CN103924096A - Method for recycling vanadium-chromium resources - Google Patents

Method for recycling vanadium-chromium resources Download PDF

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Publication number
CN103924096A
CN103924096A CN201410175785.6A CN201410175785A CN103924096A CN 103924096 A CN103924096 A CN 103924096A CN 201410175785 A CN201410175785 A CN 201410175785A CN 103924096 A CN103924096 A CN 103924096A
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vanadium
chromium
slag
vanadium chromium
acid leaching
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CN103924096B (en
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吴恩辉
李军
侯静
李强
黄平
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Jiaxing Lifutong New Material Technology Co ltd
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Panzhihua University
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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 invention relates to a method for recycling vanadium-chromium resources, belonging to the field of resource recycling. The invention aims at providing a method for recycling vanadium-chromium resources. The method for recycling vanadium-chromium resources comprises the following steps: a. mixing vanadium-chromium slag with calcium carbonate to obtain a primary mixture material, and oxidizing-roasting the primary mixture material to obtain a primary roasting clinker; b. performing acid leaching to the primary roasting clinker to obtain acid leaching liquor and acid leaching slag; c. drying acid leaching slag, grinding and mixing together with sodium carbonate to obtain a secondary mixture material, oxidizing-roasting the secondary mixture material to obtain secondary roasting clinker; d. performing water leaching to the secondary roasting clinker, to obtain water leaching liquor and water leaching slag; and e. respectively separating and extracting vanadium, chromium and iron from the acid leaching liquor, water leaching liquor and water leaching slag. The method for recycling vanadium-chromium resources has the advantages of being high in vanadium and chromium recycling rate, simple in technology, low in equipment requirement, less in environmental pollution and the like.

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 the vanadium content in raw ore 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 Vanadium Pentoxide in FLAKES, the rate of recovery of vanadium is more than 90%.The subject matter of alkaline leaching 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 the object of vanadium chromium comprehensive reutilization.
(2) sintering-blast-furnace smelting method
Vanadium leached-out chromium residue is mixed with a small amount of magnetic separation scum and coke, sinter into from molten type agglomerate, then pack blast furnace ironmaking into, hexavalent chrome reduction is become to chromium metal.Although the method has solved the problem of the environmental pollution of vanadium chromium slag utilization, but vanadium chromium resource is wherein failed to carry out effective recycling, but along with ironmaking flow process enters in steel, concerning some steel grade, vanadium chromium is not only unhelpful harmful on the contrary, and sintering-blast furnace smelting process itself is also highly energy-consuming, expensive flow process, economic benefit is also bad.
(3) sulfuric acid slaking method
Taking vanadium chromium slag as raw material, add water, sulfuric acid etc., prepare chromium sulphate through reaction, slaking, filtration, vacuum concentration, drying and other steps.The subject matter of this technique is that acid consumption is large, wastewater treatment capacity, and production cost is high, and has only recycled the chromium resource in vanadium chromium.
(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, reaction process is mainly liquid-solid reaction, realizes efficient oxidation, conversion and the dissolving of vanadium chromium.The subject matter of the method is that equipment requirements is higher, and 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 specifically disclose sodium roasting-water seaoning, but method disclosed by the invention is studied as basis taking synthetic slag, for the vanadium chromium slag that blows out through peroxidation, vanadium chromium slag thing is more complicated mutually, intractability is larger, it is raw material that the present invention adopts through the peroxidation vanadium chromium slag obtaining that blows, raw material is more representative, higher with actual industrial production conjugation, and the present invention adopts first calcification baking acid leaching extraction vanadium resource, chromium resource is extracted in rear sodium roasting-water logging, there is 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, separated the method for vanadium chromium in the urgent need to a kind of vanadium chromium slag.
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 article grog;
B, bakes to burn the article grog is carried out to acidleach, obtain pickling 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 re-baking grog;
D, re-baking grog is carried out to water logging, obtain infusion and water logging slag;
E, from pickling 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, V 2o 510.96～13.35wt%, Cr 2o 39～11.66wt%; 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 are more 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 is preferable over oxidizing roasting 3～4h at 950～1150 DEG C; V in calcium carbonate and vanadium chromium slag 2o 5mass ratio be preferably, CaCO 3: V 2o 5=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 is preferably 40～60 DEG C, more preferably 50 DEG C; Leaching time is 60～80min preferably, and pickling liquor pH value is preferably 2～3, and the solid-to-liquid ratio of bakes to burn the article grog and pickling liquor is preferably 1:5～7g/ml.
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 over oxidizing roasting 2～3h at 1050～1150 DEG C; In acid leaching residue ,-120 order granularity content are preferably more than 80wt%; Cr in sodium carbonate and acid leaching residue 2o 3mass ratio be preferably, Na 2cO 3: Cr 2o 3=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 is preferably 60～80 DEG C, and the water logging time is preferably 60～80min, and the solid-to-liquid ratio of re-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 the raw material of vanadium, chromium, has realized the comprehensive utilization of vanadium chromium slag, has the advantages such as technique is simple, equipment requirements 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 the rate of recovery that chromium enters infusion is 70～80%, and vanadium, chromium recovery ratio are higher.
3, the present invention not only adapt to vanadium chromium slag in the Separation and Recovery of vanadium chromium resource, be also applicable to the Separation and Recovery utilization of vanadium chromium slag in high-chromic vanadium-titanium ferroferrite, 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.
Embodiment
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 article grog;
B, bakes to burn the article grog is carried out to acidleach, obtain pickling 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 re-baking grog;
D, re-baking grog is carried out to water logging, obtain infusion and water logging slag;
E, from pickling 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, V 2o 510.96～13.35wt%, Cr 2o 39～11.66wt%; 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 are more 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 is preferable over oxidizing roasting 3～4h at 950～1150 DEG C; V in calcium carbonate and vanadium chromium slag 2o 5mass ratio be preferably, CaCO 3: V 2o 5=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 is preferably 40～60 DEG C, more preferably 50 DEG C; Leaching time is 60～80min preferably, and pickling liquor pH value is preferably 2～3, and the solid-to-liquid ratio of bakes to burn the article grog and pickling liquor is preferably 1:5～7g/ml.
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 over oxidizing roasting 2～3h at 1050～1150 DEG C; In acid leaching residue ,-120 order granularity content are preferably more than 80wt%; Cr in sodium carbonate and acid leaching residue 2o 3mass ratio be preferably, Na 2cO 3: Cr 2o 3=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 is preferably 60～80 DEG C, and the water logging time is preferably 60～80min, and the solid-to-liquid ratio of re-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 among described scope of embodiments.
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 slag 2o 5mass ratio be, CaCO 3: V 2o 5=1:1.
B, bakes to burn the article grog is soaked to 60min in the pickling liquor that 40 DEG C, pH value are 2, filter, obtain pickling liquor and acid leaching residue; Wherein, the solid-to-liquid ratio 1:7g/ml of bakes to burn the article grog and pickling liquor;
C, by acid leaching residue dry, grind ,-120 order granularity content in dry acid leaching residue, more than 80wt%, are then mixed with sodium carbonate, obtain secondary mixture material, by secondary mixture material oxidizing roasting 2h at 1050 DEG C, obtain re-baking grog; Wherein, Cr in sodium carbonate and acid leaching residue 2o 3mass ratio be, Na 2cO 3: Cr 2o 3=2.8:1;
D, re-baking grog is soaked to 60min in 80 DEG C of water, filter, obtain infusion and water logging slag; Wherein, the solid-to-liquid ratio of re-baking grog and water is 1:5g/ml;
E, from pickling liquor, infusion and water logging slag, separation and Extraction goes out vanadium, chromium and iron respectively.
Wherein, vanadium chromium slag ingredient is: TFe31.5%, V 2o 510.96%, Cr 2o 310.66%; Granularity is the 80wt% that < 120 orders account for total material.
After measured, the rate of recovery that vanadium enters pickling liquor is 85%, and the rate of recovery of chromium in acid leaching residue is about 90%, and the rate of recovery that chromium enters infusion 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 slag 2o 5mass ratio be, CaCO 3: V 2o 5=1.2:1.
B, bakes to burn the article grog is soaked to 60min in the pickling liquor that 50 DEG C, pH value are 2.5, filter, obtain pickling liquor and acid leaching residue; Wherein, the solid-to-liquid ratio 1:6g/ml of bakes to burn the article grog and pickling liquor;
C, by acid leaching residue dry, grind ,-120 order granularity content in dry acid leaching residue, more than 80wt%, are then mixed with sodium carbonate, obtain secondary mixture material, by secondary mixture material oxidizing roasting 3h at 1100 DEG C, obtain re-baking grog; Wherein, Cr in sodium carbonate and acid leaching residue 2o 3mass ratio be, Na 2cO 3: Cr 2o 3=3:1;
D, re-baking grog is soaked to 80min in 60 DEG C of water, filter, obtain infusion and water logging slag; Wherein, the solid-to-liquid ratio of re-baking grog and water is 1:6g/ml;
E, from pickling liquor, infusion and water logging slag, separation and Extraction goes out vanadium, chromium and iron respectively.
Wherein, vanadium chromium slag ingredient is: TFe38%, V 2o 512.05%, Cr 2o 39.86%; Granularity is the 80wt% that < 120 orders account for total material.
After measured, the rate of recovery that vanadium enters pickling liquor is 90%, and the rate of recovery of chromium in acid leaching residue is about 94%, and the rate of recovery that chromium enters infusion 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 slag 2o 5mass ratio be, CaCO 3: V 2o 5=1.3:1.
B, bakes to burn the article grog is soaked to 80min in the pickling liquor that 50 DEG C, pH value are 3, filter, obtain pickling liquor and acid leaching residue; Wherein, the solid-to-liquid ratio 1:6g/ml of bakes to burn the article grog and pickling liquor;
C, by acid leaching residue dry, grind ,-120 order granularity content in dry acid leaching residue, more than 80wt%, are then mixed with sodium carbonate, obtain secondary mixture material, by secondary mixture material oxidizing roasting 3h at 1150 DEG C, obtain re-baking grog; Wherein, Cr in sodium carbonate and acid leaching residue 2o 3mass ratio be, Na 2cO 3: Cr 2o 3=3.5:1;
D, re-baking grog is soaked to 50min in 80 DEG C of water, filter, obtain infusion and water logging slag; Wherein, the solid-to-liquid ratio of re-baking grog and water is 1:7g/ml;
E, from pickling liquor, infusion and water logging slag, separation and Extraction goes out vanadium, chromium and iron respectively.
Wherein, vanadium chromium slag ingredient is: TFe42.5%, V 2o 513.5%, Cr 2o 311.66%; Granularity is the 80wt% that < 120 orders account for total material.
After measured, the rate of recovery that vanadium enters pickling liquor is 90%, and the rate of recovery of chromium in acid leaching residue is about 95%, and the rate of recovery that chromium enters infusion is 80%.

Claims (6)

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 article grog;
B, bakes to burn the article grog is carried out to acidleach, obtain pickling 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 re-baking grog;
D, re-baking grog is carried out to water logging, obtain infusion and water logging slag;
E, from pickling 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: TFe31.5～42.5wt% in described vanadium chromium slag, V 2o 510.96～13.35wt%, Cr 2o 39～11.66wt%; In vanadium chromium slag ,-120 order granularity content are more than 80wt%.
3. the method for recovery vanadium chromium resource according to claim 1 and 2, is characterized in that: mixed once material oxidizing roasting 3～4h at 950～1150 DEG C in described a step; V in calcium carbonate and vanadium chromium slag 2o 5mass ratio be, CaCO 3: V 2o 5=1.0～1.4:1.
4. according to the method for the recovery vanadium chromium resource described in claim 1～3 any one, it is characterized in that: in described b step, acidleach temperature is 40～60 DEG C, leaching time 60～80min, pickling liquor pH value is 2～3, the solid-to-liquid ratio of bakes to burn the article grog and pickling liquor is 1:5～7g/ml.
5. according to the method for the recovery vanadium chromium resource described in claim 1～4 any one, it is characterized in that: secondary mixture material oxidizing roasting 2～3h at 1050～1150 DEG C in described c step; In acid leaching residue ,-120 order granularity content are more than 80wt%; Cr in sodium carbonate and acid leaching residue 2o 3mass ratio be, Na 2cO 3: Cr 2o 3=2.8～3.5:1.
6. according to the method for the recovery vanadium chromium resource described in claim 1～5 any one, it is characterized in that: in described d step, water soaking temperature is 60～80 DEG C, the water logging time is 60～80min, and the solid-to-liquid ratio of re-baking grog and water is 1:5～7g/ml.
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Cited By (13)

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CN104109758A (en) * 2014-07-21 2014-10-22 中国科学院过程工程研究所 Clean process method for extracting vanadium, chromium and iron from vanadium slag step by step
CN104152703A (en) * 2014-07-31 2014-11-19 攀钢集团攀枝花钢铁研究院有限公司 Method for separating and recovering vanadium and chromium from vanadium-chromium slag
CN104152704A (en) * 2014-07-31 2014-11-19 攀钢集团攀枝花钢铁研究院有限公司 Method for separating and recovering vanadium and chromium from vanadium-chromium slag
CN104178638A (en) * 2014-07-31 2014-12-03 攀钢集团攀枝花钢铁研究院有限公司 Method for separating and recycling vanadium and chromium from chromium vanadium reducing slag
CN104178637A (en) * 2014-07-31 2014-12-03 攀钢集团攀枝花钢铁研究院有限公司 Method for separating and recycling vanadium and chrome from vanadium-chrome slag
CN104451201A (en) * 2014-11-21 2015-03-25 长沙矿冶研究院有限责任公司 Two-grade curing vanadium extraction method for stone coal vanadium ores
CN104451202A (en) * 2014-11-21 2015-03-25 长沙矿冶研究院有限责任公司 Two-stage curing vanadium extraction method of stone coal vanadium ores
CN105734308A (en) * 2016-04-18 2016-07-06 东北大学 Vanadium leaching method for high-chrome vanadium residues
CN106065436A (en) * 2016-07-18 2016-11-02 江苏省冶金设计院有限公司 A kind of method and system processing vanadium slag
CN107502760A (en) * 2017-08-14 2017-12-22 攀钢集团钒业有限公司 Improve the process of vanadium slag yield
CN108531718A (en) * 2018-04-23 2018-09-14 东北大学 A method of producing chrome green using tailings in vanadium extraction
CN109055724A (en) * 2018-10-11 2018-12-21 攀钢集团钒钛资源股份有限公司 The method of vanadium and chromium is extracted from chrome alum mine/slag
CN109207728A (en) * 2017-07-07 2019-01-15 中国科学院过程工程研究所 A kind of method that high-temperature roasting method extracts chromium and vanadium from slag containing chrome alum

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CN104109758A (en) * 2014-07-21 2014-10-22 中国科学院过程工程研究所 Clean process method for extracting vanadium, chromium and iron from vanadium slag step by step
CN104152704B (en) * 2014-07-31 2016-04-13 攀钢集团攀枝花钢铁研究院有限公司 A kind of method of Separation and Recovery vanadium and chromium from vanadium chromium slag
CN104152704A (en) * 2014-07-31 2014-11-19 攀钢集团攀枝花钢铁研究院有限公司 Method for separating and recovering vanadium and chromium from vanadium-chromium slag
CN104178638A (en) * 2014-07-31 2014-12-03 攀钢集团攀枝花钢铁研究院有限公司 Method for separating and recycling vanadium and chromium from chromium vanadium reducing slag
CN104178637A (en) * 2014-07-31 2014-12-03 攀钢集团攀枝花钢铁研究院有限公司 Method for separating and recycling vanadium and chrome from vanadium-chrome slag
CN104152703A (en) * 2014-07-31 2014-11-19 攀钢集团攀枝花钢铁研究院有限公司 Method for separating and recovering vanadium and chromium from vanadium-chromium slag
CN104178638B (en) * 2014-07-31 2016-03-23 攀钢集团攀枝花钢铁研究院有限公司 A kind of method of Separation and Recovery vanadium and chromium from vanadium chromium reducing slag
CN104451201B (en) * 2014-11-21 2017-04-12 长沙矿冶研究院有限责任公司 Two-grade curing vanadium extraction method for stone coal vanadium ores
CN104451202A (en) * 2014-11-21 2015-03-25 长沙矿冶研究院有限责任公司 Two-stage curing vanadium extraction method of stone coal vanadium ores
CN104451201A (en) * 2014-11-21 2015-03-25 长沙矿冶研究院有限责任公司 Two-grade curing vanadium extraction method for stone coal vanadium ores
CN105734308A (en) * 2016-04-18 2016-07-06 东北大学 Vanadium leaching method for high-chrome vanadium residues
CN106065436A (en) * 2016-07-18 2016-11-02 江苏省冶金设计院有限公司 A kind of method and system processing vanadium slag
CN109207728A (en) * 2017-07-07 2019-01-15 中国科学院过程工程研究所 A kind of method that high-temperature roasting method extracts chromium and vanadium from slag containing chrome alum
CN107502760A (en) * 2017-08-14 2017-12-22 攀钢集团钒业有限公司 Improve the process of vanadium slag yield
CN108531718A (en) * 2018-04-23 2018-09-14 东北大学 A method of producing chrome green using tailings in vanadium extraction
CN109055724A (en) * 2018-10-11 2018-12-21 攀钢集团钒钛资源股份有限公司 The method of vanadium and chromium is extracted from chrome alum mine/slag

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