CN108179265A - A kind of method from separation and Extraction vanadium in material containing chrome alum - Google Patents
A kind of method from separation and Extraction vanadium in material containing chrome alum Download PDFInfo
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- CN108179265A CN108179265A CN201810084493.XA CN201810084493A CN108179265A CN 108179265 A CN108179265 A CN 108179265A CN 201810084493 A CN201810084493 A CN 201810084493A CN 108179265 A CN108179265 A CN 108179265A
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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
- C22B34/00—Obtaining refractory metals
- C22B34/20—Obtaining niobium, tantalum or vanadium
- C22B34/22—Obtaining vanadium
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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
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet 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
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/04—Working-up slag
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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 present invention relates to a kind of method from separation and Extraction vanadium in material containing chrome alum, this method uses additive NaOH+Na2CO3It adds in material containing chrome alum and carries out microwave calcining, after roasting, carry out water logging, be separated by filtration later, obtain containing vanadium solution and tailings.The method of the present invention effectively reduces the temperature of roasting, reduces the energy, the reaction time also greatly shortens, efficient, energy- and time-economizing reduces cost, easy to operate, while the pollution-free generation of roasting process, the rate of recovery of vanadium greatly improves, and can reach more than 99%, while recyclable chromium while vanadium is recycled.
Description
Technical field
The present invention relates to the methods of Leaching of Vanadium from Vanadium slag, and in particular to a kind of method from separation and Extraction vanadium in material containing chrome alum.
Background technology
Vanadium is " monosodium glutamate of modern industry ", is that development modern industry, modern national defense and modern science and technology are indispensable
Important materials.Vanadium dosage in Metallurgy Industry is maximum.From the point of view of world wide, it is total that consumption of the vanadium in steel and iron industry accounts for its production
The 85% of amount.At the same time, application of the vanadium in other fields such as chemical industry, vanadium cell, aerospace is also constantly extending, and have
Good development prospect.
In steel and iron industry by vanadium titano-magnetite produce vanadium slag be vanadium extraction primary raw material, the vfanadium compound in China about 80%
It is produced by raw material of vanadium slag.Pig iron containing vanadium of the vanadium titano-magnetite through blast furnace or direct-reduction flow production, further passes through selection
Property oxidation molten iron, make vanadium aoxidize after enter clinker, obtain the higher vanadium slag of content of vanadium.During vanadium is blown in converter, in iron ore
Containing chromium, because vanadium, chromium property are close, also oxidation enters vanadium slag to chromium together, i.e., in material containing chrome alum.
And have traditional sodium roasting method and calcification baking method currently with process for extracting vanadium of the vanadium slag for raw material, (1) sodium
Roasting method uses NaCl, NaSO4The compound of sodium is waited, oxidizing roasting 4-8 hours in the range of 800-100 DEG C, generation is water-soluble
Sodium vanadate, then hot water leaching vanadium；Both caused liquid slag energy consumption higher during this, and used in roasting process
NaCl、NaSO4The a large amount of Cl that sodium salts is waited to be generated as additive2、HCl、SO2Pernicious gases are waited, so as to pollute environment, danger
Evil health.(2) it using calcification baking method, with addition of lime stone or lime in vanadium slag, is roasted in the range of 1000-1400 DEG C
2 hours or so, be that calcium vanadate not soluble in water is generated in roasting material, then the Leaching Vanadium in 200 DEG C or so of aqueous slkali, precipitation
Detach the vanadic anhydride in leachate.Relative to sodium roasting method, calcification baking does not have pernicious gas spilling, and pollution is few, but
It generally requires in follow-up vanadium extracting process and is leached using sulfuric acid, so the corrosion resistance to leaching equipment is more demanding, and
Impurity is more in the molten leachate of acid and pentoxide content is low, is unfavorable for the recycling of follow-up vanadium product.
In addition, traditional sodium roasting extraction process, is susceptible to vanadium slag and sintered bond, caking phenomenon, Er Qiechuan occurs
The sodium roasting vanadium-extracting technique of system can only recycle vanadium, and chromium has then been remained in tailings, and part chromium therein is converted into after baking
Cr6+Potential environmental hazard is not only brought, while causes the loss of valuable element.
To sum up, existing method is mainly shown as that vanadium recovery is relatively low, and there are high-temperature roasting, energy consumption is higher and environment is dirty
The problems such as dye.
Invention content
(1) technical problems to be solved
In order to solve the above problem of the prior art, the present invention provides a kind of from the side of separation and Extraction vanadium in material containing chrome alum
Method, this method can effectively extract vanadium, while can be by waste liqouor, and it is low to consume energy, pollution-free.
(2) technical solution
In order to achieve the above object, the main technical schemes that the present invention uses include：
A kind of method from separation and Extraction vanadium in material containing chrome alum includes the following steps：
S1, by sodium hydroxide and sodium carbonate by quality parts ratio it is 1~5:5~1 mixing, by obtained mixture with containing chromium
Vanadium material is 1 in mass ratio:1 is mixed, and reactant is made；
S2, reactant is used to microwave calcining, calcination temperature is 400~800 DEG C；
S3, the sample after being roasted in step S2 is subjected to water logging, separation of solid and liquid, obtains containing vanadium solution and tailings later.
Method as described above, it is preferable that in step s 2, the roasting time is 3~60 minutes.
Method as described above, it is preferable that in step s 2, during the roasting, the reaction of generation is：
4FeO·V2O3+24NaOH+5O2=8Na3VO4+2Fe2O3+12H2O
4FeO·V2O3+12Na2CO3+5O2=8Na3VO4+2Fe2O3+12CO2
4FeO·Cr2O3+16NaOH+7O2=8Na2CrO4+2Fe2O3+8H2O
4FeO·Cr2O3+8Na2CO3+7O2=8Na2CrO4+2Fe2O3+8CO2。
In follow-up water logging, Na3VO4And Na2CrO4Water is dissolved in, is formed containing vanadium solution, Fe2O3It is not soluble in water, into tailings.
Method as described above, it is preferable that in step s3, the sample after the roasting chooses grain by crushing and screening
Carry out water logging of the degree less than or equal to 74 μm.
Method as described above, it is preferable that in step s3,25~95 DEG C of the temperature of the water logging, the water logging when
Between be 10~120 minutes.
Method as described above, it is preferable that in step s3, the water consumption of the water logging is is used for water logging sample after roasting
1~10 times of quality.
Further, it is preferable in step s 2, the temperature of the roasting is 550~650 DEG C；The time of the roasting is 5
~20 minutes；In step s3, the water consumption of the water logging is 5~10 times that water logging sample quality is used for after roasting, and vanadium returns
Yield is preferable.
Method as described above, it is preferable that in step sl, the grain size of the material containing chrome alum is less than or equal to 74 μm.Grain
The abundant progress defined conducive to reaction of diameter, improves the rate of recovery.
Method as described above, the weight ratio of constituents content being primarily adapted for use in material containing chrome alum are：FeO for 30~
38%, Cr2O3For 5.5~8.5%, Al2O3For 0.5~1.5%, TiO2For 8~12%, SiO2For 12~15%, MgO 0.5
~1.5%, CaO be 0.5~1.5%, V be 6.5~9.5%, Mn be 4~6%, P be 0.01~0.1% and Na be 0.2~
0.8%.
(3) advantageous effect
The beneficial effects of the invention are as follows：
The method from separation and Extraction vanadium in material containing chrome alum of the offer of the present invention, using additive NaOH+Na2CO3, and
Using microwave calcining, the temperature of roasting can be effectively reduced, reduces energy consumption, the reaction time also greatly shortens, efficient, section
Can be time saving, cost is reduced, it is easy to operate, while the pollution-free generation of roasting process, the rate of recovery of vanadium greatly improve, it can be to 99%
More than, and recyclable chromium while vanadium is recycled.
Description of the drawings
Fig. 1 is the flow chart of the method for the present invention.
Specific embodiment
Inventor carries out many experiments, when research finds to roast to containing chrome alum material, individually using NaOH
If a kind of additive, fusing point is relatively low, and reaction is fiercer, relatively bad control and is easily sintered blocking, while independent NaOH
Cost is also high；And individually use Na2CO3If a kind of additive, reaction temperature then needs relatively high, heating process cost
It is higher, and the conversion ratio of vanadium is relatively low.The two is used in combination, and can reduce W-response temperature, moreover it is possible to improve vanadium
Conversion ratio, while can also reduce and be sintered blocking rate and reduce the cost of follow-up Leach reaction (firing product are relatively easily crushed to institute
Need granularity).
NaOH and Na is used in the present invention2CO3As additive, NaOH and Na2CO3Facilitation can be mutually played, it can
Large area is sintered blocking or bulk when reducing roasting so that sample keeps preferable particle sponginess after roasting.Mainly occur
It chemically reacts and is：
4FeO·V2O3+24NaOH+5O2=8Na3VO4+2Fe2O3+12H2O
4FeO·V2O3+12Na2CO3+5O2=8Na3VO4+2Fe2O3+12CO2
4FeO·Cr2O3+16NaOH+7O2=8Na2CrO4+2Fe2O3+8H2O
4FeO·Cr2O3+8Na2CO3+7O2=8Na2CrO4+2Fe2O3+8CO2。
The situation of traditional Muffle furnace roasting, belongs to heat transfer, heating is from outside to inside；And microwave roasting is employed in the present invention
Burn, belong to inner ion resonant heating, by interior cause outside, heating is rapid, and due to a degree of ion resonance heat it is asynchronous
Cause it is uneven in temperature, easily cause reaction particles division dusting, the reaction made is more thorough, and required temperature be not need very
High temperature, and the reaction time is short, effectively reduces energy consumption and saves the time.
Further study show that the suitable calcination temperature of the method for the present invention is 400~800 DEG C, and during higher than 700 DEG C, by
It being increased faster than other temperature sections in ferrous oxygenation efficiency, the heat release of this temperature section is rapider, is easy for that furnace charge is caused to be sintered,
The ferrous package to vanadium is made to reduce the oxygenation efficiency of vanadium, make the leaching rate of vanadium reduce than more serious.When calcination temperature is preferably 550
At~650 DEG C, the leaching rate of vanadium is preferable.
In order to preferably explain the present invention, in order to understand, below in conjunction with the accompanying drawings, by specific embodiment, to this hair
It is bright to be described in detail.
The ingredient of the material containing chrome alum used in following embodiment of the present invention is as shown in table 1, and be weight percentage content.
The Contents of Main Components of 1. material containing chrome alum of table
| TFe% | FeO% | Cr2O3% | Al2O3% | TiO2% | SiO2% |
| 27.51 | 34.47 | 6.25 | 1.29 | 10.66 | 14.30 |
| MgO% | CaO% | V% | Mn% | P% | Na% |
| 1.16 | 1.21 | 7.89 | 5.41 | 0.066 | 0.64 |
Embodiment 1
A kind of method from separation and Extraction vanadium in material containing chrome alum, as shown in Figure 1, carrying out as follows：
(1) it is 1 in mass ratio by sodium hydroxide and sodium carbonate:1 mixing, by the mixing of obtained sodium hydroxide and sodium carbonate
Object is 1 according to mass ratio with material containing chrome alum:1 progress dispensing is uniformly mixed to obtain mixture；Wherein, the material containing chrome alum of selection
Granularity is more than or equal to 200 mesh, i.e., less than or equal to 74 μm.
(2) mixture is put into microwave heating instrument and be sintered, the microwave frequency of microwave heating instrument is 2450MHz, institute
It is 0~4Kw with power；600 DEG C are warming up to, sintering time 10min；Roasting sample is taken out and carries out room temperature cooling；It will roasting
Sample broke after burning, and sieved with 200 mesh sieve；The roasting sample that grain size is less than or equal to 74 μm is chosen, will be screened
Sample be put into distilled water, sample quality and distilled water mass ratio are 1:5, water temperature is maintained at 60 DEG C, and extraction time is
60min；Obtained mixed liquor solid solution filter paper or filter membrane are filtered separation or standing can be used in the industrial production
The precipitation method carry out separation of solid and liquid, obtain tailings and containing vanadium solution.Wherein, after testing containing containing NaNO in vanadium solution2, NaMnO2,
Na2SiO3, NaAlO2, Na3VO4And Na2CrO4, contain Fe in tailings2O3, Na2TiO3, MgTiO3, CaSiO3, SiO2, MgO,
Al2O3, MnO2, CaO etc..
Through being detected to the vanadium in tailings, the rate of recovery is calculated using leaching rate in the present invention, by formulaIt calculates, calculation formula, m0Represent the quality of vanadium in tailings, mtRepresent the quality of vanadium in sample after roasting, R
For leaching rate.Wherein, the chemical composition content before roasting after the chemical composition content of the material samples containing chrome alum and leaching in tailings,
It is detected with inductive coupling plasma emission spectrograph (ICP-OES).
The leaching rate of vanadium is 99.18% in the present embodiment.
Embodiment 2
The present embodiment is on the basis of embodiment 1, and difference is that sodium hydroxide and sodium carbonate are 3 in mass ratio:1 is mixed
It closes, roasting is warming up to 550 DEG C, roasting time 8min, and the leaching rate for finally obtaining vanadium is 99.21%.
Embodiment 3
A kind of method from separation and Extraction vanadium in material containing chrome alum carries out as follows：
(1) it is 2 in mass ratio by sodium hydroxide and sodium carbonate:3 mixing, by the mixing of obtained sodium hydroxide and sodium carbonate
Object is 1 according to mass ratio with material containing chrome alum:1 progress dispensing is uniformly mixed to obtain mixture；
(2) mixture is put into microwave heating instrument to be sintered, by microwave heating instrument to 650 DEG C, sintering time is
10min；Roasting sample is taken out and carries out room temperature cooling；It is sieved by the sample broke after roasting, and with 200 mesh sieve；
The roasting sample that grain size is less than or equal to 74 μm is chosen, the sample screened is put into distilled water, sample quality and distillation water quality
Amount is than being 1:8, water temperature is maintained at 60 DEG C, extraction time 60min；By obtained mixed liquor solid solution filter paper or filter membrane into
Row is separated by filtration, and obtains tailings and containing vanadium solution.
After testing, it calculates (with embodiment 1), the leaching rate of vanadium is 98.65% in the present embodiment.
Embodiment 4
A kind of method from separation and Extraction vanadium in material containing chrome alum carries out as follows：
(1) it is 4 in mass ratio by sodium hydroxide and sodium carbonate:1 mixing, by the mixing of obtained sodium hydroxide and sodium carbonate
Object is 1 according to mass ratio with material containing chrome alum:1 progress dispensing is uniformly mixed to obtain mixture；Wherein, the grain of material containing chrome alum used
It spends for less than or equal to 74 μm.
(2) mixture is put into microwave heating instrument to be sintered, microwave heating instrument is warming up to 700 DEG C, sintering time is
20min；Roasting sample is taken out and carries out room temperature cooling；It is sieved by the sample broke after roasting, and with 200 mesh sieve；
The roasting sample that grain size is less than or equal to 74 μm is chosen, the sample screened is put into distilled water, sample quality and distillation water quality
Amount is than being 1:10, water temperature is maintained at 60 DEG C, extraction time 60min；The mixed liquor solid solution filter paper or filter membrane that will be obtained
Separation is filtered, obtains tailings and containing vanadium solution.
After testing, it calculates (with embodiment 1), the leaching rate of vanadium is 99.09% in the present embodiment.
Embodiment 5
On the basis of being embodiment 4, difference is the present embodiment, and sodium hydroxide is 3 in mass ratio with sodium carbonate:1, when
When extraction time is 120min, the leaching rate of vanadium is 99.52% in the present embodiment.
The above described is only a preferred embodiment of the present invention, being not the limitation that other forms are done to the present invention, appoint
What those skilled in the art can be changed or be modified as the equivalence enforcement of equivalent variations using technology contents disclosed above
Example.But it is every without departing from technical solution of the present invention content, technical spirit according to the present invention is appointed to what above example was made
What simple modification, equivalent variations and remodeling still falls within the protection domain of technical solution of the present invention.
Claims (9)
- A kind of 1. method from separation and Extraction vanadium in material containing chrome alum, which is characterized in that it includes the following steps：S1, by sodium hydroxide and sodium carbonate by quality parts ratio it is 1~5:5~1 mixing, by obtained mixture and object containing chrome alum Material is 1 in mass ratio:1 is mixed, and reactant is made；S2, reactant is used to microwave calcining, calcination temperature is 400~800 DEG C；S3, the sample after being roasted in step S2 is subjected to water logging, separation of solid and liquid, obtains containing vanadium solution and tailings later.
- 2. the method as described in claim 1, which is characterized in that in step s 2, the roasting time is 3~60 minutes.
- 3. the method as described in claim 1, which is characterized in that in step s 2, during the roasting, the reaction of generation is：4FeO·V2O3+24NaOH+5O2=8Na3VO4+2Fe2O3+12H2O4FeO·V2O3+12Na2CO3+5O2=8Na3VO4+2Fe2O3+12CO24FeO·Cr2O3+16NaOH+7O2=8Na2CrO4+2Fe2O3+8H2O4FeO·Cr2O3+8Na2CO3+7O2=8Na2CrO4+2Fe2O3+8CO2。
- 4. the method as described in claim 1, which is characterized in that in step s3, the sample after the roasting is by broken sieve Point, choose the carry out water logging that granularity is less than or equal to 74 μm.
- 5. the method as described in claim 1, which is characterized in that in step s3,25~95 DEG C of the temperature of the water logging is described The time of water logging is 10~120 minutes.
- 6. the method as described in claim 1, which is characterized in that the water consumption of the water logging is is used for water logging sample matter after roasting 1~10 times of amount.
- 7. the method as described in claim 1, which is characterized in that in step s 2, the temperature of the roasting is 550~650 DEG C； The time of the roasting is 5~20 minutes；In step s3, the water consumption of the water logging is is used for water logging sample quality after roasting 5~10 times.
- 8. the method as described in claim 1, which is characterized in that in step sl, the grain size of the material containing chrome alum is less than etc. In 74 μm.
- 9. the method as described in any one of claim 1-8, which is characterized in that weight ratio of constituents contains in the material containing chrome alum It measures and is：FeO is 30~38%, Cr2O3For 5.5~8.5%, Al2O3For 0.5~1.5%, TiO2For 8~12%, SiO2For 12~ It is 0.5~1.5%, V be 6.5~9.5%, Mn be 4~6%, P is 0.01~0.1% that 15%, MgO, which are 0.5~1.5%, CaO, It is 0.2~0.8% with Na.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109280776A (en) * | 2018-11-15 | 2019-01-29 | 华南理工大学 | A kind of method that sub-molten salt method recycles chromium in electroplating sludge |
| CN111378846A (en) * | 2020-04-08 | 2020-07-07 | 东北大学 | Method for extracting vanadium from manganese vanadium slag prepared based on vanadium blowing of converter |
| CN113912122A (en) * | 2021-12-01 | 2022-01-11 | 昆明理工大学 | Method for preparing molybdenum oxide from low-grade molybdenite |
| CN114540629A (en) * | 2021-12-30 | 2022-05-27 | 华南理工大学 | Method for extracting and recovering heavy metal chromium from metallurgical waste slag based on crystalline phase regulation |
| CN114703362A (en) * | 2022-03-17 | 2022-07-05 | 四川省银河化学股份有限公司 | Method for combined sodium roasting of vanadium-containing and chromium-containing raw materials |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109280776A (en) * | 2018-11-15 | 2019-01-29 | 华南理工大学 | A kind of method that sub-molten salt method recycles chromium in electroplating sludge |
| CN109280776B (en) * | 2018-11-15 | 2020-11-24 | 华南理工大学 | Method for recycling chromium in electroplating sludge by using sub-molten salt method |
| CN111378846A (en) * | 2020-04-08 | 2020-07-07 | 东北大学 | Method for extracting vanadium from manganese vanadium slag prepared based on vanadium blowing of converter |
| CN113912122A (en) * | 2021-12-01 | 2022-01-11 | 昆明理工大学 | Method for preparing molybdenum oxide from low-grade molybdenite |
| CN114540629A (en) * | 2021-12-30 | 2022-05-27 | 华南理工大学 | Method for extracting and recovering heavy metal chromium from metallurgical waste slag based on crystalline phase regulation |
| CN114703362A (en) * | 2022-03-17 | 2022-07-05 | 四川省银河化学股份有限公司 | Method for combined sodium roasting of vanadium-containing and chromium-containing raw materials |
| CN114703362B (en) * | 2022-03-17 | 2024-04-05 | 四川明宏恒正科技股份有限公司 | Method for combined sodium roasting of vanadium-containing and chromium-containing raw materials |
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Application publication date: 20180619 |