CN103924096B - Reclaim the method for vanadium chromium resource - Google Patents

Reclaim the method for vanadium chromium resource Download PDF

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Publication number
CN103924096B
CN103924096B CN201410175785.6A CN201410175785A CN103924096B CN 103924096 B CN103924096 B CN 103924096B CN 201410175785 A CN201410175785 A CN 201410175785A CN 103924096 B CN103924096 B CN 103924096B
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vanadium chromium
water
slag
grog
resource
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CN201410175785.6A
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CN103924096A (en
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吴恩辉
李军
侯静
李强
黄平
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攀枝花学院
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    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
    • Y02P10/20Recycling

Abstract

The present invention relates to reclaim the method for vanadium chromium resource, belong to resource and reclaim field. The technical problem to be solved in the present invention is to provide a kind of method that reclaims vanadium chromium resource. The present invention reclaims the method for vanadium chromium resource, comprises the steps: a, vanadium chromium slag is mixed with calcium carbonate, obtains mixed once material, by the oxidizing roasting of mixed once material, obtains bakes to burn the article grog; B, bakes to burn the article grog is carried out to acidleach, obtain pickle liquor and acid leaching residue; C, by acid leaching residue dry, grind after and sodium carbonate be mixed to get secondary mixture material, by the oxidizing roasting of secondary mixture material, obtain after baking grog; D, after baking grog is carried out to water logging, obtain infusion and water logging slag; E, from pickle liquor, infusion and water logging slag, separation and Extraction goes out vanadium, chromium and iron respectively. The advantages such as the method that the present invention reclaims vanadium chromium resource has vanadium, chromium recovery ratio is higher, technique is simple, equipment requirement is low, and environmental pollution is little.

Description

Reclaim the method for vanadium chromium resource
Technical field
The present invention relates to reclaim the method for vanadium chromium resource, belong to resource and reclaim field.
Background technology
Panxi Diqu vanadium titano-magnetite aboundresources, and association has chromium resource, particularly red lattice vanadium titano-magnetite, chromium and vanadium are formerContent in ore deposit is suitable, and processing at present vanadium chromium slag both at home and abroad has following several method:
(1) alkaline leaching
By vanadium chromium slag carry out that alkali soaks, purification, precipitation vanadic anhydride, the rate of recovery of vanadium is more than 90%. The master of alkaline leachingWanting problem is that process flow is long, and alkali consumption is high, has only utilized the vanadium resource in vanadium chromium, and chromium resource is processed, and does not reach vanadiumThe object of chromium comprehensive reutilization.
(2) sintering-blast furnace process method
Vanadium leached-out chromium residue is mixed with a small amount of magnetic separation scum and coke, sinters into from molten type sintering deposit, then pack blast furnace ironmaking into,Hexavalent chrome reduction is become to crome metal. Although the method has solved the problem of the environmental pollution of vanadium chromium slag utilization, to vanadium whereinChromium resource fails to carry out effective recycling, but along with ironmaking flow process enter in steel, concerning some steel grade, vanadium chromium not only withoutBenefit is harmful on the contrary, and sintering-blast furnace smelting process itself is also highly energy-consuming, expensive flow process, and economic benefit is also bad.
(3) sulfuric acid slaking method
Taking vanadium chromium slag as raw material, add water, sulfuric acid etc., through reaction, slaking, filtration, Vacuum Concentration, drying and other steps preparationChromium sulfate. The subject matter of this technique is that acid consumption is large, wastewater treatment capacity, and production cost is high, and has only recycled vanadium chromiumIn chromium resource.
(4) sub-molten salt method
By Chinese Academy of Sciences's process the vanadium slag sub-molten salt method developed jointly with Hebei steel enterprise Cheng Gang company extract vanadium chromium technology, reactionProcess is mainly liquid-solid reaction, realizes efficient oxidation, conversion and the dissolving of vanadium chromium. The subject matter of the method be equipment requirementHeight, vanadium chromium is oxidized jointly, fails vanadium chromium to carry out effective separating treatment.
(5) sodium roasting-water seaoning
Publication number be CN103614566 Patent Application Publication a kind of method of extracting vanadium and chromium from converter vanadium chromium slag, and toolBody discloses sodium roasting-water seaoning, but method disclosed by the invention studies as basis taking synthetic slag, for processThe vanadium chromium slag that oxidation blows out, vanadium chromium slag thing is more complicated mutually, and intractability is larger, and the present invention adopts and blows through peroxidatingThe vanadium chromium slag that refining obtains is raw material, and raw material is more representative, higher with actual industrial production conjugation, and the present invention adopts first calciumChange baking acid immersion and extract vanadium resource, chromium resource is extracted in rear sodium roasting-water logging, has essential distinction with the technology of the present invention technique.
In sum, the domestic method that vanadium chromium slag is processed all can not effectively separate vanadium chromium in vanadium chromium slag utilize,Limit the practical application of the whole bag of tricks, along with the further exploitation of v-ti magnetite ore resources, in the urgent need to a kind of vanadium chromium slagSeparate the method for vanadium chromium.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of method that reclaims vanadium chromium resource.
The present invention reclaims the method for vanadium chromium resource, comprises the steps:
A, vanadium chromium slag is mixed with calcium carbonate, obtain mixed once material, by the oxidizing roasting of mixed once material, obtain bakes to burn the articleGrog;
B, bakes to burn the article grog is carried out to acidleach, obtain pickle liquor and acid leaching residue;
C, by acid leaching residue dry, grind after with sodium carbonate be mixed to get secondary mixture material, by the oxidizing roasting of secondary mixture material, mustTo after baking grog;
D, after baking grog is carried out to water logging, obtain infusion and water logging slag;
E, from pickle liquor, infusion and water logging slag, separation and Extraction goes out vanadium, chromium and iron respectively.
The present invention reclaims the method flow diagram of vanadium chromium resource and sees Fig. 1.
Wherein, TFe31.5~42.5wt% in vanadium chromium slag of the present invention, V2O510.96~13.35wt%,Cr2O39~11.66wt%;In order to improve raw material availability, also improve the rate of recovery of vanadium chromium resource of the present invention simultaneously, in vanadium chromium slag ,-120 order granularity content existMore than 80wt%, more than in vanadium chromium slag, granularity is less than the 80wt% that 120 object materials account for whole vanadium chromium slag weight.
Further, in order to improve in the present invention the rate of recovery of vanadium resource in vanadium chromium, in a step mixed once material be preferable over 950~Oxidizing roasting 3~4h at 1150 DEG C; V in calcium carbonate and vanadium chromium slag2O5Mass ratio be preferably, CaCO3:V2O5=1.0~1.4:1。
Further, in order to improve the rate of recovery of the vanadium resource of vanadium chromium slag in the present invention, in b step acidleach temperature be preferably 40~60 DEG C, more preferably 50 DEG C; Leaching time is 60~80min preferably, and pickle liquor pH value is preferably 2~3, bakes to burn the article grogBe preferably 1:5~7g/ml with the solid-to-liquid ratio of pickle liquor.
Further, in order to improve in the present invention the rate of recovery of chromium resource in acid leaching residue, in c step, secondary mixture material is preferable overOxidizing roasting 2~3h at 1050~1150 DEG C; In acid leaching residue ,-120 order granularity content are preferably more than 80wt%; Sodium carbonate and acidSoak Cr in slag2O3Mass ratio be preferably, Na2CO3:Cr2O3=2.8~3.5:1。
Further, in order to improve in the present invention the rate of recovery of chromium resource in acid leaching residue, in d step water soaking temperature be preferably 60~80 DEG C, the water logging time is preferably 60~80min, and the solid-to-liquid ratio of after baking grog and water is preferably 1:5~7g/ml.
Beneficial effect of the present invention:
1. adopting the inventive method to reclaim vanadium chromium resource can separate vanadium chromium in vanadium chromium slag effectively, obtains extracting vanadium, chromiumRaw material, realized the comprehensive utilization of vanadium chromium slag, there is the advantages such as technique is simple, equipment requirement is low, and environmental pollution is little.
2. in the recovery method of vanadium chromium resource of the present invention, in vanadium chromium slag, to enter the rate of recovery of infusion be 80~90% to vanadium, and chromium entersThe rate of recovery of infusion is 70~80%, and vanadium, chromium recovery ratio are higher.
3, the present invention not only adapts to and the recovery that separates of vanadium chromium resource in vanadium chromium slag, is also applicable to vanadium chromium in high-chromic vanadium-titanium ferroferriteThe separation of slag is recycled, and has improved the comprehensive utilization ratio of high-chromic vanadium-titanium ferroferrite.
Brief description of the drawings
Fig. 1 the present invention reclaims the method flow diagram of vanadium chromium resource.
Detailed description of the invention
The present invention reclaims the method for vanadium chromium resource, comprises the steps:
A, vanadium chromium slag is mixed with calcium carbonate, obtain mixed once material, by the oxidizing roasting of mixed once material, obtain bakes to burn the articleGrog;
B, bakes to burn the article grog is carried out to acidleach, obtain pickle liquor and acid leaching residue;
C, by acid leaching residue dry, grind after with sodium carbonate be mixed to get secondary mixture material, by the oxidizing roasting of secondary mixture material, mustTo after baking grog;
D, after baking grog is carried out to water logging, obtain infusion and water logging slag;
E, from pickle liquor, infusion and water logging slag, separation and Extraction goes out vanadium, chromium and iron respectively.
The present invention reclaims the method flow diagram of vanadium chromium resource and sees Fig. 1.
Wherein, TFe31.5~42.5wt% in vanadium chromium slag of the present invention, V2O510.96~13.35wt%,Cr2O39~11.66wt%;In order to improve raw material availability, also improve the rate of recovery of vanadium chromium resource of the present invention simultaneously, in vanadium chromium slag ,-120 order granularity content existMore than 80wt%, more than in vanadium chromium slag, granularity is less than the 80wt% that 120 object materials account for whole vanadium chromium slag weight.
Further, in order to improve in the present invention the rate of recovery of vanadium resource in vanadium chromium, in a step mixed once material be preferable over 950~Oxidizing roasting 3~4h at 1150 DEG C; V in calcium carbonate and vanadium chromium slag2O5Mass ratio be preferably, CaCO3:V2O5=1.0~1.4:1。
Further, in order to improve the rate of recovery of the vanadium resource of vanadium chromium slag in the present invention, in b step acidleach temperature be preferably 40~60 DEG C, more preferably 50 DEG C; Leaching time is 60~80min preferably, and pickle liquor pH value is preferably 2~3, bakes to burn the article grogBe preferably 1:5~7g/ml with the solid-to-liquid ratio of pickle liquor.
Further, in order to improve in the present invention the rate of recovery of chromium resource in acid leaching residue, in c step, secondary mixture material is preferable overOxidizing roasting 2~3h at 1050~1150 DEG C; In acid leaching residue ,-120 order granularity content are preferably more than 80wt%; Sodium carbonate and acidSoak Cr in slag2O3Mass ratio be preferably, Na2CO3:Cr2O3=2.8~3.5:1。
Further, in order to improve in the present invention the rate of recovery of chromium resource in acid leaching residue, in d step water soaking temperature be preferably 60~80 DEG C, the water logging time is preferably 60~80min, and the solid-to-liquid ratio of after baking grog and water is preferably 1:5~7g/ml.
Below in conjunction with embodiment, the specific embodiment of the present invention is further described, does not therefore limit the present invention to instituteAmong the scope of embodiments of stating.
The method that embodiment 1 adopts the present invention to reclaim vanadium chromium resource reclaims vanadium chromium slag
A, vanadium chromium slag is mixed with calcium carbonate, obtain mixed once material, by mixed once material oxidizing roasting 4h at 950 DEG C,Obtain bakes to burn the article grog; Wherein, V in calcium carbonate and vanadium chromium slag2O5Mass ratio be, CaCO3:V2O5=1:1。
B, bakes to burn the article grog is soaked to 60min in the pickle liquor that 40 DEG C, pH value are 2, filter, obtain pickle liquor and acidleachSlag; Wherein, the solid-to-liquid ratio 1:7g/ml of bakes to burn the article grog and pickle liquor;
C, acid leaching residue is dried, ground, make in dry acid leaching residue-120 order granularity content more than 80wt%, then with carbonAcid sodium mixes, and obtains secondary mixture material, by secondary mixture material oxidizing roasting 2h at 1050 DEG C, obtains after baking grog;Wherein, Cr in sodium carbonate and acid leaching residue2O3Mass ratio be, Na2CO3:Cr2O3=2.8:1;
D, after baking grog is soaked to 60min in 80 DEG C of water, filter, obtain infusion and water logging slag; Wherein, secondary roastingThe solid-to-liquid ratio of overburnt material and water is 1:5g/ml;
E, from pickle liquor, infusion and water logging slag, separation and Extraction goes out vanadium, chromium and iron respectively.
Wherein, vanadium chromium slag ingredient is: TFe31.5%, V2O510.96%,Cr2O310.66%; Granularity is that < 120 orders account for total material80wt%.
After measured, the rate of recovery that vanadium enters pickle liquor is 85%, and the rate of recovery of chromium in acid leaching residue is about 90%, and chromium enters water loggingThe rate of recovery of liquid is 70%.
The method that embodiment 2 adopts the present invention to reclaim vanadium chromium resource reclaims vanadium chromium slag
A, vanadium chromium slag is mixed with calcium carbonate, obtain mixed once material, by mixed once material oxidizing roasting 3h at 1050 DEG C,Obtain bakes to burn the article grog; Wherein, V in calcium carbonate and vanadium chromium slag2O5Mass ratio be, CaCO3:V2O5=1.2:1。
B, bakes to burn the article grog is soaked to 60min in the pickle liquor that 50 DEG C, pH value are 2.5, filter, obtain pickle liquor and acidSoak slag; Wherein, the solid-to-liquid ratio 1:6g/ml of bakes to burn the article grog and pickle liquor;
C, acid leaching residue is dried, ground, make in dry acid leaching residue-120 order granularity content more than 80wt%, then with carbonAcid sodium mixes, and obtains secondary mixture material, by secondary mixture material oxidizing roasting 3h at 1100 DEG C, obtains after baking grog;Wherein, Cr in sodium carbonate and acid leaching residue2O3Mass ratio be, Na2CO3:Cr2O3=3:1;
D, after baking grog is soaked to 80min in 60 DEG C of water, filter, obtain infusion and water logging slag; Wherein, secondary roastingThe solid-to-liquid ratio of overburnt material and water is 1:6g/ml;
E, from pickle liquor, infusion and water logging slag, separation and Extraction goes out vanadium, chromium and iron respectively.
Wherein, vanadium chromium slag ingredient is: TFe38%, V2O512.05%,Cr2O39.86%; Granularity is that < 120 orders account for total material80wt%。
After measured, the rate of recovery that vanadium enters pickle liquor is 90%, and the rate of recovery of chromium in acid leaching residue is about 94%, and chromium enters water loggingThe rate of recovery of liquid is 75%.
The method that embodiment 3 adopts the present invention to reclaim vanadium chromium resource reclaims vanadium chromium slag
A, vanadium chromium slag is mixed with calcium carbonate, obtain mixed once material, by mixed once material oxidizing roasting 4h at 1150 DEG C,Obtain bakes to burn the article grog; Wherein, V in calcium carbonate and vanadium chromium slag2O5Mass ratio be, CaCO3:V2O5=1.3:1。
B, bakes to burn the article grog is soaked to 80min in the pickle liquor that 50 DEG C, pH value are 3, filter, obtain pickle liquor and acidleachSlag; Wherein, the solid-to-liquid ratio 1:6g/ml of bakes to burn the article grog and pickle liquor;
C, acid leaching residue is dried, ground, make in dry acid leaching residue-120 order granularity content more than 80wt%, then with carbonAcid sodium mixes, and obtains secondary mixture material, by secondary mixture material oxidizing roasting 3h at 1150 DEG C, obtains after baking grog;Wherein, Cr in sodium carbonate and acid leaching residue2O3Mass ratio be, Na2CO3:Cr2O3=3.5:1;
D, after baking grog is soaked to 50min in 80 DEG C of water, filter, obtain infusion and water logging slag; Wherein, secondary roastingThe solid-to-liquid ratio of overburnt material and water is 1:7g/ml;
E, from pickle liquor, infusion and water logging slag, separation and Extraction goes out vanadium, chromium and iron respectively.
Wherein, vanadium chromium slag ingredient is: TFe42.5%, V2O513.5%,Cr2O311.66%; Granularity is that < 120 orders account for total material80wt%.
After measured, the rate of recovery that vanadium enters pickle liquor is 90%, and the rate of recovery of chromium in acid leaching residue is about 95%, and chromium enters water loggingThe rate of recovery of liquid is 80%.

Claims (17)

1. the method that reclaims vanadium chromium resource, is characterized in that, comprises the steps:
A, vanadium chromium slag is mixed with calcium carbonate, obtain mixed once material, by the oxidizing roasting of mixed once material, obtain bakes to burn the articleGrog; Wherein, TFe31.5~42.5wt% in described vanadium chromium slag, V2O510.96~13.35wt%,Cr2O39~11.66wt%;
B, bakes to burn the article grog is carried out to acidleach, obtain pickle liquor and acid leaching residue;
C, by acid leaching residue dry, grind after with sodium carbonate be mixed to get secondary mixture material, by the oxidizing roasting of secondary mixture material, mustTo after baking grog;
D, after baking grog is carried out to water logging, obtain infusion and water logging slag;
E, from pickle liquor, infusion and water logging slag, separation and Extraction goes out vanadium, chromium and iron respectively.
2. the method for recovery vanadium chromium resource according to claim 1, is characterized in that: in vanadium chromium slag ,-120 order granularities containAmount is more than 80wt%.
3. the method for recovery vanadium chromium resource according to claim 1 and 2, is characterized in that: once mixed in described a stepCompound material is oxidizing roasting 3~4h at 950~1150 DEG C; V in calcium carbonate and vanadium chromium slag2O5Mass ratio be, CaCO3:V2O5=1.0~1.4:1。
4. the method for recovery vanadium chromium resource according to claim 1 and 2, is characterized in that: acidleach temperature in described b stepDegree is 40~60 DEG C, leaching time 60~80min, and pickle liquor pH value is 2~3, the solid-liquid of bakes to burn the article grog and pickle liquorThan being 1:5~7g/ml.
5. the method for recovery vanadium chromium resource according to claim 3, is characterized in that: in described b step, acidleach temperature is40~60 DEG C, leaching time 60~80min, pickle liquor pH value is 2~3, the solid-to-liquid ratio of bakes to burn the article grog and pickle liquor is1:5~7g/ml。
6. the method for recovery vanadium chromium resource according to claim 1 and 2, is characterized in that: in described c step, secondary is mixedCompound material is oxidizing roasting 2~3h at 1050~1150 DEG C; In acid leaching residue ,-120 order granularity content are more than 80wt%; Sodium carbonateWith Cr in acid leaching residue2O3Mass ratio be, Na2CO3:Cr2O3=2.8~3.5:1。
7. the method for recovery vanadium chromium resource according to claim 3, is characterized in that: secondary mixture in described c stepExpect oxidizing roasting 2~3h at 1050~1150 DEG C; In acid leaching residue ,-120 order granularity content are more than 80wt%; Sodium carbonate and acidSoak Cr in slag2O3Mass ratio be, Na2CO3:Cr2O3=2.8~3.5:1。
8. the method for recovery vanadium chromium resource according to claim 4, is characterized in that: secondary mixture in described c stepExpect oxidizing roasting 2~3h at 1050~1150 DEG C; In acid leaching residue ,-120 order granularity content are more than 80wt%; Sodium carbonate and acidSoak Cr in slag2O3Mass ratio be, Na2CO3:Cr2O3=2.8~3.5:1。
9. the method for recovery vanadium chromium resource according to claim 5, is characterized in that: secondary mixture in described c stepExpect oxidizing roasting 2~3h at 1050~1150 DEG C; In acid leaching residue ,-120 order granularity content are more than 80wt%; Sodium carbonate and acidSoak Cr in slag2O3Mass ratio be, Na2CO3:Cr2O3=2.8~3.5:1。
10. the method for recovery vanadium chromium resource according to claim 1 and 2, is characterized in that: water logging in described d stepTemperature is 60~80 DEG C, and the water logging time is 60~80min, and the solid-to-liquid ratio of after baking grog and water is 1:5~7g/ml.
The method of 11. recovery vanadium chromium resources according to claim 3, is characterized in that: water soaking temperature in described d stepBe 60~80 DEG C, the water logging time is 60~80min, and the solid-to-liquid ratio of after baking grog and water is 1:5~7g/ml.
The method of 12. recovery vanadium chromium resources according to claim 4, is characterized in that: water soaking temperature in described d stepBe 60~80 DEG C, the water logging time is 60~80min, and the solid-to-liquid ratio of after baking grog and water is 1:5~7g/ml.
The method of 13. recovery vanadium chromium resources according to claim 5, is characterized in that: water soaking temperature in described d stepBe 60~80 DEG C, the water logging time is 60~80min, and the solid-to-liquid ratio of after baking grog and water is 1:5~7g/ml.
The method of 14. recovery vanadium chromium resources according to claim 6, is characterized in that: water soaking temperature in described d stepBe 60~80 DEG C, the water logging time is 60~80min, and the solid-to-liquid ratio of after baking grog and water is 1:5~7g/ml.
The method of 15. recovery vanadium chromium resources according to claim 7, is characterized in that: water soaking temperature in described d stepBe 60~80 DEG C, the water logging time is 60~80min, and the solid-to-liquid ratio of after baking grog and water is 1:5~7g/ml.
The method of 16. recovery vanadium chromium resources according to claim 8, is characterized in that: water soaking temperature in described d stepBe 60~80 DEG C, the water logging time is 60~80min, and the solid-to-liquid ratio of after baking grog and water is 1:5~7g/ml.
The method of 17. recovery vanadium chromium resources according to claim 9, is characterized in that: water soaking temperature in described d stepBe 60~80 DEG C, the water logging time is 60~80min, and the solid-to-liquid ratio of after baking grog and water is 1:5~7g/ml.
CN201410175785.6A 2014-04-28 2014-04-28 Reclaim the method for vanadium chromium resource CN103924096B (en)

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