CN105624435A - Method for selectively leaching vanadium from vanadium-contained stone coals - Google Patents
Method for selectively leaching vanadium from vanadium-contained stone coals Download PDFInfo
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- CN105624435A CN105624435A CN201610175183.XA CN201610175183A CN105624435A CN 105624435 A CN105624435 A CN 105624435A CN 201610175183 A CN201610175183 A CN 201610175183A CN 105624435 A CN105624435 A CN 105624435A
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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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- 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
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Abstract
The invention relates to a method for selectively leaching vanadium from vanadium-contained stone coals. The method comprises the following steps: firstly, a crude ore of the vanadium-contained stone coals is crushed, and is ground to obtain vanadium-contained stone coal mineral powder with particle sizes lower than 0.074 mm of 65-80 wt%; the vanadium-contained stone coal mineral powder is added in water; 0.5-1.25 kg vanadium-contained stone coal mineral powder is added in each liter of water; then, a leaching agent is added; 0.3-1 kg leaching agent is added in each liter of water; the stirring is performed by 3-7 h under the condition of 80-100 DEG C; and the solid-liquid separation is performed to obtain vanadium-contained leaching liquid and leaching slag. The leaching agent is a mixture consisting of fluorides and oxalic acid; the mass ratio of the fluorides to the oxalic acid in the leaching agent is 1: (8-15); and the fluorides are more than one of calcium fluoride, sodium fluoride, potassium fluoride, ammonia fluoride and ammonium bifluoride. The method can selectively leach vanadium from the vanadium-contained stone coals, realizes effective separation of vanadium and impurity iron, obtains the vanadium-contained leaching liquid with low iron content, and reduces the influence of iron on subsequent process.
Description
Technical field
The invention belongs to Rock coal containing alum leaching-out technique field. It is specifically related to a kind of method of Rock coal containing alum Selectively leaching vanadium.
Background technology
Rock coal containing alum usually adds leaching agent with sulfuric acid and obtains containing vanadium leachate, main leaching agent is fluorine-containing compound, in leaching process, impurity iron in Rock coal containing alum and vanadium can leach simultaneously and enter solution, and containing too high follow-up extraction or the ability of ion exchange process enrichment vanadium of reducing of concentration of iron in vanadium leachate, the follow-up purity obtaining Vanadium Pentoxide in FLAKES product can be affected simultaneously.
(the Liu great Xue such as Liu great Xue, Li Yanjiang, Chang Yaochao, Wang Yun, Yuan Chaoxin, Guo Chihao. bone coal navajoite direct sulfuric acid leaching technique expanding test [J]. mining and metallurgy, 2013,22 (4): 60-66.) adopt two sections of leachings, one section is leached as normal temperature, extraction time is 1.5h, and two sections of extraction temperatures are 90 DEG C, extraction time is 8h, maintenance vitriol oil addition be 25%, leaching agent HJZ-1?Addition be 2.5% and HJZ-2?Addition when being 2.5%, V leaching rate is stabilized in about 86%, and in leach liquor, vanadium concentration is 2.12g/L, concentration of iron is 11.32g/L, and concentration of iron is 5.3 times of vanadium concentration.
Field ancestor equality (Tian Zongping, Deng Shengwei, Cao Jian, Li Jianwen, Chen Zheng, Zhou Yongxing. the direct sulfuric acid leaching experimental study [J] of bone coal navajoite. Hunan's nonferrous metals, 2012,28 (3): 17-20.) be 165 ~ 180g/L, solid-to-liquid ratio to bone coal navajoite at sulfuric acid concentration it is 1: direct sulfuric acid leaching when (1.2 ~ 1.5), extraction time to be 6h, extraction temperature be 95 �� 5 DEG C and additive amount is 3wt%, the rate of recovery of vanadium is 78%, in leach liquor, vanadium concentration is 2.73g/L, concentration of iron is 4.22g/L, and concentration of iron is 1.5 times of vanadium concentration.
(the Yang Xiao such as Yang Xiao, Zhang Yimin, citrine, Liu Tao, Fu Lipan, Zhao Jie, Liu Juan. leaching agent CX is on the impact [J] of extracting vanadium by acid leaching of stone coal effect. metal mine, 2012, (3): 86-89.) adopt the direct acidleach of sulfuric acid to carry out detailed comparative study with the vitriol lixiviation adding leaching agent CX, result shows, the leaching yield of vanadium can be improved 18.74% by adding of leaching agent CX; CX consumption be ore quality 5%, sulfuric acid concentration be 20%, extraction temperature be 90 DEG C and under extraction time is 4h situation, in the leach liquor obtained, vanadium concentration is 1.8g/L, concentration of iron is 5.42g/L, and concentration of iron is 3 times of vanadium concentration.
(the Huang Yunsheng such as Huang Yunsheng, Wu Haiying, Dai Zilin, danger is blue or green, Li Guiying. the Separation Research [J] of vanadium and iron in the bone coal navajoite pickling liquor of Shaanxi. and mining metallurgical engineering, 2013,33 (4): 104-107.) to somewhere, Shaanxi bone coal navajoite through the leaching of 5 grades, sulfuric acid, No. 1 thickening pond supernatant liquor extraction process separation vanadium of the 6 dense washings of stage countercurrent and iron, wherein in supernatant liquor, vanadium concentration is 1.34g/L, concentration of iron is 4.12g/L, and concentration of iron is 3.1 times of vanadium concentration.
In sum, existing extracting vanadium from stone coal leaches in gained leach liquor exists the high shortcoming of iron ion content, not only have impact on the technique of follow-up enrichment vanadium, and reduces gained Vanadium Pentoxide in FLAKES product purity.
Summary of the invention
The present invention is intended to overcome prior art defect, it is intended that provide a kind of method of Rock coal containing alum Selectively leaching vanadium, the method
To the vanadium Selectively leaching in Rock coal containing alum, can realize vanadium and be separated with the effective of impurity iron, obtain iron-holder low containing vanadium leachate, iron can be reduced on the impact of subsequent technique.
For achieving the above object, the concrete steps of the technical solution used in the present invention are:
Step one, by Rock coal containing alum crushing raw ore, ore grinding to particle diameter is less than 0.074mm and accounts for 65 ~ 80wt%, obtains Rock coal containing alum ore deposit powder.
Step 2, being added to the water by described Rock coal containing alum ore deposit powder, the Rock coal containing alum ore deposit powder added in every premium on currency is 0.5 ~ 1.25kg; Adding leaching agent again, the leaching agent added in every premium on currency is 0.3 ~ 1kg; Then under 80 ~ 100 DEG C of conditions, stir 3 ~ 7h, solid-liquid separation, containing vanadium leachate and slag must be leached.
Described leaching agent is fluorochemical and the mixture of oxalic acid composition, and in leaching agent, the mass ratio of fluorochemical and oxalic acid is 1 (8 ~ 15), and described fluorochemical is more than one in Calcium Fluoride (Fluorspan), Sodium Fluoride, Potassium monofluoride, Neutral ammonium fluoride and ammonium bifluoride.
In described Rock coal containing alum raw ore, the grade of vanadium is 0.3 ~ 0.9wt%, and the grade of iron is 1.5 ~ 5.5wt%; To be the ferro element to be greater than 85% as divalence compose described iron is stored in Rock coal containing alum raw ore.
Owing to adopting technique scheme, the present invention compared with prior art has following positively effect:
1, the leaching of vanadium in Rock coal containing alum is had selectivity by the present invention, achieve vanadium to be separated with the effective of impurity iron, from the last stage of process for extracting vanadium from stone coal flow process, vanadium is separated with impurity iron, make significantly to reduce containing the impurity iron in vanadium leachate, avoid the ability decline of follow-up extraction or ion exchange process enrichment vanadium and the impact on Vanadium Pentoxide in FLAKES product purity.
2, in the present invention: the leaching yield of vanadium is 70 ~ 78%, gained is 1.2 ~ 1.7g/L containing vanadium concentration in vanadium leachate, and concentration of iron is 0.5 ~ 0.9g/L, and concentration of iron is only 0.4 ~ 0.6 times of vanadium concentration. Significantly reduce iron to the impact of subsequent technique.
Therefore, the present invention can to the vanadium Selectively leaching in Rock coal containing alum, it is achieved that vanadium is separated with the effective of impurity iron, obtain iron-holder low containing vanadium leachate, reduce iron to the impact of subsequent technique.
Embodiment
Below in conjunction with embodiment, the present invention will be further described, not to the restriction of its protection domain:
In this embodiment, described fluorochemical is more than one in Calcium Fluoride (Fluorspan), Sodium Fluoride, Potassium monofluoride, Neutral ammonium fluoride and ammonium bifluoride; Embodiment repeats no more.
Embodiment 1
A kind of method of Rock coal containing alum Selectively leaching vanadium. The concrete steps of the method are:
Step one, by Rock coal containing alum crushing raw ore, ore grinding to particle diameter is less than 0.074mm and accounts for 65 ~ 80wt%, obtains Rock coal containing alum ore deposit powder.
Step 2, being added to the water by described Rock coal containing alum ore deposit powder, the Rock coal containing alum ore deposit powder added in every premium on currency is 0.5 ~ 0.9kg; Adding leaching agent again, the leaching agent added in every premium on currency is 0.3 ~ 0.8kg; Then under 80 ~ 95 DEG C of conditions, stir 3 ~ 6h, solid-liquid separation, containing vanadium leachate and slag must be leached.
Described leaching agent is fluorochemical and the mixture of oxalic acid composition, and in leaching agent, the mass ratio of fluorochemical and oxalic acid is 1 (8 ~ 13).
In described Rock coal containing alum raw ore, the grade of vanadium is 0.3 ~ 0.7wt%, and the grade of iron is 1.5 ~ 4wt%; To be the ferro element to be greater than 85% as divalence compose described iron is stored in Rock coal containing alum raw ore.
In the present embodiment: the leaching yield of vanadium is 70 ~ 75%; In leach liquor, vanadium concentration is 1.2 ~ 1.5g/L, and concentration of iron is 0.5 ~ 0.7g/L, and concentration of iron is 0.4 ~ 0.55 times of vanadium concentration.
Embodiment 2
A kind of method of Rock coal containing alum Selectively leaching vanadium. The concrete steps of the method are:
Step one, by Rock coal containing alum crushing raw ore, ore grinding to particle diameter is less than 0.074mm and accounts for 65 ~ 80wt%, obtains Rock coal containing alum ore deposit powder.
Step 2, being added to the water by described Rock coal containing alum ore deposit powder, the Rock coal containing alum ore deposit powder added in every premium on currency is 0.85 ~ 1.25kg; Adding leaching agent again, the leaching agent added in every premium on currency is 0.5 ~ 1kg; Then under 85 ~ 100 DEG C of conditions, stir 5 ~ 7h, solid-liquid separation, containing vanadium leachate and slag must be leached.
Described leaching agent is fluorochemical and the mixture of oxalic acid composition, and in leaching agent, the mass ratio of fluorochemical and oxalic acid is 1 (10 ~ 15).
In described Rock coal containing alum raw ore, the grade of vanadium is 0.5 ~ 0.9wt%, and the grade of iron is 3 ~ 5.5wt%; To be the ferro element to be greater than 85% as divalence compose described iron is stored in Rock coal containing alum raw ore.
In the present embodiment: the leaching yield of vanadium is 72 ~ 78%; In leach liquor, vanadium concentration is 1.5 ~ 1.7g/L, and concentration of iron is 0.6 ~ 0.9g/L, and concentration of iron is vanadium concentration 0.4 ~ 0.6 times.
This embodiment compared with prior art has following positively effect:
1, the leaching of vanadium in Rock coal containing alum is had selectivity by the leaching process of this embodiment, namely realize vanadium at leaching process to be separated with the effective of impurity iron, from the last stage of process for extracting vanadium from stone coal flow process, vanadium is separated with impurity iron, avoids the ability reducing follow-up extraction or ion exchange process enrichment vanadium containing containing a large amount of impurity irons in vanadium leachate and impurity iron on the impact of Vanadium Pentoxide in FLAKES product purity.
2, in this embodiment, the leaching yield of vanadium is 70 ~ 78%, and gained is 1.2 ~ 1.7g/L and concentration of iron containing vanadium concentration in vanadium leachate is 0.5 ~ 0.9g/L, and the concentration of iron is lower relative to vanadium, and concentration of iron is only 0.4 ~ 0.6 times of vanadium concentration. Significantly reduce iron to the impact of subsequent technique.
Therefore, the present invention has and to the vanadium Selectively leaching in Rock coal containing alum, can namely realize vanadium at leaching process and be separated with the effective of impurity iron, obtain iron-holder low containing vanadium leachate, reduce the advantage that subsequent technique is affected by iron.
Claims (2)
1. the method for a Rock coal containing alum Selectively leaching vanadium, it is characterised in that described method is:
Step one, by Rock coal containing alum crushing raw ore, ore grinding to particle diameter is less than 0.074mm and accounts for 65 ~ 80wt%, obtains Rock coal containing alum ore deposit powder;
Step 2, being added to the water by described Rock coal containing alum ore deposit powder, the Rock coal containing alum ore deposit powder added in every premium on currency is 0.5 ~ 1.25kg; Adding leaching agent again, the leaching agent added in every premium on currency is 0.3 ~ 1kg; Then under 80 ~ 100 DEG C of conditions, stir 3 ~ 7h, solid-liquid separation, containing vanadium leachate and slag must be leached;
Described leaching agent is fluorochemical and the mixture of oxalic acid composition, and in leaching agent, the mass ratio of fluorochemical and oxalic acid is 1 (8 ~ 15), and described fluorochemical is more than one in Calcium Fluoride (Fluorspan), Sodium Fluoride, Potassium monofluoride, Neutral ammonium fluoride and ammonium bifluoride.
2. the method for Rock coal containing alum Selectively leaching vanadium according to claim 1, it is characterised in that in described Rock coal containing alum raw ore, the grade of vanadium is 0.3 ~ 0.9wt%, and the grade of iron is 1.5 ~ 5.5wt%; To be the ferro element to be greater than 85% as divalence compose described iron is stored in Rock coal containing alum raw ore.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109517973A (en) * | 2018-12-17 | 2019-03-26 | 武汉科技大学 | A kind of method of vanadium-containing shale biology-baking acid immersion joint Vanadium Concentrationin |
| CN116516180A (en) * | 2023-07-04 | 2023-08-01 | 北京科技大学 | Method for extracting vanadium by high-efficiency direct leaching of stone coal |
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Non-Patent Citations (1)
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109517973A (en) * | 2018-12-17 | 2019-03-26 | 武汉科技大学 | A kind of method of vanadium-containing shale biology-baking acid immersion joint Vanadium Concentrationin |
| CN109517973B (en) * | 2018-12-17 | 2020-06-09 | 武汉科技大学 | Method for enriching vanadium by combining biological roasting and acid leaching of vanadium-containing shale |
| CN116516180A (en) * | 2023-07-04 | 2023-08-01 | 北京科技大学 | Method for extracting vanadium by high-efficiency direct leaching of stone coal |
| CN116516180B (en) * | 2023-07-04 | 2023-09-22 | 北京科技大学 | Method for extracting vanadium by high-efficiency direct leaching of stone coal |
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