CN109022783A - The method of the vanadium manganese of immersion liquid containing vanadic acid separation - Google Patents
The method of the vanadium manganese of immersion liquid containing vanadic acid separation Download PDFInfo
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- CN109022783A CN109022783A CN201811152151.3A CN201811152151A CN109022783A CN 109022783 A CN109022783 A CN 109022783A CN 201811152151 A CN201811152151 A CN 201811152151A CN 109022783 A CN109022783 A CN 109022783A
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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
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/44—Treatment or purification of solutions, e.g. obtained by leaching by chemical processes
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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
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- 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 belongs to non-ferrous metal separation and recovery technology fields, and in particular to the method for the vanadium manganese of immersion liquid containing vanadic acid separation.Present invention solves the technical problem that being that the existing demanganization process of immersion liquid containing vanadic acid is complicated, at high cost, manganese cannot be recycled well.The present invention provides the method for the manganese of vanadium containing vanadium leachate separation, includes the following steps: that the demanganization agent of oxalic acid class is added in vanadium slag pickle liquor, and the acidity of adjusting vanadium slag pickle liquor hydrogen ion concentration into solution is 10‑5Mol/L~3.16 × 10‑2Mol/L carries out demanganization, and demanganization after-purification liquid and filter cake are separated by solid-liquid separation to obtain after demanganization, and demanganization after-purification liquid is used for subsequent precipitation technique, obtains manganese oxalate byproduct after filter cake drying.Present invention process process is simple, can efficiently separate the manganese in vanadium slag pickle liquor with vanadium, and obtain manganese oxalate byproduct.
Description
Technical field
The invention belongs to non-ferrous metal separation and recovery technology fields, and in particular to the method for the vanadium manganese of immersion liquid containing vanadic acid separation.
Background technique
Vanadium has many excellent physicochemical properties and mechanical property, is widely used in modern industry.As China is existing
The high speed development of generationization construction, the demand of V and its compounds is increasing, and wants to high-purity V and its compounds
Ask higher and higher.There are about 80% vanadium to come from Leaching of Vanadium from Vanadium slag in the whole world, and the production technology of scale has sodium roasting water at present
Leaching and vanadium extraction technique and two kinds of calcification baking process for extracting vanadium by acid leaching.
Due to usually containing manganese in vanadium slag, when using process for extracting vanadium by acid leaching, manganese can enter leachate by sulfuric acid dissolution,
To influence subsequent precipitation effect and vanadium product quality.Usual processing mode for such high manganese immersion liquid containing vanadic acid is directly to adopt
With hydrolysis precipitation or ammonium salt precipitation, hydration vanadic anhydride (vanadic acid) or poly ammonium vanadate and extraction raffinate containing manganese are obtained, then from containing
Manganese is recycled in manganese extraction raffinate.Due to not preparatory demanganization, impurity manganese content is high in final products obtained therefrom, vanadic anhydride product purity
The low market competitiveness is poor.Therefore want to obtain the vanadic anhydride of high-quality, vanadium slag pickle liquor must be carried out before precipitation
Impurity and purification processing.Conventional demanganization method has chemical precipitation method, absorption method, ion-exchange and extraction.According to chemistry
Precipitation method demanganization then needs to adjust pH value to the Mn in 8~12 removal vanadium leachates, adds acid for adjusting pH to 1.5~2.5 again after removal of impurities
Precipitation, acid and alkali consumption amount is big, while the hydrous oxide precipitation adsorption vanadium that impurity is formed in purification process, and a large amount of vanadium is caused to damage
It loses.Ion exchange is only suitable for using on a small scale, and the Mn of solution middle and high concentration cannot be efficiently separated；Absorption method is also only to low
Concentration Mn removal is effective；Solvent extraction sulfonation and stripping section before extraction consume a large amount of high concentrated acid solution, and containing having on a small quantity
The strip liquor of machine phase cannot recycle, and form new pollution sources.In addition to this, ion exchange and solvent extraction purification contain vanadium
Solution complex procedures, it is at high cost.
Summary of the invention
Present invention solves the technical problem that being that the existing demanganization process of immersion liquid containing vanadic acid is complicated, at high cost, manganese cannot obtain
It recycles well.
Technical proposal that the invention solves the above-mentioned problems is to provide the method for the manganese of vanadium containing vanadium leachate separation, including walks as follows
It is rapid: demanganization agent to be added in vanadium slag pickle liquor, the acidity of adjusting vanadium slag pickle liquor hydrogen ion concentration into solution is 10-5Mol/L~
3.16×10-2Mol/L carries out demanganization, and demanganization after-purification liquid and filter cake are separated by solid-liquid separation to obtain after demanganization, and the demanganization agent is grass
At least one of acid or oxalates.
Wherein, oxalates is at least one of sodium oxalate, potassium oxalate, sodium bioxalate and potassium binoxalate.
Wherein, the additional amount of demanganization agent is 1.2~1.5 times of manganese content in vanadium slag pickle liquor with molar amount.
Wherein, vanadium slag pickle liquor is obtained after sulfuric acid leaching by the vanadium slag clinker after calcification baking.
Wherein, the acidity of the vanadium slag pickle liquor is adjusted using sulfuric acid or ammonium hydroxide.
Wherein, demanganization stands at least 30min after reacting 30~100min at 40~90 DEG C.
Wherein, vanadium concentration is 5~50g/L in vanadium slag pickle liquor, and manganese concentration is 2~30g/L.
Wherein, demanganization after-purification liquid is used for subsequent precipitation technique, obtains manganese oxalate byproduct after filter cake drying.
Wherein, MnC in manganese oxalate2O4Content is between 95.23%~97.12%.
Wherein, Mn concentration is reduced to < 0.05g/L in demanganization after-purification liquid.
Beneficial effects of the present invention:
The present invention can be efficiently separated the manganese in vanadium slag pickle liquor with vanadium by the way that demanganization agent is added, vanadium slag pickle liquor
The removal rate of middle manganese is 90~99%, while vanadium loss late is lower than 2% during demanganization；Present invention demanganization before precipitation reduces
The V that purity is greater than 99% can be obtained subsequently through conventional precipitation technique in adverse effect of the manganese to subsequent precipitation2O5Product；This hair
It is bright to obtain manganese oxalate byproduct, MnC in manganese oxalate while separating manganese and vanadium2O4Content between 95.23%~97.12%,
It can be sold directly as product；The present invention has process flow simple, the low advantage of manganese cost recovery.
Specific embodiment
The present invention provides the method for the vanadium manganese of immersion liquid containing vanadic acid separation, and steps are as follows: demanganization agent being added in vanadium slag pickle liquor, adjusts
The acidity of section vanadium slag pickle liquor hydrogen ion concentration into solution is 10-5Mol/L~3.16 × 10-2Mol/L carries out demanganization, demanganization
After be separated by solid-liquid separation to obtain demanganization after-purification liquid and filter cake, the demanganization agent is at least one of oxalic acid or oxalates.
In acid condition, manganese generates manganese oxalate precipitating easily in conjunction with solution oxalate, and vanadium is with vanadium acid anion
Form exist in solution, to reach the separation of manganese and vanadium.The chemical reaction being related to during demanganization is as follows:
V2O5+H+→VO2 +
MnO+H+→Mn2+
Mn2++C2O4 2-→MnC2O4↓
Suitable hydrogen ion concentration is to realize one of essential condition of the invention, when hydrogen ion concentration is too low in leachate
Vanadium, iron facile hydrolysis generate precipitating, not only cause the vanadium in leachate to lose, while the precipitating of iron also easily makes oxalic acid manganese product pure
Degree reduces；When hydrogen ion concentration is excessively high, the solubility increase of manganese oxalate is difficult to form crystallization precipitation.
Wherein, oxalates is at least one of sodium oxalate, potassium oxalate, sodium bioxalate and potassium binoxalate.
Wherein, the additional amount of demanganization agent is 1.2~1.5 times of manganese content in vanadium slag pickle liquor with molar amount.Demanganization agent
The Controlling principle of additional amount is to make manganese precipitating completely, but be unlikely to add causes to waste too much.
Wherein, vanadium slag pickle liquor is obtained after sulfuric acid leaching by the vanadium slag clinker after calcification baking.
Wherein, the acidity of the vanadium slag pickle liquor is adjusted using sulfuric acid or ammonium hydroxide.
Wherein, demanganization stands at least 30min after reacting 30~100min at 40~90 DEG C.
Wherein, vanadium concentration is 5~50g/L in vanadium slag pickle liquor, and manganese concentration is 2~30g/L.
Wherein, demanganization after-purification liquid is used for subsequent precipitation technique, obtains manganese oxalate byproduct after filter cake drying.
Wherein, MnC in manganese oxalate byproduct is obtained after filter cake drying2O4Content is between 95.23%~97.12%.
Wherein, Mn concentration is reduced to < 0.05g/L in demanganization after-purification liquid.
Embodiment 1
2.67L vanadium slag pickle liquor is taken to carry out demanganization test, the 5.95g/L of concentration containing vanadium of vanadium slag pickle liquor, manganese concentration
2.72g/L, hydrogen ion concentration 3.2 × 10-4mol/L；1.5 times of anhydrous oxalic acid of manganese molar content is added into the solution
17.8g stirring and dissolving；Using hydrogen ion concentration in ammonium hydroxide adjusting solution to 1.5 × 10-4mol/L；Solution is stirred at 90 DEG C
120min stands 30min after stirring；It is separated by solid-liquid separation to obtain demanganization after-purification liquid and filter cake, demanganization after-purification liquid is for subsequent
Precipitation technique obtains the manganese oxalate byproduct of purity 95.83% after filter cake drying.Through detecting, wherein manganese removal rate 92.36%, vanadium
Loss late 1.73%, product V after ammonium salt precipitation2O5Index of correlation it is as shown in table 1, comparative example 1 be added without demanganization agent, other
Product V is prepared in the identical situation of technique2O5。
Table 1
Embodiment 2
5.35L vanadium slag pickle liquor is taken to carry out demanganization test, the 14.56g/L of concentration containing vanadium of vanadium slag pickle liquor, manganese concentration
11.46g/L, hydrogen ion concentration 2 × 10-4mol/L；1.4 times of sodium oxalate 201.66g of manganese molar content is added into the solution
Stirring and dissolving；Hydrogen ion concentration is adjusted in solution to 2.3 × 10-3mol/L；Solution is quiet after stirring in 80 DEG C of stirring 50min
Set 30min；It is separated by solid-liquid separation to obtain demanganization after-purification liquid and filter cake, demanganization after-purification liquid is used for subsequent precipitation technique, after filter cake drying
Obtain the manganese oxalate byproduct of purity 97.02%.Through detecting, wherein manganese removal rate 97.82%, vanadium loss late 1.08%, ammonium salt are heavy
Product V after vanadium2O5Index of correlation it is as shown in table 2, comparative example 2 be added without demanganization agent, prepared in the identical situation of other techniques
Obtain product V2O5。
Table 2
Embodiment 3
12.50L vanadium slag pickle liquor is taken to carry out demanganization test, the 22.38g/L of concentration containing vanadium of vanadium slag pickle liquor, manganese concentration
18.72g/L, hydrogen ion concentration 6.3 × 10-3mol/L；1.3 times of potassium oxalates of manganese molar content are added into the solution
1018.96g stirring and dissolving；Hydrogen ion concentration is adjusted in solution to 1.3 × 10-2mol/L；Solution is in 75 DEG C of stirring 80min, stirring
After stand 30min；It is separated by solid-liquid separation to obtain demanganization after-purification liquid and filter cake, demanganization after-purification liquid is used for subsequent precipitation technique, filter
The manganese oxalate byproduct of purity 97.10% is obtained after cake drying.Through detecting, wherein manganese removal rate 98.12%, vanadium loss late
0.98%, product V after ammonium salt precipitation2O5Index of correlation it is as shown in table 3, comparative example 3 be added without demanganization agent, other technique phases
Product V is prepared in the case where2O5。
Table 3
Embodiment 4
8.00L vanadium slag pickle liquor is taken to carry out demanganization test, the 45.76g/L of concentration containing vanadium of vanadium slag pickle liquor, manganese concentration
28.89g/L hydrogen ion concentration 0.97mol/L；1.0 times of potassium binoxalate 538.43g that manganese molar content is added into the solution are stirred
Mix dissolution；Hydrogen ion concentration is adjusted in solution to 2.11 × 10-2mol/L；Solution is quiet after stirring in 60 DEG C of stirring 90min
Set 30min；It is separated by solid-liquid separation to obtain demanganization after-purification liquid and filter cake, demanganization after-purification liquid is used for subsequent precipitation technique, after filter cake drying
Obtain the manganese oxalate byproduct of purity 96.33%.Through detecting, wherein manganese removal rate 98.89%, vanadium loss late 0.21%, ammonium salt are heavy
Product V after vanadium2O5Index of correlation it is as shown in table 4, comparative example 4 be added without demanganization agent, prepared in the identical situation of other techniques
Obtain product V2O5。
Table 4
Embodiment 5
10.50L vanadium slag pickle liquor is taken to carry out demanganization test, the 40.12g/L of concentration containing vanadium of vanadium slag pickle liquor, manganese concentration
23.38g/L hydrogen ion concentration 0.35mol/L；1.20 times of sodium bioxalate 600.53g of manganese molar content are added into the solution
Stirring and dissolving；Hydrogen ion concentration is adjusted in solution to 0.781 × 10-3mol/L；Solution terminates in 65 DEG C of stirring 100min, stirring
After stand 30min；It is separated by solid-liquid separation to obtain demanganization after-purification liquid and filter cake, demanganization after-purification liquid is used for subsequent precipitation technique, and filter cake dries
The manganese oxalate byproduct of purity 96.56% is obtained after dry.Through detecting, wherein manganese removal rate 96.54%, vanadium loss late 0.57%, ammonium
Product V after salt precipitation2O5Index of correlation it is as shown in table 5, comparative example 5 be added without demanganization agent, in the identical situation of other techniques
Product V is prepared2O5。
Table 5
From 1~table of table 5 as can be seen that using after the method for the present invention, compared to the direct precipitation of not demanganization, precipitation rate and V2O5
Product purity has a distinct increment.
Claims (10)
1. the method for the vanadium manganese of immersion liquid containing vanadic acid separation, it is characterised in that include the following steps: that demanganization agent is added in vanadium slag pickle liquor,
The acidity of adjusting vanadium slag pickle liquor hydrogen ion concentration into solution is 10-5Mol/L~3.16 × 10-2Mol/L carries out demanganization, removes
Demanganization after-purification liquid and filter cake are separated by solid-liquid separation to obtain after manganese, the demanganization agent is at least one of oxalic acid or oxalates.
2. the method for the vanadium manganese of immersion liquid containing vanadic acid separation according to claim 1, it is characterised in that: the oxalates is oxalic acid
At least one of sodium, potassium oxalate, sodium bioxalate and potassium binoxalate.
3. the method for the vanadium manganese of immersion liquid containing vanadic acid separation according to claim 1 or 2, it is characterised in that: the demanganization agent
Additional amount is with 1.2~1.5 times that molar amount is manganese content in vanadium slag pickle liquor.
4. the method for the described in any item vanadium manganese of immersion liquid containing vanadic acid separation according to claim 1~3, it is characterised in that: the vanadium
Slag pickle liquor is obtained by the vanadium slag clinker after calcification baking through sulfuric acid leaching.
5. the method for the vanadium manganese of immersion liquid containing vanadic acid separation according to any one of claims 1 to 4, it is characterised in that: use sulphur
Acid or ammonium hydroxide adjust the acidity of the vanadium slag pickle liquor.
6. the method for the described in any item vanadium manganese of immersion liquid containing vanadic acid separation according to claim 1~5, it is characterised in that: described to remove
Manganese stands at least 30min after reacting 30~100min at 40~90 DEG C.
7. the method for the described in any item vanadium manganese of immersion liquid containing vanadic acid separation according to claim 1~6, it is characterised in that: the vanadium
Vanadium concentration is 5~50g/L in slag pickle liquor, and manganese concentration is 2~30g/L.
8. the method for the described in any item vanadium manganese of immersion liquid containing vanadic acid separation according to claim 1~7, it is characterised in that: described to remove
Manganese after-purification liquid is used for subsequent precipitation technique, obtains manganese oxalate byproduct after filter cake drying.
9. the method for the vanadium manganese of immersion liquid containing vanadic acid separation according to claim 8, it is characterised in that: the manganese oxalate byproduct
Middle MnC2O4Content is between 95.23%~97.12%.
10. the method for the described in any item vanadium manganese of immersion liquid containing vanadic acid separation according to claim 1~9, it is characterised in that: described to remove
Mn concentration is reduced to < 0.05g/L in manganese after-purification liquid.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110331298A (en) * | 2019-08-22 | 2019-10-15 | 成都先进金属材料产业技术研究院有限公司 | The method containing manganese in vanadium leachate of removal |
| CN112195347A (en) * | 2020-09-27 | 2021-01-08 | 攀钢集团攀枝花钢铁研究院有限公司 | Vanadium extraction method of calcified vanadium slag |
| CN112266018A (en) * | 2020-10-16 | 2021-01-26 | 成都先进金属材料产业技术研究院有限公司 | Method for preparing nano vanadium dioxide by reverse hydrolysis precipitation |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103922454A (en) * | 2014-04-15 | 2014-07-16 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for removing manganese from acidic molybdenum precipitation wastewater |
| CN107541599A (en) * | 2017-10-27 | 2018-01-05 | 成都先进金属材料产业技术研究院有限公司 | Use the preparation method of acid high manganese high purity containing vanadium leachate vanadium |
-
2018
- 2018-09-29 CN CN201811152151.3A patent/CN109022783A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103922454A (en) * | 2014-04-15 | 2014-07-16 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for removing manganese from acidic molybdenum precipitation wastewater |
| CN107541599A (en) * | 2017-10-27 | 2018-01-05 | 成都先进金属材料产业技术研究院有限公司 | Use the preparation method of acid high manganese high purity containing vanadium leachate vanadium |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110331298A (en) * | 2019-08-22 | 2019-10-15 | 成都先进金属材料产业技术研究院有限公司 | The method containing manganese in vanadium leachate of removal |
| CN112195347A (en) * | 2020-09-27 | 2021-01-08 | 攀钢集团攀枝花钢铁研究院有限公司 | Vanadium extraction method of calcified vanadium slag |
| CN112266018A (en) * | 2020-10-16 | 2021-01-26 | 成都先进金属材料产业技术研究院有限公司 | Method for preparing nano vanadium dioxide by reverse hydrolysis precipitation |
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