiently recovering vanadium in vanadium-containing underflow slag, mixing, grinding and soaking vanadium-containing underflow slag slurry and vanadium-containing clinker alkaline leaching slurry according to the mass ratio of 1: 1-3 to obtain mixed slurry, filtering to obtain vanadium liquid and filter residue, wherein the vanadium liquid is used for preparing ammonium polyvanadate; and mixing the filter residue with water, and performing secondary leaching to realize high-efficiency recovery of vanadium in the underflow slag.
CN101182037 discloses a method for recovering vanadium oxide from phosphorus removal underflow, which comprises directly leaching phosphorus removal underflow slag with a carbonate aqueous solution, performing solid-liquid separation after the leaching reaction is finished, removing silicon from the leachate, using the leachate for vanadium precipitation to prepare ammonium polyvanadate or ammonium metavanadate, and returning vanadium precipitation wastewater to the leaching process for use.
At present, no report related to leaching and recovering vanadium in vanadium-containing underflow slag by utilizing a liquid phase of acid vanadium precipitation of the vanadium slag is found.
Disclosure of Invention
The invention aims to provide a method for recovering vanadium from vanadium-containing underflow slag.
The invention provides a method for recovering vanadium from vanadium-containing underflow slag, which comprises the following steps: collecting a liquid phase of the acid vanadium precipitation of the vanadium slag, and according to a liquid-solid ratio (2-4): 1 ml/g, adding vanadium-containing underflow slag into the liquid phase, fully leaching at 70-90 ℃, carrying out solid-liquid separation, and collecting leachate to obtain a vanadium-containing solution.
Further, the liquid phase of the acid vanadium precipitation of the vanadium slag meets at least one of the following conditions:
the liquid phase of the acid vanadium precipitation of the vanadium slag contains the following chemical components: cr (chromium) component6+1.2-2.5g/L、Cr3+≤0.01g/L、V4+0.2-0.4g/L、Na+25-35g/L、NH4 +0-0.1g/L、SO4 2-80-110g/L、Cl-1-3g/L、Ca2+0.2-0.4g/L；
The solid content of the liquid phase of the acid vanadium precipitation of the vanadium slag is 120-150 g/L;
the pH value of the liquid phase of the acid vanadium precipitation of the vanadium slag is 2-3;
controlling the temperature of the liquid phase of the acid vanadium precipitation of the vanadium slag to be above 60 ℃;
preferably, the temperature of the liquid phase of the acid vanadium precipitation of the vanadium slag is controlled to be 60-85 ℃.
Further, the vanadium-containing underflow slag comprises the following chemical components in percentage by mass: v2O520～28％，Ca10～18％，Al 3～15％，Si 5～12％，P 0.5～3.5％，Fe 3～8％，Ti 2～5％，Mg 0.5～2.5％，Mn 3～8％。
Further, the pH value of the vanadium-containing underflow slag is 8-10.
Further, the stirring time is 60-90 min.
Preferably, the stirring time is 65-80 min.
The invention provides a preparation method of vanadium pentoxide, which comprises the following steps: and recovering vanadium from vanadium-containing underflow slag according to the method, then performing acidic vanadium precipitation, performing solid-liquid separation, collecting a solid phase to obtain ammonium polyvanadate, and calcining to obtain vanadium pentoxide.
Further, the preparation method of the vanadium pentoxide meets at least one of the following conditions:
carrying out acid vanadium precipitation under the condition that the pH value is 2.0-3.0;
preferably, acid vanadium precipitation is carried out under the condition that the pH value is 2.0-2.5;
adding ammonium salt to precipitate vanadium;
preferably, the ammonium salt is at least one selected from ammonium sulfate, ammonium chloride, ammonium carbonate and ammonium bicarbonate;
preferably, the ratio of ammonium: the mass ratio of vanadium is (1.5-3): 1;
the temperature of the acid vanadium precipitation is 90-95 ℃;
the time for precipitating vanadium in the acid is 80-90 min.
Further, mixing the recovered vanadium-containing solution with the solution of the vanadium slag leaching solution after impurity removal, and performing acidic vanadium precipitation together.
The invention provides a preparation method of vanadium trioxide, which comprises the following steps: and preparing vanadium pentoxide according to the method, and then reducing to obtain vanadium trioxide.
Further, the reaction with coal gas is carried out for reduction.
The vanadium-containing underflow slag refers to impurity-removing slag generated when leachate obtained by sodium salt vanadium extraction water of vanadium slag is dephosphorized or impurity-removed by adopting calcium chloride or aluminum sulfate.
The invention provides a method for recovering vanadium from vanadium-containing underflow slag, which utilizes a liquid phase of acid vanadium precipitation of the vanadium slag to leach the vanadium-containing underflow slag, can prepare a high-purity vanadium oxide product, has high vanadium recovery rate, and realizes the recycling of acid vanadium precipitation waste liquid. Compared with the existing recovery method, the method has the advantages of low material consumption, short flow, low cost and the like.
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FIG. 1 is a process flow diagram of an embodiment of the present invention.
Detailed Description
The scheme of the invention will be explained with reference to the examples. It will be appreciated by those skilled in the art that the following examples are illustrative of the invention only and should not be taken as limiting the scope of the invention. The examples, where specific techniques or conditions are not indicated, are to be construed according to the techniques or conditions described in the literature in the art or according to the product specifications. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products commercially available.
The supernatant described in the following examples, namely the supernatant produced when vanadium slag is subjected to sodium salt roasting, water leaching and impurity removal, and then the impurity removal solution is subjected to acid vanadium precipitation, and the chemical components of the supernatant comprise: cr (chromium) component6+1.67g/L、Cr3+0.005g/L、V4+0.28g/L、Na+30.43g/L、NH4 +0.05g/L、SO4 2-91.28g/L、Cl-2.09g/L、Ca2+0.321g/L, solid content of 140g/L and pH of 2-3.
The underflow slag described in the following examples, namely the impurity-removing slag generated when leachate obtained by sodium salt vanadium extraction water of vanadium slag is dephosphorized or impurity-removed by calcium chloride or aluminum sulfate, contains the following chemical components in percentage by mass: v2O520-28%, Ca 10-18%, Al 3-15%, Si 5-12%, P0.5-3.5%, Fe 3-8%, Ti 2-5%, Mg 0.5-2.5%, Mn 3-8%, and pH 8-10.
The qualified liquid for mass production described in the following examples is a leachate produced by sodium roasting and water leaching of vanadium slag, and a qualified solution obtained by component detection after impurity removal.
Example 1 recovery of vanadium from vanadium-containing underflow slag Using the method of the invention
Taking 300mL of supernatant at 65 ℃, adding underflow slag according to the liquid-solid ratio of 2:1, mL/g, stirring for 65min at 90 ℃, filtering, allowing the residue to outgas, mixing the obtained vanadium solution with 500mL of large-scale production qualified liquid, and mixing according to the weight ratio of ammonium: adding ammonium sulfate into vanadium at a mass ratio of 1.5:1, adding sulfuric acid to adjust the pH value to 2.2, heating at 95 ℃ for 80min, precipitating to obtain ammonium polyvanadate, filtering, washing, drying, calcining and melting to obtain a vanadium pentoxide product, wherein the vanadium pentoxide product meets the quality requirement of 98-grade vanadium tablets, and the vanadium recovery rate in the whole process is 90%.
Example 2 recovery of vanadium from vanadium-containing underflow slag by the method of the invention
Taking 100mL of supernatant at 80 ℃, adding underflow slag according to the liquid-solid ratio of 3:1, mL/g, stirring for 70min at 80 ℃, filtering, allowing the residue to outgas, mixing the obtained vanadium solution with 200mL of large-scale production qualified liquid, and mixing according to the weight ratio of ammonium: adding ammonium sulfate into vanadium 2:1 (mass ratio), adding sulfuric acid to adjust the pH value to 2.2, heating at 90 ℃ for 90min, precipitating to obtain ammonium polyvanadate, filtering, washing, drying and calcining to obtain a vanadium pentoxide product, wherein the vanadium pentoxide product meets the quality requirement of 98-grade powder vanadium, and the vanadium recovery rate in the whole process is 92%.
Example 3 recovery of vanadium from vanadium-containing underflow slag Using the method of the invention
Taking 400mL of supernatant at 85 ℃, adding underflow slag according to a liquid-solid ratio of 3:1, mL/g, stirring for 80min at 75 ℃, filtering, allowing the residue to outgas, mixing the obtained vanadium solution with 800mL of large-scale production qualified liquid, and mixing according to the weight ratio of ammonium: adding ammonium sulfate into vanadium at a mass ratio of 3:1, adding sulfuric acid to adjust the pH value to 2.4, heating at 95 ℃ for 85min, precipitating to obtain ammonium polyvanadate, filtering, washing, drying, calcining and melting to obtain a vanadium pentoxide product, wherein the vanadium pentoxide product meets the quality requirement of 99-grade vanadium tablets, and the vanadium recovery rate in the whole process is 94.2%.
Example 4 recovery of vanadium from vanadium-containing underflow slag by the method of the present invention
Taking 200mL of supernatant at 75 ℃, adding underflow slag according to a liquid-solid ratio of 4:1, mL/g, stirring for 75min at 85 ℃, filtering, allowing the residue to outgas, mixing the obtained vanadium solution with 300mL of large-scale production qualified liquid, and mixing according to the weight ratio of ammonium: adding ammonium sulfate into vanadium 2.5:1 (mass ratio), adding sulfuric acid to adjust pH to 2.5, heating at 93 deg.C for 80min, precipitating to obtain ammonium polyvanadate, filtering, washing, drying, reacting with reducing gas to obtain vanadium trioxide satisfying 64V grade2O3The quality requirement is that the vanadium recovery rate of the whole process is 93.8 percent.
It should be appreciated that the particular features, structures, materials, or characteristics described in this specification may be combined in any suitable manner in any one or more embodiments. Furthermore, the various embodiments and features of the various embodiments described in this specification can be combined and combined by one skilled in the art without contradiction.
Claims (10)
1. The method for recovering vanadium from vanadium-containing underflow slag is characterized by comprising the following steps of: the method comprises the following steps: collecting a liquid phase of the acid vanadium precipitation of the vanadium slag, and according to a liquid-solid ratio (2-4): 1 ml/g, adding vanadium-containing underflow slag into the liquid phase, fully leaching at 70-90 ℃, carrying out solid-liquid separation, and collecting leachate to obtain a vanadium-containing solution.
2. The method of claim 1, further comprising: the liquid phase of the acid vanadium precipitation of the vanadium slag meets at least one of the following conditions:
the liquid phase of the acid vanadium precipitation of the vanadium slag contains the following chemical components: cr (chromium) component6+1.2-2.5g/L、Cr3+≤0.01g/L、V4+0.2-0.4g/L、Na+25-35g/L、NH4 +0-0.1g/L、SO4 2-80-110g/L、Cl-1-3g/L、Ca2+0.2-0.4g/L；
The solid content of the liquid phase of the acid vanadium precipitation of the vanadium slag is 120-150 g/L;
the pH value of the liquid phase of the acid vanadium precipitation of the vanadium slag is 2-3;
controlling the temperature of the liquid phase of the acid vanadium precipitation of the vanadium slag to be above 60 ℃;
preferably, the temperature of the liquid phase of the acid vanadium precipitation of the vanadium slag is controlled to be 60-85 ℃.
3. The method of claim 1, further comprising: the vanadium-containing underflow slag comprises the following chemical components in percentage by mass: v2O520～28％，Ca 10～18％，Al 3～15％，Si 5～12％，P 0.5～3.5％，Fe 3～8％，Ti2～5％，Mg 0.5～2.5％，Mn 3～8％。
4. A method as claimed in claim 1 or 3, characterized by: the pH value of the vanadium-containing underflow slag is 8-10.
5. The method of claim 1, further comprising: stirring for 60-90 min; preferably, the stirring time is 65-80 min.
6. The preparation method of the vanadium pentoxide is characterized by comprising the following steps: the method comprises the following steps: the method according to any one of claims 1 to 5, wherein vanadium is recovered from vanadium-containing underflow slag, then acid vanadium precipitation, solid-liquid separation, solid phase collection to obtain ammonium polyvanadate, and calcination is performed to obtain vanadium pentoxide.
7. The method of claim 6, wherein: at least one of the following is satisfied:
carrying out acid vanadium precipitation under the condition that the pH value is 2.0-3.0;
preferably, acid vanadium precipitation is carried out under the condition that the pH value is 2.0-2.5;
adding ammonium salt to precipitate vanadium;
preferably, the ammonium salt is at least one selected from ammonium sulfate, ammonium chloride, ammonium carbonate and ammonium bicarbonate;
preferably, the ratio of ammonium: the mass ratio of vanadium is (1.5-3): 1;
the temperature of the acid vanadium precipitation is 90-95 ℃;
the time for precipitating vanadium in the acid is 80-90 min.
8. The method of claim 6 or 7, wherein: and mixing the recovered vanadium-containing solution with the solution obtained by removing impurities from the vanadium slag leaching solution, and performing acidic vanadium precipitation together.
9. The preparation method of vanadium trioxide is characterized by comprising the following steps: the method comprises the following steps: the method according to any one of claims 6 to 8, wherein vanadium pentoxide is prepared and then reduced to obtain vanadium trioxide.
10. The method of claim 9, wherein: reacting with coal gas to reduce.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112410569A (en) * | 2020-10-30 | 2021-02-26 | 攀钢集团研究院有限公司 | Method for recovering vanadium from acidic vanadium-containing underflow slag |
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Application publication date: 20200403 |