CN110106344A - Vanadium slag carbonating leaches cleaning extraction vanadium method - Google Patents
Vanadium slag carbonating leaches cleaning extraction vanadium method Download PDFInfo
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- CN110106344A CN110106344A CN201910549124.8A CN201910549124A CN110106344A CN 110106344 A CN110106344 A CN 110106344A CN 201910549124 A CN201910549124 A CN 201910549124A CN 110106344 A CN110106344 A CN 110106344A
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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
- C22B1/00—Preliminary treatment of ores or scrap
- C22B1/02—Roasting 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
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
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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
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Abstract
The invention belongs to the technical field of wet metallurgy of vanadium, and in particular to vanadium slag carbonating leaches cleaning extraction vanadium method.The vanadium slag carbonating leaching cleaning extraction vanadium method that technical problem to be solved by the invention is to provide one kind can reduce solid waste, improves precipitation rate.This method comprises the following steps: vanadium slag and calcium salt a, being mixed roasting, obtain roasting clinker；B, water, carbonate containing sodium and carbonate containing ammonium is added to leach into roasting clinker, separation of solid and liquid obtains leachate；The dosage of the carbonate containing sodium is 1.0~1.5 times that vanadium mole in roasting clinker is calculated as with Na；C, desiliconizing agent is added into leachate, separation of solid and liquid obtains obtaining ammonium metavanadate and Upper-liquor of Precipitating Vanadate Process except solution after silicon, precipitation, separation of solid and liquid, ammonium metavanadate is calcined up to vanadic anhydride.The method of the present invention improves precipitation rate, reduces the use of leaching agent, while drastically reducing the generation of solid waste.
Description
Technical field
The invention belongs to the technical field of wet metallurgy of vanadium, and in particular to vanadium slag carbonating leaches cleaning extraction vanadium method.
Background technique
Vanadium slag is the primary raw material for producing vanadium oxide, and traditional production technology is sodium roasting-water logging vanadium extraction.In the vanadium extraction
In technique, the sodium oxide molybdena tailings in vanadium extraction containing 6% or so can be generated, tailings in vanadium extraction secondary use is more difficult, and vanadium chromium restores
Filter cake and a large amount of solid waste sodium sulphate are difficult to handle, and environmentally friendly hidden danger is larger；Can consume a large amount of sodium carbonate in vanadium extracting process, technique at
This is higher.For the production cost for reducing vanadium oxide, environmentally friendly hidden danger is eliminated, vanadium slag calcification baking-carbonating is proposed and leaches preparation
The technique thinking of vanadium oxide.
The University Of Chongqing Ph.D. Dissertation that Li new life delivers discloses " the low-grade vanadium slag roasting-Leach reaction mistake of high calcium
Journey mechanism study ", wherein the leaching agent concentration of sodium carbonate used in vanadium slag calcification baking Sodium Carbonate Leaching process study for
160g/L, leaching liquid-solid ratio are 10:1 (mL/g).The leachate vanadium concentration obtained using this method is relatively low, and Na/V causes than high
Precipitation rate when post precipitation ammonium metavanadate is low.
Patent document CN102560086A discloses a kind of extraction vanadium method of ammonium carbonate leaching vanadium slag clinker, and this method uses
The sal volatile of 200~800g/L is leached according to liquid-solid ratio 5:1~30:1 at 60~98 DEG C with vanadium slag clinker.Using this
The leaching agent consumption that method uses is big, high production cost；Also, since the solubility of ammonium metavanadate is small, in order to avoid vanadium with
The form precipitating of ammonium metavanadate enters residue, and this method is needed to control biggish liquid-solid ratio when being leached using ammonium carbonate, therefore, obtained
Vanadium concentration to leachate is relatively low；The reduction of the solubility with temperature of another aspect ammonium metavanadate and become smaller, this method leachate
Ammonium metavanadate is easily precipitated when reducing in temperature, causes solution system unstable.
Summary of the invention
The vanadium slag carbonating that technical problem to be solved by the invention is to provide one kind can reduce solid waste, improves precipitation rate
Leach cleaning extraction vanadium method.
The present invention solves above-mentioned technical problem the technical solution adopted is that providing vanadium slag carbonating leaches cleaning vanadium extraction side
Method, this method comprises the following steps:
A, vanadium slag and calcium salt are mixed and is roasted, obtain roasting clinker；
B, water, carbonate containing sodium and carbonate containing ammonium is added to leach into roasting clinker, separation of solid and liquid obtains leachate；Containing sodium
The dosage of carbonate is 1.0~1.5 times that vanadium mole in roasting clinker is calculated as with Na；The dosage of the carbonate containing ammonium is with CO3 2-
It is calculated as 1.5~2.5 times of roasting clinker vanadium mole；
C, desiliconizing agent is added into leachate, separation of solid and liquid is obtained except solution after silicon, precipitation, and separation of solid and liquid obtains metavanadic acid
Ammonium and Upper-liquor of Precipitating Vanadate Process calcine ammonium metavanadate up to vanadic anhydride.
Wherein, above-mentioned vanadium slag carbonating leaches in cleaning extraction vanadium method, meets in step a at least one of following:
The granularity of the vanadium slag is less than 0.096mm.
The dosage of the calcium salt is calculated as the 0%~8% of vanadium slag quality with CaO.
The calcium salt is at least one of calcium carbonate, calcium hydroxide, calcium oxide.
The condition of the roasting is in 800~950 DEG C of 40~200min of roasting.
Wherein, above-mentioned vanadium slag carbonating leaches in cleaning extraction vanadium method, in step b, the carbonate containing sodium be sodium carbonate,
At least one of sodium bicarbonate.
Preferably, the carbonate containing sodium is sodium bicarbonate.
Further, in step b, the carbonate containing ammonium is at least one of ammonium carbonate, ammonium hydrogen carbonate.Preferably,
Institute
Stating carbonate containing ammonium is ammonium hydrogen carbonate.
Further, in step b, the temperature of the leaching is 80~100 DEG C；The time of leaching is 90~150min.
Further, in step b, the leaching liquid-solid ratio control is in 1.8~2.5:1；The unit for leaching liquid-solid ratio
It is mL:g.
Wherein, above-mentioned vanadium slag carbonating leaches in cleaning extraction vanadium method, and in step c, the desiliconizing agent is sodium aluminate；It is described
The molar ratio that the dosage of sodium aluminate is Al/Si is 0.5~1.0；The precipitation is using ammonium hydrogen carbonate or ammonium carbonate, control
NH4 +The molar ratio of/V is 0.9~2.0.
Further, in step c, it is described except after silicon solution return leaching step absorb the ammonia escaped in leaching process,
Precipitation again after carbon dioxide.
Further, in step c, the pH for controlling Upper-liquor of Precipitating Vanadate Process is 9.0~9.6.
Further, in step c, Upper-liquor of Precipitating Vanadate Process is returned into leaching step as leaching agent and is recycled.
Vanadium slag of the present invention is that the obtained common vanadium slag of oxidation blowing or high calcium high phosphorus vanadium are carried out to vanadium-bearing hot metal
Slag.
The beneficial effects of the present invention are:
The method of the present invention leaches roasting clinker using the mixture of carbonate containing ammonium and the carbonate containing sodium, by controlling sodium salt
Dosage obtain low sodium content leachate, convenient for improve precipitation rate, make precipitation rate up to 90% or more.The method of the present invention passes through
Liquid-solid ratio and extraction temperature are leached in control, and obtain high concentration contains vanadium leachate, avoid precipitation ammonium metavanadate, improve molten
The stability of liquid system.The method of the present invention is utilized except the ammonia escaped in solution absorption leaching process after silicon realizes following for ammonia solution
Ring utilizes, and reduces the dosage of precipitation process ammonium hydrogen carbonate, while avoiding environmental pollution.The method of the present invention will not generate vanadium chromium also
Former filter cake and solid waste sodium sulphate, and obtained Upper-liquor of Precipitating Vanadate Process can return and leach process as leaching agent recycling, in fact
Show vanadium slag low cost clean manufacturing vanadium oxide, reduced the consumption of leaching agent, solves traditional vanadium slag sodium roasting-flooding
The problem of process costs existing for vanadium are high, and solid waste tailings, vanadium chromium reduction filter cake, sodium sulphate difficulty utilize.
Specific embodiment
Raw material, equipment used in the specific embodiment of the invention are known product, are obtained by purchase commercial product.
It is carbonated the present invention provides vanadium slag and leaches cleaning extraction vanadium method, included the following steps:
A, vanadium slag and calcium salt are mixed and is roasted, obtain roasting clinker；
B, water, carbonate containing sodium and carbonate containing ammonium is added to leach into roasting clinker, separation of solid and liquid obtains leachate；Containing sodium
The dosage of carbonate is 1.0~1.5 times that vanadium mole in roasting clinker is calculated as with Na；The dosage of the carbonate containing ammonium is with CO3 2-
It is calculated as 1.5~2.5 times of roasting clinker vanadium mole；
C, desiliconizing agent is added into leachate, separation of solid and liquid is obtained except solution after silicon, precipitation, and separation of solid and liquid obtains metavanadic acid
Ammonium and Upper-liquor of Precipitating Vanadate Process calcine ammonium metavanadate up to vanadic anhydride.
In step a of the present invention, the vanadium slag of use be vanadium-bearing hot metal is carried out oxidation blow obtained common vanadium slag or
Vanadium-bearing slag of high calcium and high phosphor.In order to expose the vanadium iron spinelle in vanadium slag sufficiently, conducive to the oxidation of vanadium iron spinelle, also it is conducive to vanadium slag
It comes into full contact with and reacts with calcium salt, vanadium slag is crushed, granularity is selected to be less than the vanadium slag of 0.096mm.Since metavanadic acid calcium is in water
In solubility it is bigger than pyrovanadic acid calcium and positive calcium vanadate and be conducive to leach, in order to control the vanadium in calcification baking clinker with inclined vanadium
Sour calcium is main existence form, and the amount of calcium salt is added with CaO and is calculated as the 0%~8% of vanadium slag quality.
In step b of the present invention, roasting clinker is mixed using carbonate containing sodium and carbonate containing ammonium and is used as leaching agent, one
Aspect, ammonium carbonate or ammonium hydrogen carbonate provide carbonate and react generation calcium carbonate with calcium ion, since the solubility of calcium carbonate is less than
Metavanadic acid calcium, pyrovanadic acid calcium and positive calcium vanadate, the calcium carbonate of generation enter in slag, enter vanadium in solution；On the other hand, carbonic acid
Ammonium and ammonium hydrogen carbonate are thermally decomposed to generate ammonia, realize the separation of ammonia and sodium, and ammonia is made to escape solution, are the steady of high vanadium concentrations solution
Determine to exist and create condition.In addition, inventor is Na/V=1.0~1.5 (molar ratio) by the dosage of control carbonate containing sodium,
The concentration of sodium in solution is reduced, is convenient for post precipitation ammonium metavanadate, convenient for the raising of precipitation rate.Inventor is in order to further obtain
Obtain high concentration contains vanadium leachate, is conducive to precipitating ammonium metavanadate, will leach liquid-solid ratio and control at 1.8~2.5:1 (mL:g).At this
In inventive step b, in order to be conducive to the dissolution of metavanadic acid calcium, the temperature of leaching is controlled at 80~100 DEG C, while being conducive to ammonia
Solution is escaped, precipitation ammonium metavanadate is avoided, improves the stability of solution system.
It, will be except the ammonia and dioxy escaped in solution return leaching step absorption leaching process after silicon in step c of the present invention
Change carbon, realize recycling for ammonia solution, reduce the dosage of ammonium hydrogen carbonate in precipitation process, while avoiding and causing environment dirty
Dye.Gained Upper-liquor of Precipitating Vanadate Process mainly contains sodium carbonate, ammonium carbonate and a small amount of sodium vanadate, can directly return to leaching step as leaching
Agent is leached roasting clinker and is recycled, and when using Upper-liquor of Precipitating Vanadate Process circulating leaching, sodium salt is suitably added according to na concn keeps it full
Sufficient Na/V=1.0~1.5 (molar ratio), reduce the dosage of leaching agent.The present invention controls in precipitation when precipitating ammonium metavanadate
Layer liquid pH=9.0~9.6 are to control the HCO in precipitation liquid3 -Concentration avoids sodium from being precipitated out in the form of sodium bicarbonate.
In step c of the present invention, ammonium metavanadate is subjected to oxidizing roasting up to vanadic anhydride.
The present invention will further be elaborated by specific embodiment below.
Embodiment 1
Take vanadium slag of the granularity less than 0.096mm (containing V2O517.2%, CaO 1.84%, P 0.04%) 100g, uses Muffle
Furnace roasts 40min in the case where 950 DEG C of maturing temperature, blowing air and obtains roasting clinker；It is added to after roasting clinker is crushed
In 200mL water, while 23.6g sodium bicarbonate and 25.3g ammonium hydrogen carbonate is added, leaching under conditions of 95 DEG C of slurry temperature
120min, leaching liquid-solid ratio are 2:1, are separated by solid-liquid separation and obtain leachate and residue, residue TV 0.92wt% and Na0.39%, vanadium
Turn leaching rate 90.3%；0.8g sodium aluminate is added into leachate, filtering is obtained except solution after silicon after stirring 20min；Except molten after silicon
Liquid is cooled to 15 DEG C, and 32g ammonium bicarbonate precipitation is added in the case of stirring and reacts 180min, is separated by solid-liquid separation, obtains metavanadic acid
Ammonium and Upper-liquor of Precipitating Vanadate Process；Upper-liquor of Precipitating Vanadate Process TV 3.94g/L；Ammonium metavanadate is in 500 DEG C of oxidizing roasting 5h, the sample V of acquisition2O5Contain
Amount 98.9%.Precipitation rate is 90.94%.
Upper-liquor of Precipitating Vanadate Process is directly used in next round as leaching agent and leaches, and when leaching suitably adds sodium carbonate or sodium bicarbonate
It is set to meet the control of Na/V=1.0~1.5 (molar ratio) requirement；Ammonium salt does not have to add.
Embodiment 2
Take vanadium slag of the granularity less than 0.096mm (containing V2O517.2%, CaO 1.84%, P 0.04%) 100g and calcium oxide
3g is uniformly mixed, and roasts 80min in the case where 900 DEG C of maturing temperature, blowing air with Muffle furnace；Roasting clinker is added after crushing
Into 250mL water, while 19.5g sodium carbonate and 30.8g ammonium hydrogen carbonate is added, leaching is stirred under conditions of 100 DEG C of slurry temperature
150min out, leaching liquid-solid ratio are 2.5:1, are separated by solid-liquid separation and obtain containing vanadium leachate and residue, residue TV 1.06wt% and Na
0.34%, vanadium turns leaching rate 88.8%；0.7g sodium aluminate is added into leachate, filtering is obtained except solution after silicon after stirring 20min；
By except the ammonia and carbon dioxide escaped in solution return leaching step absorption leaching process after silicon, solution is cooling after then removing silicon
To 18 DEG C, addition 30g ammonium bicarbonate precipitation reacts 180min in the case of stirring, is separated by solid-liquid separation, and obtains ammonium metavanadate and sinks
Vanadium upper liquid, Upper-liquor of Precipitating Vanadate Process TV 3.14g/L；Ammonium metavanadate is in 500 DEG C of oxidizing roasting 5h, the sample V of acquisition2O5Content
98.7%.Precipitation rate is 90.82%.
Upper-liquor of Precipitating Vanadate Process is directly used in next round as leaching agent and leaches, and when leaching suitably adds sodium carbonate or sodium bicarbonate
It is set to meet the control of Na/V=1.0~1.5 (molar ratio) requirement；Ammonium salt does not have to add.
Embodiment 3
Take vanadium slag of the granularity less than 0.096mm (containing V2O517.2%, CaO 1.84%, P 0.04%) 100g and calcium oxide
8g is uniformly mixed, and roasts 180min in the case where 850 DEG C of maturing temperature, blowing air with Muffle furnace；It roasts after clinker crushes and adds
Enter into 250mL water, while 17.8g sodium carbonate and 37.2g ammonium hydrogen carbonate is added, leaching is stirred under conditions of 85 DEG C of slurry temperature
100min out, leaching liquid-solid ratio are 2.3:1, are separated by solid-liquid separation and obtain leachate and residue, residue TV 1.02wt% and Na
0.37%, vanadium turns leaching rate 89.4%；0.7g sodium aluminate is added into leachate, filtering is obtained except solution after silicon after stirring 20min；
By except the ammonia and carbon dioxide escaped in solution return leaching step absorption leaching process after silicon, solution is cooling after then removing silicon
To 20 DEG C, addition 30g ammonium bicarbonate precipitation reacts 180min in the case of stirring, is separated by solid-liquid separation, and obtains ammonium metavanadate and sinks
Vanadium upper liquid, Upper-liquor of Precipitating Vanadate Process TV 3.34g/L；Ammonium metavanadate is in 500 DEG C of oxidizing roasting 5h, the sample V of acquisition2O5Content
98.9%.Precipitation rate is 90.31%.
Upper-liquor of Precipitating Vanadate Process is directly used in next round as leaching agent and leaches, and when leaching suitably adds sodium carbonate or sodium bicarbonate
It is set to meet the control of Na/V=1.0~1.5 (molar ratio) requirement；Ammonium salt does not have to add.
In conclusion obtaining the leachate of low sodium content by the dosage of control sodium salt using the method for the present invention, improve
Vanadium turns leaching rate and precipitation rate, makes precipitation rate 90.31%~90.94%.The method of the present invention will not generate vanadium chromium reduction filter cake
With solid waste sodium sulphate, and obtained Upper-liquor of Precipitating Vanadate Process can return leach process as leaching agent recycling, realize vanadium
Slag low cost clean manufacturing vanadium oxide, reduces the consumption of leaching agent, solves traditional vanadium slag sodium roasting-water logging vanadium extraction and exists
Process costs it is high, the problem of solid waste tailings, vanadium chromium reduction filter cake, sodium sulphate difficulty utilize.
Claims (10)
1. vanadium slag carbonating leaches cleaning extraction vanadium method, it is characterised in that include the following steps:
A, vanadium slag and calcium salt are mixed and is roasted, obtain roasting clinker；
B, water, carbonate containing sodium and carbonate containing ammonium is added to leach into roasting clinker, separation of solid and liquid obtains leachate；Carbonic acid containing sodium
The dosage of salt is 1.0~1.5 times that vanadium mole in roasting clinker is calculated as with Na；The dosage of the carbonate containing ammonium is with CO3 2-It is calculated as
Roast 1.5~2.5 times of clinker vanadium mole；
C, be added desiliconizing agent into leachate, separation of solid and liquid is obtained except solution after silicon, precipitation, separation of solid and liquid obtain ammonium metavanadate and
Upper-liquor of Precipitating Vanadate Process calcines ammonium metavanadate up to vanadic anhydride.
2. vanadium slag according to claim 1 carbonating leaches cleaning extraction vanadium method, it is characterised in that: meet in step a with
It is at least one of lower:
The granularity of the vanadium slag is less than 0.096mm；
The dosage of the calcium salt is calculated as the 0%~8% of vanadium slag quality with CaO；
The calcium salt is at least one of calcium carbonate, calcium hydroxide, calcium oxide；
The condition of the roasting is in 800~950 DEG C of 40~200min of roasting.
3. vanadium slag carbonating according to claim 1 or 2 leaches cleaning extraction vanadium method, it is characterised in that: in step b, institute
Stating carbonate containing sodium is at least one of sodium carbonate, sodium bicarbonate；Preferably, the carbonate containing sodium is sodium bicarbonate.
4. described in any item vanadium slag carbonatings leach cleaning extraction vanadium method according to claim 1~3, it is characterised in that: step b
In, the carbonate containing ammonium is at least one of ammonium carbonate, ammonium hydrogen carbonate；Preferably, the carbonate containing ammonium is bicarbonate
Ammonium.
5. vanadium slag carbonating according to any one of claims 1 to 4 leaches cleaning extraction vanadium method, it is characterised in that: step b
In, the temperature of the leaching is 80~100 DEG C；The time of leaching is 90~150min.
6. described in any item vanadium slag carbonatings leach cleaning extraction vanadium method according to claim 1~5, it is characterised in that: step b
In, the leaching liquid-solid ratio control is in 1.8~2.5:1.
7. described in any item vanadium slag carbonatings leach cleaning extraction vanadium method according to claim 1~6, it is characterised in that: step c
In, the desiliconizing agent is sodium aluminate；The molar ratio that the dosage of the sodium aluminate is Al/Si is 0.5~1.0；The precipitation uses
Be ammonium hydrogen carbonate or ammonium carbonate, control NH4 +The molar ratio of/V is 0.9~2.0.
8. described in any item vanadium slag carbonatings leach cleaning extraction vanadium method according to claim 1~7, it is characterised in that: step c
In, it is described except precipitation again after the ammonia escaped in solution return leaching step absorption leaching process after silicon, carbon dioxide.
9. described in any item vanadium slag carbonatings leach cleaning extraction vanadium method according to claim 1~8, it is characterised in that: step c
In, the pH for controlling Upper-liquor of Precipitating Vanadate Process is 9.0~9.6.
10. described in any item vanadium slag carbonatings leach cleaning extraction vanadium method according to claim 1~9, it is characterised in that: step
In c, Upper-liquor of Precipitating Vanadate Process is returned into leaching step as leaching agent and is recycled.
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| CN201910549124.8A CN110106344A (en) | 2019-06-24 | 2019-06-24 | Vanadium slag carbonating leaches cleaning extraction vanadium method |
| PCT/CN2020/097742 WO2020259500A1 (en) | 2019-06-24 | 2020-06-23 | Method for clean vanadium extraction by carbonation leaching of vanadium slag |
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| WO2020259500A1 (en) * | 2019-06-24 | 2020-12-30 | 攀钢集团研究院有限公司 | Method for clean vanadium extraction by carbonation leaching of vanadium slag |
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| CN114959251A (en) * | 2022-05-27 | 2022-08-30 | 四川大学 | Vanadium slag roasting leaching method |
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