CN109868365B - Method for deeply extracting vanadium from vanadium-containing raw material - Google Patents
Method for deeply extracting vanadium from vanadium-containing raw material Download PDFInfo
- Publication number
- CN109868365B CN109868365B CN201910221221.4A CN201910221221A CN109868365B CN 109868365 B CN109868365 B CN 109868365B CN 201910221221 A CN201910221221 A CN 201910221221A CN 109868365 B CN109868365 B CN 109868365B
- Authority
- CN
- China
- Prior art keywords
- vanadium
- phosphate
- solution
- containing raw
- leaching
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Classifications
-
- 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
Landscapes
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention relates to a method for deeply extracting vanadium from a vanadium-containing raw material, belonging to the technical field of vanadium metallurgy. The invention solves the technical problems of large vanadium loss and complex process flow of the existing vanadium extraction process. The invention discloses a method for deeply extracting vanadium from a vanadium-containing raw material, which comprises the steps of A, mixing the vanadium-containing material, phosphate and sulfuric acid, controlling the pH value of the mixed slurry to be 0.5-1.5, carrying out acid leaching, and carrying out solid-liquid separation to obtain a leaching solution; B. adjusting the pH value of the leachate to 3.0-4.2, and performing solid-liquid separation to obtain phosphate slag and a dephosphorizing solution; C. and (4) returning the phosphate slag to the step A for recycling, and using the dephosphorizing solution for preparing vanadium oxide. The method for deeply extracting vanadium by one-time acid leaching of the vanadium-containing material shortens the vanadium extraction process flow, reduces the production cost and has the advantage of simple operation.
Description
Technical Field
The invention belongs to the technical field of vanadium metallurgy, and particularly relates to a method for deeply extracting vanadium from a vanadium-containing raw material.
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.
Disclosure of Invention
The invention solves the technical problems of large vanadium loss and complex process flow of the existing vanadium extraction process.
The technical scheme for solving the problems is to provide a method for deeply extracting vanadium from a vanadium-containing raw material, which comprises the following steps:
A. mixing vanadium-containing materials, phosphate and sulfuric acid, carrying out acid leaching, and carrying out solid-liquid separation to obtain a leaching solution;
B. regulating the pH value of the leachate for dephosphorization, and performing solid-liquid separation to obtain phosphate slag and a dephosphorization solution;
C. and (4) returning the phosphate slag to the step A to be used as an acid leaching material for recycling, and using the dephosphorizing solution to prepare vanadium oxide.
Wherein, the vanadium-containing material in the step A is V5+The vanadium-containing raw material with the mass content of more than 1 percent.
Wherein the phosphate is at least one of aluminum phosphate and iron phosphate.
And B, controlling the pH value of the mixed slurry to be 0.5-1.5 in the acid leaching process in the step A.
Wherein, the concentration of phosphorus in the leaching solution is controlled to be 0.3-3 g/L V in the step A5+The concentration is 10-30 g/L.
And B, adjusting the pH value of the leaching solution to 3.0-4.2.
And B, adjusting the pH of the leachate by using at least one reagent selected from ammonia water, ammonium carbonate, ammonium bicarbonate, magnesium oxide, magnesium hydroxide, magnesium carbonate, calcium oxide, calcium hydroxide and calcium carbonate.
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; the method firstly carries out acid leaching at a lower pH level, can fully leach vanadium in the vanadium-containing raw material, and then removes phosphorus in the leachate by adjusting the pH value, thereby achieving the purpose of deep vanadium extraction; the method for deeply extracting vanadium by one-time acid leaching of the vanadium-containing material shortens the vanadium extraction process flow, reduces the production cost and has the advantage of simple operation.
Detailed Description
The invention provides a method for deeply extracting vanadium from a vanadium-containing raw material, which specifically comprises the following steps:
A. mixing vanadium-containing materials, phosphate and sulfuric acid, controlling the pH value of the mixed slurry to be 0.5-1.5, carrying out acid leaching, and carrying out solid-liquid separation to obtain a leaching solution;
B. regulating the pH value of the leachate to 3.0-4.2 for dephosphorization, and performing solid-liquid separation to obtain phosphate slag and a dephosphorization solution;
C. and (4) returning the aluminum phosphate slag to the step A to be used as an acid leaching material for recycling, and using the dephosphorizing solution to prepare vanadium oxide.
Wherein, the vanadium-containing material in the step A 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。
Firstly, the pH value of the mixed slurry containing the vanadium-containing material is controlled to be 0.5-1.5 so as to fully dissolve vanadium in the vanadium-containing material into the leachate, and meanwhile, phosphate is added in the acid leaching process so as to improve the phosphorus concentration in the mixed slurry and the leachate, so that vanadium and phosphorus form a vanadium-phosphorus heteropoly acid complex, and the vanadium loss caused by vanadium hydrolysis precipitation is avoided.
Wherein the phosphate is at least one of aluminum phosphate and iron phosphate.
And then, adjusting the pH value of the leachate obtained in the step A to be 3.0-4.2, so that phosphorus, aluminum and iron in the leachate form aluminum phosphate and/or iron phosphate precipitates and enter phosphate slag, thereby achieving the purpose of separating phosphorus.
Wherein, the concentration of phosphorus in the leaching solution is controlled to be 0.3-3 g/L V in the step A5+The concentration is 10-30 g/L.
And B, adjusting the pH of the leachate by using at least one reagent selected from ammonia water, ammonium carbonate, ammonium bicarbonate, magnesium oxide, magnesium hydroxide, magnesium carbonate, calcium oxide, calcium hydroxide and calcium carbonate.
The invention is further illustrated and described by the following examples.
Example 1
Taking roasted vanadium-containing material (V)2O517.85%, P0.04%) 100g, 2.98g of aluminum phosphate, was added to 350m L 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 60min, 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 of 27.46 g/L and the P concentration of 2.55 g/L, the pH value of the leaching solution is adjusted to 3.8 by calcium oxide, the P concentration of the solution obtained by solid-liquid separation is 0.05 g/L, and the solution can be used for preparing vanadium oxide.
Example 2
Taking roasted vanadium-containing material (V)2O517.85%, P0.04%) 100g, was added to 450m L tap water together with 2.67g of aluminum phosphate, 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 of the P is 21.26 g/L, the concentration of the P is 1.72 g/L, the pH value of the leaching solution is adjusted to be 4.0 by magnesium oxide, the concentration of the P of the solution obtained by solid-liquid separation is 0.05 g/L, and the solution can be used for preparing vanadium oxide.
Example 3
Taking roasted vanadium-containing material (V)2O54.43% and P0.04%) in 250m L tap water, adding 0.58g of aluminum phosphate into the mixture, adjusting the pH of the slurry to 1.3 to 1.5 with sulfuric acid at normal temperature, stirring the mixture to react for 30min, performing solid-liquid separation, and obtaining V in the acid leaching residue2O5The content is 1.07 percent, and the vanadium leaching rate is 75.82 percent; leachate V5+The concentration of the P is 13.43 g/L, the concentration of the P is 0.68 g/L, the pH of the leaching solution is adjusted to be 4.2 by ammonium bicarbonate, and the concentration of the P of the solution obtained by solid-liquid separation is 0.04 g/L, so that the vanadium oxide can be prepared.
Example 4
Taking roasted vanadium-containing material (V)2O54.43% and P0.04%), 0.72g, and 0.72g of iron phosphate were added to 250m L 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 83.88 percent; leachate V5+The concentration of the P is 14.86 g/L, the concentration of the P is 0.68 g/L, the pH value of the leaching solution is adjusted to 3.2 by ammonium bicarbonate, and the concentration of the P of the solution obtained by solid-liquid separation is 0.04 g/L, so that the vanadium oxide can be prepared.
Claims (4)
1. The method for deeply extracting vanadium from a vanadium-containing raw material is characterized by comprising the following steps of:
A. mixing vanadium-containing materials, phosphate and sulfuric acid, carrying out acid leaching, and carrying out solid-liquid separation to obtain a leaching solution, wherein the pH of a mixed slurry is controlled to be 0.5-1.5 in the acid leaching process, the phosphorus concentration in the leaching solution is 0.3-3 g/L, and V is5+The concentration is 10-30 g/L;
B. regulating the pH value of the leachate to 3.0-4.2 for dephosphorization, and performing solid-liquid separation to obtain phosphate slag and a dephosphorization solution;
C. and (4) returning the phosphate slag to the step A to be used as an acid leaching material for recycling, and using the dephosphorizing solution to prepare vanadium oxide.
2. The method for deeply extracting vanadium from vanadium-containing raw materials according to claim 1, is characterized in that: the vanadium-containing material in the step A is V5+The vanadium-containing raw material with the mass content of more than 1 percent.
3. The method for deeply extracting vanadium from vanadium-containing raw materials according to claim 1 or 2, characterized by comprising the following steps: in the step A, the phosphate is at least one of aluminum phosphate and iron phosphate.
4. The method for deeply extracting vanadium from vanadium-containing raw materials according to claim 1, is characterized in that: and B, adjusting the pH of the leachate by using at least one of ammonia water, ammonium carbonate, ammonium bicarbonate, magnesium oxide, magnesium hydroxide, magnesium carbonate, calcium oxide, calcium hydroxide and calcium carbonate as a reagent.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910221221.4A CN109868365B (en) | 2019-03-22 | 2019-03-22 | Method for deeply extracting vanadium from vanadium-containing raw material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910221221.4A CN109868365B (en) | 2019-03-22 | 2019-03-22 | Method for deeply extracting vanadium from vanadium-containing raw material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN109868365A CN109868365A (en) | 2019-06-11 |
| CN109868365B true CN109868365B (en) | 2020-07-28 |
Family
ID=66921072
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910221221.4A Active CN109868365B (en) | 2019-03-22 | 2019-03-22 | Method for deeply extracting vanadium from vanadium-containing raw material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109868365B (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112795787A (en) * | 2020-11-19 | 2021-05-14 | 重庆第二师范学院 | Method for extracting vanadium and dephosphorizing phosphorus-containing vanadium slag |
| CN114214514B (en) * | 2021-11-12 | 2024-04-30 | 攀钢集团研究院有限公司 | Method for leaching and removing phosphorus in high-phosphorus calcified roasting vanadium-containing clinker and recycling leaching liquid |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8657917B2 (en) * | 2011-05-06 | 2014-02-25 | Hong Jing Metal Corporation | Method for recycling metals from waste molybdic catalysts |
| CN104480308A (en) * | 2015-01-02 | 2015-04-01 | 重庆大学 | Dephosphorizing method for acid vanadium leached solution |
| CN105714102A (en) * | 2016-03-03 | 2016-06-29 | 中国科学院过程工程研究所 | Method for extracting vanadium by leaching vanadium-contained raw material roasting clinkers through ammonium phosphate |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103667710B (en) * | 2013-12-04 | 2015-06-17 | 四川省川威集团有限公司 | Technology for clean production of vanadium pentoxide employing high-calcium vanadium slag |
| CN108359797A (en) * | 2018-04-11 | 2018-08-03 | 武汉科技大学 | A method of the selectively removing impurity P from vanadium solution obtained by vanadium slag calcification acidleach |
| CN109182752A (en) * | 2018-10-23 | 2019-01-11 | 攀钢集团研究院有限公司 | The method that desilication slag removes phosphorus in acid vanadium liquid |
| CN109207740B (en) * | 2018-11-30 | 2020-12-01 | 攀钢集团研究院有限公司 | Vanadium extraction method of high-calcium high-phosphorus vanadium slag |
-
2019
- 2019-03-22 CN CN201910221221.4A patent/CN109868365B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8657917B2 (en) * | 2011-05-06 | 2014-02-25 | Hong Jing Metal Corporation | Method for recycling metals from waste molybdic catalysts |
| CN104480308A (en) * | 2015-01-02 | 2015-04-01 | 重庆大学 | Dephosphorizing method for acid vanadium leached solution |
| CN105714102A (en) * | 2016-03-03 | 2016-06-29 | 中国科学院过程工程研究所 | Method for extracting vanadium by leaching vanadium-contained raw material roasting clinkers through ammonium phosphate |
Also Published As
| Publication number | Publication date |
|---|---|
| CN109868365A (en) | 2019-06-11 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| RU2743355C1 (en) | Method of extracting vanadium from vanadium slag with high content of calcium and phosphorus | |
| CN109338099B (en) | Calcified roasting vanadium extracting material and vanadium extracting method thereof | |
| CN101182037B (en) | Method for reclaiming vanadium oxide from dephosphorization underflow slag | |
| CN104071835B (en) | A kind of preparation method of titanium dioxide | |
| CN109868365B (en) | Method for deeply extracting vanadium from vanadium-containing raw material | |
| CN110512095B (en) | Method for extracting and stabilizing arsenic from tungsten metallurgy phosphorus arsenic slag | |
| CN109913660A (en) | A method of rich vanadium richness iron charge is prepared using v-bearing steel slag | |
| CN110358920B (en) | Method for separating vanadium from vanadium-chromium waste residue | |
| CN104357652A (en) | Method for directly extracting vanadium from high-calcium vanadium slag by roasting-alkali leaching | |
| CN112111661B (en) | Method for extracting vanadium by calcium-manganese composite roasting of vanadium slag | |
| CN110643838A (en) | Method for roasting vanadium slag by adopting calcium sulfate | |
| CN102312090A (en) | Process for extracting scandium from ore containing scandium through pressure leaching | |
| CN106011469B (en) | The method of the continuous precipitation of high vanadium concentrations solution | |
| CN103045868A (en) | Method for extracting vanadium from extracted vanadium tailings | |
| CN112011693A (en) | Method for preparing vanadium-chromium alloy by roasting, acid leaching and vanadium extracting of vanadium-chromium slag | |
| CN1936037A (en) | Method for oxidizing-converting-leaching vanadium from converter steelmaking extracted vanadium slag under pressure field | |
| CN111100996B (en) | Method for preparing vanadium oxide from acidic low-concentration vanadium liquid | |
| CN107937737B (en) | A method of reducing chromium content in high chromium calcium vanadate | |
| CN104609472B (en) | A kind of titanium tetrachloride refines the method except vanadium mud produces vanadic anhydride | |
| CN109943734B (en) | Method for improving stability of pentavalent vanadium leaching solution | |
| CN102534267A (en) | Vanadium extracting method | |
| CN109930008B (en) | Method for cleanly extracting vanadium from vanadium slag | |
| CN104894374B (en) | A kind of method of acidity dephosphorization containing vanadium solution | |
| CN112899483B (en) | Method for selectively extracting and separating vanadium from vanadium-molybdenum waste residues | |
| CN109811123B (en) | Method for extracting vanadium by calcium-magnesium composite reinforcement |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20220624 Address after: 610306 Chengdu City, Chengdu, Sichuan, China (Sichuan) free trade test zone, Chengdu City, Qingbaijiang District, xiangdao Boulevard, Chengxiang Town, No. 1509 (room 13, A District, railway port mansion), room 1319 Patentee after: Chengdu advanced metal material industry technology Research Institute Co.,Ltd. Patentee after: Panzhihua Iron and Steel Group Panzhihua iron and Steel 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. |
|
| TR01 | Transfer of patent right |