CN105624435B - A kind of method of Rock coal containing alum Selectively leaching vanadium - Google Patents
A kind of method of Rock coal containing alum Selectively leaching vanadium Download PDFInfo
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- CN105624435B CN105624435B CN201610175183.XA CN201610175183A CN105624435B CN 105624435 B CN105624435 B CN 105624435B CN 201610175183 A CN201610175183 A CN 201610175183A CN 105624435 B CN105624435 B CN 105624435B
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- fluoride
- vanadium
- coal containing
- rock coal
- containing alum
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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
Abstract
The present invention relates to a kind of method of Rock coal containing alum Selectively leaching vanadium.Its technical scheme is：Rock coal containing alum crushing raw ore, ore grinding to particle diameter are first accounted for into 65 ~ 80wt% less than 0.074mm, obtain Rock coal containing alum miberal powder, the Rock coal containing alum miberal powder is added to the water, the Rock coal containing alum miberal powder added in every liter of water is 0.5 ~ 1.25kg；Leaching agent is added, the leaching agent added in every liter of water is 0.3 ~ 1kg；Then 3 ~ 7h is stirred under the conditions of 80 ~ 100 DEG C, separation of solid and liquid, is obtained containing vanadium leachate and leached mud.The leaching agent is the mixture that fluoride and oxalic acid form, and the mass ratio of fluoride and oxalic acid be 1 ︰ (8 ~ 15) in leaching agent, and the fluoride is one or more of calcirm-fluoride, sodium fluoride, potassium fluoride, ammonium fluoride and ammonium acid fluoride.The present invention can realize efficiently separating for vanadium and impurity iron to the vanadium Selectively leaching in Rock coal containing alum, obtained iron-holder it is low contain vanadium leachate, reduce influence of the iron to subsequent technique.
Description
Technical field
The invention belongs to Rock coal containing alum leaching-out technique field.More particularly to a kind of side of Rock coal containing alum Selectively leaching vanadium
Method.
Background technology
Rock coal containing alum generally adds leaching agent to obtain containing vanadium leachate with sulfuric acid, and main leaching agent is fluorine-containing compound,
In leaching process, the impurity iron in Rock coal containing alum can be leached into solution simultaneously with vanadium, and containing concentration of iron mistake in vanadium leachate
Height can reduce the ability of follow-up extraction or ion-exchange process Vanadium Concentrationin, while can influence subsequently to obtain vanadic anhydride product
Purity.
(Liu great Xue, Li Yanjiang, Chang Yaochao, Wang Yun, Yuan Chaoxin, Guo hold the white direct sulfuric acid leaching of bone coal navajoites to Liu great Xue etc.
Technique expanding test [J] mining and metallurgys, 2013,22 (4)：60-66.) using two sections of leachings, one section of leaching is normal temperature, and extraction time is
1.5h, two sections of extraction temperatures are 90 DEG C, extraction time 8h, are 25%, leaching agent HJZ-1 keeping concentrated sulfuric acid addition﹟Add
Dosage is 2.5% and HJZ-2﹟Addition when being 2.5%, the stable vanadium concentration in 86% or so, leachate of V leaching rate is
2.12g/L, concentration of iron 11.32g/L, concentration of iron are 5.3 times of vanadium concentration.
Field ancestor's equality (Tian Zongping, Deng Shengwei, Cao Jian, Li Jianwen, Chen Zheng, the direct sulfuric acid leaching examination of Zhou Yongxing bone coal navajoites
Test research [J] Hunan's nonferrous metals, 2012,28 (3)：It is 17-20.) 165 ~ 180g/L, admittedly in sulfuric acid concentration to bone coal navajoite
Liquor ratio is 1: (1.2 ~ 1.5), extraction time 6h, extraction temperature are 95 ± 5 DEG C and additive amount is direct under the conditions of 3wt%
Sulfuric acid leaching, the rate of recovery of vanadium are 78%, in leachate vanadium concentration be 2.73g/L, concentration of iron 4.22g/L, concentration of iron is that vanadium is dense
1.5 times of degree.
(Yang Xiao, Zhang Yimin, citrine, Liu Tao, Fu Lipan, Zhao Jie, Liu Juan leaching agents CX is to extracting vanadium by acid leaching of stone coal by Yang Xiao etc.
Influence [J] metal mines of effect, 2012, (3)：86-89.) using the direct acidleach of sulfuric acid and the sulfuric acid acid for adding leaching agent CX
It is impregnated into and has gone detailed comparative study, the results showed that, the leaching rate of vanadium can be improved 18.74% by adding for leaching agent CX；Used in CX
Measure 5% for ore quality, sulfuric acid concentration 20%, in the case of extraction temperature is 90 DEG C and extraction time is 4h, obtained leaching
In liquid vanadium concentration be 1.8g/L, concentration of iron 5.42g/L, concentration of iron is 3 times of vanadium concentration.
Huang Yunsheng etc. (Huang Yunsheng, Wu Haiying, Dai Zilin, danger is blue or green, in the bone coal navajoite pickle liquor of Li Guiying Shaanxi vanadium with
Separation Research [J] mining metallurgical engineerings of iron, 2013,33 (4)：104-107.) Shaanxi somewhere bone coal navajoite is leached for 5 grades through sulfuric acid,
No. 1 thickening pond supernatant of the dense washing of 6 stage countercurrents separates vanadium and iron with extraction, and vanadium concentration is 1.34g/ wherein in supernatant
L, concentration of iron is 4.12g/L, and concentration of iron is 3.1 times of vanadium concentration.
In summary, existing extracting vanadium from stone coal, which is leached in gained leachate, has the shortcomings that iron ion content is high, not only influences
The technique of follow-up Vanadium Concentrationin, and reduce gained vanadic anhydride product purity.
The content of the invention
It is contemplated that overcome prior art defect, it is therefore an objective to a kind of method of Rock coal containing alum Selectively leaching vanadium is provided,
This method
Vanadium Selectively leaching in Rock coal containing alum can be realized efficiently separating for vanadium and impurity iron, it is low to obtain iron-holder
Contain vanadium leachate, influence of the iron to subsequent technique can be reduced.
To achieve the above object, the technical solution adopted by the present invention comprises the concrete steps that：
Step 1: by Rock coal containing alum crushing raw ore, ore grinding to particle diameter accounts for 65 ~ 80wt% less than 0.074mm, obtains containing scherbinaite
Colliery powder.
Step 2: the Rock coal containing alum miberal powder is added to the water, the Rock coal containing alum miberal powder added in every liter of water is 0.5 ~
1.25kg；Leaching agent is added, the leaching agent added in every liter of water is 0.3 ~ 1kg；Then under the conditions of 80 ~ 100 DEG C stirring 3 ~
7h, separation of solid and liquid, obtain containing vanadium leachate and leached mud.
The leaching agent is the mixture that fluoride and oxalic acid form, and the mass ratio of fluoride and oxalic acid is 1 ︰ in leaching agent
(8 ~ 15), the fluoride are one or more of calcirm-fluoride, sodium fluoride, potassium fluoride, ammonium fluoride and ammonium acid fluoride.
The grade of vanadium is 0.3 ~ 0.9wt% in the Rock coal containing alum raw ore, and the grade of iron is 1.5 ~ 5.5wt%；The iron is
It is divalence preservation in Rock coal containing alum raw ore using the ferro element more than 85%.
Due to being had the positive effect that compared with prior art using above-mentioned technical proposal, the present invention：
1st, leaching of the present invention to vanadium in Rock coal containing alum has selectivity, realizes efficiently separating for vanadium and impurity iron, from
The last stage of process for extracting vanadium from stone coal flow separates vanadium with impurity iron, makes to significantly reduce containing the impurity iron in vanadium leachate, avoids
The ability of follow-up extraction or ion-exchange process Vanadium Concentrationin declines and influence to vanadic anhydride product purity.
2nd, in the present invention：The leaching rate of vanadium is 70 ~ 78%, and it is 1.2 ~ 1.7g/L that gained, which contains vanadium concentration in vanadium leachate, and iron is dense
It is only 0.4 ~ 0.6 times of vanadium concentration to spend for 0.5 ~ 0.9g/L, concentration of iron.Significantly reduce influence of the iron to subsequent technique.
Therefore, the present invention can realize efficiently separating for vanadium and impurity iron, obtain to the vanadium Selectively leaching in Rock coal containing alum
Arrived iron-holder it is low contain vanadium leachate, reduce influence of the iron to subsequent technique.
Embodiment
With reference to embodiment, the present invention will be further described, not to the limitation of its protection domain：
In present embodiment, the fluoride is in calcirm-fluoride, sodium fluoride, potassium fluoride, ammonium fluoride and ammonium acid fluoride
More than one；Repeated no more in embodiment.
Embodiment 1
A kind of method of Rock coal containing alum Selectively leaching vanadium.This method comprises the concrete steps that：
Step 1: by Rock coal containing alum crushing raw ore, ore grinding to particle diameter accounts for 65 ~ 80wt% less than 0.074mm, obtains containing scherbinaite
Colliery powder.
Step 2: the Rock coal containing alum miberal powder is added to the water, the Rock coal containing alum miberal powder added in every liter of water is 0.5 ~
0.9kg；Leaching agent is added, the leaching agent added in every liter of water is 0.3 ~ 0.8kg；Then under the conditions of 80 ~ 95 DEG C stirring 3 ~
6h, separation of solid and liquid, obtain containing vanadium leachate and leached mud.
The leaching agent is the mixture that fluoride and oxalic acid form, and the mass ratio of fluoride and oxalic acid is 1 ︰ in leaching agent
(8~13)。
The grade of vanadium is 0.3 ~ 0.7wt% in the Rock coal containing alum raw ore, and the grade of iron is 1.5 ~ 4wt%；The iron be with
Ferro element more than 85% is divalence preservation in Rock coal containing alum raw ore.
In the present embodiment：The leaching rate of vanadium is 70 ~ 75%；Vanadium concentration is 1.2 ~ 1.5g/L in leachate, concentration of iron is 0.5 ~
0.7g/L, concentration of iron are 0.4 ~ 0.55 times of vanadium concentration.
Embodiment 2
A kind of method of Rock coal containing alum Selectively leaching vanadium.This method comprises the concrete steps that：
Step 1: by Rock coal containing alum crushing raw ore, ore grinding to particle diameter accounts for 65 ~ 80wt% less than 0.074mm, obtains containing scherbinaite
Colliery powder.
Step 2: the Rock coal containing alum miberal powder is added to the water, the Rock coal containing alum miberal powder added in every liter of water is 0.85 ~
1.25kg；Leaching agent is added, the leaching agent added in every liter of water is 0.5 ~ 1kg；Then under the conditions of 85 ~ 100 DEG C stirring 5 ~
7h, separation of solid and liquid, obtain containing vanadium leachate and leached mud.
The leaching agent is the mixture that fluoride and oxalic acid form, and the mass ratio of fluoride and oxalic acid is 1 ︰ in leaching agent
(10~15)。
The grade of vanadium is 0.5 ~ 0.9wt% in the Rock coal containing alum raw ore, and the grade of iron is 3 ~ 5.5wt%；The iron be with
Ferro element more than 85% is divalence preservation in Rock coal containing alum raw ore.
In the present embodiment：The leaching rate of vanadium is 72 ~ 78%；Vanadium concentration is 1.5 ~ 1.7g/L in leachate, concentration of iron is 0.6 ~
0.9g/L, concentration of iron are 0.4 ~ 0.6 times of vanadium concentration.
Present embodiment has the positive effect that compared with prior art：
1st, leaching of the leaching process of present embodiment to vanadium in Rock coal containing alum has selectivity, is in leaching process
Efficiently separating for vanadium and impurity iron is realized, vanadium is separated with impurity iron from the last stage of process for extracting vanadium from stone coal flow, avoids containing vanadium
The ability and impurity iron of follow-up extraction or ion-exchange process Vanadium Concentrationin are reduced to five oxygen containing substantial amounts of impurity iron in leachate
Change the influence of two vanadium product purities.
2nd, in present embodiment vanadium leaching rate be 70 ~ 78%, gained contain vanadium leachate in vanadium concentration be 1.2 ~
1.7g/L and concentration of iron are 0.5 ~ 0.9g/L, and the concentration of iron is relatively low with respect to vanadium, and concentration of iron is only 0.4 ~ 0.6 times of vanadium concentration.It is aobvious
Work reduces influence of the iron to subsequent technique.
Therefore, the present invention, which has, to realize vanadium and impurity in leaching process to the vanadium Selectively leaching in Rock coal containing alum
Iron efficiently separates, obtain iron-holder it is low contain vanadium leachate, reduce the advantages of iron influences on subsequent technique.
Claims (1)
- A kind of 1. method of Rock coal containing alum Selectively leaching vanadium, it is characterised in that methods described is：Step 1: by Rock coal containing alum crushing raw ore, ore grinding to particle diameter accounts for 65~80wt% less than 0.074mm, obtains Rock coal containing alum Miberal powder；Step 2: the Rock coal containing alum miberal powder is added to the water, the Rock coal containing alum miberal powder added in every liter of water is 0.5~ 1.25kg；Leaching agent is added, the leaching agent added in every liter of water is 0.3~1kg；Then 3 are stirred under the conditions of 80~100 DEG C ~7h, separation of solid and liquid, is obtained containing vanadium leachate and leached mud；The leaching agent is the mixture that fluoride and oxalic acid form, in leaching agent the mass ratio of fluoride and oxalic acid be 1 ︰ (8~ 15), the fluoride is one or more of calcirm-fluoride, sodium fluoride, potassium fluoride, ammonium fluoride and ammonium acid fluoride；The grade of vanadium is 0.3~0.9wt% in the Rock coal containing alum raw ore, and the grade of iron is 1.5~5.5wt%；The iron is It is divalence preservation in Rock coal containing alum raw ore using the ferro element more than 85%.
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| CN201610175183.XA CN105624435B (en) | 2016-03-25 | 2016-03-25 | A kind of method of Rock coal containing alum Selectively leaching vanadium |
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| 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 |
| 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 |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103421964A (en) * | 2013-08-26 | 2013-12-04 | 武汉科技大学 | Method for leaching vanadium from stone coal containing vanadium |
| CN104099484A (en) * | 2014-07-31 | 2014-10-15 | 武汉科技大学 | Method for extracting vanadium by roasting vanadium-containing stone coal in size fraction grading and fluidization manner |
| CN104138806A (en) * | 2014-06-10 | 2014-11-12 | 中南大学 | Method for extracting V2O5 and carbon from low-carbon stone coal mine |
| CN104532017A (en) * | 2014-12-22 | 2015-04-22 | 武汉科技大学 | Method for leaching and extracting vanadium from vanadium-containing stone coal |
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- 2016-03-25 CN CN201610175183.XA patent/CN105624435B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103421964A (en) * | 2013-08-26 | 2013-12-04 | 武汉科技大学 | Method for leaching vanadium from stone coal containing vanadium |
| CN104138806A (en) * | 2014-06-10 | 2014-11-12 | 中南大学 | Method for extracting V2O5 and carbon from low-carbon stone coal mine |
| CN104099484A (en) * | 2014-07-31 | 2014-10-15 | 武汉科技大学 | Method for extracting vanadium by roasting vanadium-containing stone coal in size fraction grading and fluidization manner |
| CN104532017A (en) * | 2014-12-22 | 2015-04-22 | 武汉科技大学 | Method for leaching and extracting vanadium from vanadium-containing stone coal |
Non-Patent Citations (1)
| Title |
|---|
| 国内提钒尾渣再提钒技术研究进展;孟利鹏;《钢铁钒钛》;20150630;第49-56页 * |
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