CN110172596A - The method of vanadium is recycled from underflow slag with chlorination technique - Google Patents
The method of vanadium is recycled from underflow slag with chlorination technique Download PDFInfo
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- CN110172596A CN110172596A CN201910596991.7A CN201910596991A CN110172596A CN 110172596 A CN110172596 A CN 110172596A CN 201910596991 A CN201910596991 A CN 201910596991A CN 110172596 A CN110172596 A CN 110172596A
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- vanadium
- slag
- underflow slag
- fused salt
- recycling
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Classifications
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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
-
- 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
- C22B7/001—Dry processes
- C22B7/002—Dry processes by treating with halogens, sulfur or compounds thereof; by carburising, by treating with hydrogen (hydriding)
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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
Abstract
The invention discloses a kind of methods for recycling vanadium from underflow slag with chlorination technique, the following steps are included: using alkali metal chloride as fused salt, after fused salt is melted in heating, underflow slag and reducing agent is added, chlorine is passed through into fused salt simultaneously and carries out fused salt chlorimation reaction, the vanadium oxytrichloride that reaction is generated, which condenses, to be collected, and vanadium oxytrichloride crude product is obtained；It will react to obtain vanadic anhydride with water after vanadium oxytrichloride crude product rectifying.The present invention recycles the vanadium in underflow slag by fused salt chlorimation technology, has many advantages, such as that process is short, vanadium recovery is high, at low cost, vanadic anhydride product purity is high.
Description
Technical field
The invention belongs to vanadium extractive technique fields, and in particular to a kind of side for recycling vanadium from underflow slag with chlorination technique
Method.
Background technique
Currently, Leaching of Vanadium from Vanadium slag industrialization production is mainly sodium roasting technique, converted vanadium to by sodium roasting solvable
Property vanadate, then vanadium is extracted into solution by water logging and further prepares vanadium product.However, phosphorus, silicon during sodium roasting
Equal impurity elements also form soluble compound with sodium salt, and enter in vanadium leachate.It is received to improve vanadium leachate precipitation
Rate simultaneously obtains qualified vanadium product, it is necessary to clean to leachate.Leachate generallys use calcium chloride solution when removing silicon and phosphorus
And aluminum sulfate solution, dedoping step vanadium can form sediment with calcium or aluminium, in the underflow slag after entering removal of impurities, content of vanadium is logical
Chang Keda 10~20%.In order to improve the vanadium recovery of Leaching of Vanadium from Vanadium slag, vanadium is recycled from underflow slag and is had great importance.
CN103911521A discloses a kind of method that vanadium is recycled from dephosphorization underflow slag, and the method includes following steps
It is rapid: A, to leach dephosphorization underflow slag with oxalate solution, obtain alkalinity containing vanadium leachate；B, the alkalinity is adjusted containing vanadium leachate
PH value is 8~11, carries out precipitation processing later, obtains ammonium metavanadate.
CN102719672A discloses a kind of method and wet process process for extracting vanadium for handling vanadium wastewater underflow slag.The method
Comprising steps of vanadium wastewater underflow slag is mixed with alkaline vanadium liquid, mixed liquor is formed；Removal of impurities processing is carried out to the mixed liquor；
Mixed liquor of the filtering through removal of impurities processing, obtains filtrate containing vanadium.
Above-mentioned patent is how disclosure uses chlorination technique to recycle vanadium from underflow slag.
Summary of the invention
The purpose of the present invention is to provide a kind of methods for recycling vanadium from underflow slag with chlorination technique.
A method of vanadium is recycled from underflow slag with chlorination technique, comprising the following steps:
Using alkali metal chloride as fused salt, after fused salt is melted in heating, it is added underflow slag and reducing agent, while to fused salt
In be passed through chlorine carry out fused salt chlorimation reaction, will reaction generate vanadium oxytrichloride condense collect, obtain vanadium oxytrichloride crude product；By three
It reacts to obtain vanadic anhydride with water after chlorine vanadyl crude product rectifying.
Wherein, the above-mentioned method for recycling vanadium from underflow slag with chlorination technique, the underflow slag are in sodium process for extracting vanadium
The high silicon slag of high phosphorus obtained after being cleaned to the leachate that vanadium slag is obtained through sodium roasting and water logging using calcium chloride or aluminum sulfate.
Wherein, the above-mentioned method for recycling vanadium from underflow slag with chlorination technique, by weight percentage, in the underflow slag
Including V10~20%, Ca10~20%, Al2~12%, Si2~12%, P0.5~3.5%, Fe3~12%, Mg0.5~
2.5%, Mn2~8%.
Wherein, the above-mentioned method for recycling vanadium from underflow slag with chlorination technique, the alkali metal chloride be sodium chloride and/
Or potassium chloride.
Wherein, the above-mentioned method for recycling vanadium from underflow slag with chlorination technique, the alkali metal are sodium chloride and potassium chloride.
Wherein, the above-mentioned method for recycling vanadium from underflow slag with chlorination technique, sodium chloride and potassium chloride in the alkali metal
Weight ratio be 15~25:5~15.
Wherein, the above-mentioned method for recycling vanadium from underflow slag with chlorination technique, the reducing agent be selected from graphite, active carbon,
At least one of coke, coal dust, petroleum coke.
Wherein, the above-mentioned method for recycling vanadium from underflow slag with chlorination technique, the alkali metal chloride, are gone back underflow slag
The weight ratio of former agent and chlorine is 30:1:0.3~0.45:2~5.
Wherein, the temperature of the above-mentioned method for recycling vanadium from underflow slag with chlorination technique, the fused salt chlorimation reaction is 450
~1200 DEG C, the reaction time is 90~150min.
Wherein, the above-mentioned method for recycling vanadium from underflow slag with chlorination technique, the temperature of the condensation are 127 ± 3 DEG C；Institute
The temperature for stating rectifying is 150~200 DEG C.
The beneficial effects of the present invention are:
The present invention by fused salt chlorimation technology recycle underflow slag in vanadium, have process is short, vanadium recovery is high, it is at low cost,
The advantages that vanadic anhydride product purity is high.And calcium in underflow slag, phosphorus can be overcome etc. impurity bring general extraction methods extract
The problems such as rate is low, purifying products are difficult, long flow path.
Specific embodiment
Specifically, a kind of method for recycling vanadium from underflow slag with chlorination technique, comprising the following steps:
Using alkali metal chloride as fused salt, after fused salt is melted in heating, it is added underflow slag and reducing agent, while to fused salt
In be passed through chlorine carry out fused salt chlorimation reaction, will reaction generate vanadium oxytrichloride condense collect, obtain vanadium oxytrichloride crude product；By three
It reacts to obtain vanadic anhydride with water after chlorine vanadyl crude product rectifying.
In the method for the present invention, underflow slag is the leachate obtained to vanadium slag through sodium roasting and water logging in sodium process for extracting vanadium
Using the high silicon slag of high phosphorus obtained after calcium chloride or aluminum sulfate removal of impurities.Specifically, by weight percentage, being wrapped in the underflow slag
Include V10~20%, Ca10~20%, Al2~12%, Si2~12%, P0.5~3.5%, Fe3~12%, Mg0.5~
2.5%, Mn2~8%.
In the method for the present invention, alkali metal chloride is sodium chloride and/or potassium chloride；Preferably, the alkali metal is chlorination
Sodium and potassium chloride；It is furthermore preferred that the weight ratio of sodium chloride and potassium chloride is 15~25:5~15 in the alkali metal.
Reducing agent is selected from least one of graphite, active carbon, coke, coal dust, petroleum coke.
In the method for the present invention, the alkali metal chloride, underflow slag, reducing agent and chlorine weight ratio be 30:1:0.3~
0.45:2~5.
In the method for the present invention, the temperature of fused salt chlorimation reaction is 450~1200 DEG C, the reaction time is 90~
150min。
In the method for the present invention, although underflow slag generates different types of chloride after fused salt chlorimation is reacted, by
Widely different in the various chloride boiling points of generation, the present invention is by control condensation temperature, so that the mainly trichlorine being collected into
Vanadyl, specifically, condensation temperature is 127 ± 3 DEG C.It condenses and mainly contains vanadium oxytrichloride in the vanadium oxytrichloride crude product being collected into and lack
Measure solid dust, after rectifying, so that it may the vanadium oxytrichloride purified, specifically, the temperature of the rectifying be 150~
200℃。
A specific embodiment of the invention is further described below with reference to embodiment, is not therefore limited the present invention
System is among the embodiment described range.
Embodiment 1
Solid sodium chloride 20Kg and potassium chloride 10Kg is added into Molten salt chlorination furnace, is heated to 700 DEG C and melts solid fused salt
Change, is added in liquid fused salt and reacts after then mixing 1Kg underflow slag with 50g petroleum coke, 400g graphite, while into fused salt
It is passed through chlorine 4000g, fused salt chlorimation reaction temperature is 950~1200 DEG C, reaction time 120min.Fused salt chlorimation is reacted and is given birth to
At vanadium oxytrichloride collected in 127 DEG C of condensations, obtain vanadium oxytrichloride crude product, other chlorides by gather dust collection after with chlorination
Tailings merging treatment.
Vanadium oxytrichloride crude product is subjected to rectifying at 150 DEG C, impurity and solid slag therein is removed, is then stirring it
It is slowly added under the conditions of mixing in 5L water, controls 60 DEG C of reaction temperature <, obtain vanadic anhydride precipitating, distilled water is used in filtering
With liquid-solid ratio 1:1 washing, vanadic anhydride product is obtained after dry, meets Industry code requirements, whole process vanadium yield 96%.
Embodiment 2
Solid sodium chloride 15Kg and potassium chloride 15Kg is added into Molten salt chlorination furnace, is heated to 800 DEG C and melts solid fused salt
Change, then will be added in liquid fused salt after 1Kg underflow slag and 100g coal dust, the mixing of 200g petroleum coke and react, while to fused salt
In be passed through chlorine 5000g, fused salt chlorimation reaction temperature is 650~900 DEG C, reaction time 150min.Fused salt chlorimation is reacted
The vanadium oxytrichloride of generation is collected in 127 DEG C of condensations, obtains vanadium oxytrichloride crude product, other chlorides by gather dust collection after with chlorine
Change tailings merging treatment.
Vanadium oxytrichloride crude product is subjected to rectifying at 200 DEG C, impurity and solid slag therein is removed, is then stirring it
It is slowly added under the conditions of mixing in 5L water, controls 80 DEG C of reaction temperature <, obtain vanadic anhydride precipitating, distilled water is used in filtering
With liquid-solid ratio 2:1 washing, vanadic anhydride product is obtained after dry and meets Industry code requirements, whole process vanadium yield 92%.
Embodiment 3
Solid sodium chloride 25Kg and potassium chloride 5Kg is added into Molten salt chlorination furnace, is heated to 750 DEG C and melts solid fused salt
Change, then 1Kg underflow slag and 200g active carbon, 200g petroleum coke are added in liquid fused salt after mixing and are reacted, while to melting
Chlorine 2000g is passed through in salt, fused salt chlorimation reaction temperature is 450~900 DEG C, reaction time 90min.Fused salt chlorimation is reacted
The vanadium oxytrichloride of generation is collected in 127 DEG C of condensations, obtains vanadium oxytrichloride crude product, other chlorides by gather dust collection after with chlorine
Change tailings merging treatment.
Vanadium oxytrichloride crude product is subjected to rectifying at 180 DEG C, impurity and solid slag therein is removed, is then stirring it
It is slowly added under the conditions of mixing in 5L water, controls 50 DEG C of reaction temperature <, obtain vanadic anhydride precipitating, distilled water is used in filtering
With liquid-solid ratio 1.5:1 washing, vanadic anhydride product is obtained after dry and meets Industry code requirements, whole process vanadium yield 93%.
Comparative example 1
Solid sodium chloride 5Kg and potassium chloride 5Kg is added into Molten salt chlorination furnace, is heated to 750 DEG C and melts solid fused salt,
Then it is added in liquid fused salt and reacts after 1Kg underflow slag being mixed with 100g active carbon, 100g petroleum coke, while into fused salt
It is passed through chlorine 2000g, fused salt chlorimation reaction temperature is 700 DEG C, reaction time 90min.Three that fused salt chlorimation reaction is generated
Chlorine vanadyl is collected in 127 DEG C of condensations, obtains vanadium oxytrichloride crude product, other chlorides after collection of gathering dust with chlorination tailings by closing
And it handles.
Vanadium oxytrichloride crude product is subjected to rectifying at 200 DEG C, impurity and solid slag therein is removed, is then stirring it
It is slowly added under the conditions of mixing in 5L water, controls 50 DEG C of reaction temperature <, obtain vanadic anhydride precipitating, distilled water is used in filtering
With liquid-solid ratio 1.5:1 washing, vanadic anhydride product is obtained after dry and meets Industry code requirements, whole process vanadium yield 73%.
Claims (10)
1. the method for vanadium is recycled from underflow slag with chlorination technique, which comprises the following steps:
Using alkali metal chloride as fused salt, after fused salt is melted in heating, underflow slag and reducing agent is added, while leading into fused salt
Enter chlorine and carry out fused salt chlorimation reaction, the vanadium oxytrichloride that reaction is generated, which condenses, to be collected, and vanadium oxytrichloride crude product is obtained；By trichlorine oxygen
It reacts to obtain vanadic anhydride with water after vanadium crude product rectifying.
2. recycling the method for vanadium from underflow slag with chlorination technique according to claim 1, which is characterized in that the underflow slag
It is to be obtained after being cleaned to the leachate that vanadium slag is obtained through sodium roasting and water logging using calcium chloride or aluminum sulfate in sodium process for extracting vanadium
The high silicon slag of the high phosphorus arrived.
3. recycling the method for vanadium from underflow slag with chlorination technique according to claim 2, which is characterized in that with weight percent
It include V 10~20% in the underflow slag than meter, Ca 10~20%, Al 2~12%, Si 2~12%, P 0.5~
3.5%, Fe 3~12%, Mg 0.5~2.5%, Mn 2~8%.
4. recycling the method for vanadium from underflow slag with chlorination technique according to claim 1, which is characterized in that the alkali metal
Chloride is sodium chloride and/or potassium chloride.
5. recycling the method for vanadium from underflow slag with chlorination technique according to claim 4, which is characterized in that the alkali metal
For sodium chloride and potassium chloride.
6. the method according to claim 4 or 5 for recycling vanadium from underflow slag with chlorination technique, which is characterized in that the alkali
The weight ratio of sodium chloride and potassium chloride is 15~25:5~15 in metal.
7. recycling the method for vanadium from underflow slag with chlorination technique according to claim 1, which is characterized in that the reducing agent
Selected from least one of graphite, active carbon, coke, coal dust, petroleum coke.
8. recycling the method for vanadium from underflow slag with chlorination technique according to claim 1, which is characterized in that the alkali metal
Chloride, underflow slag, reducing agent and chlorine weight ratio be 30:1:0.3~0.45:2~5.
9. recycling the method for vanadium from underflow slag with chlorination technique according to claim 1, which is characterized in that the fused salt chlorine
The temperature for changing reaction is 450~1200 DEG C, and the reaction time is 90~150min.
10. recycling the method for vanadium from underflow slag with chlorination technique according to claim 1, which is characterized in that the condensation
Temperature be 127 ± 3 DEG C；The temperature of the rectifying is 150~200 DEG C.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110643837A (en) * | 2019-10-30 | 2020-01-03 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for extracting vanadium from blast furnace slag by chlorination |
| CN110643825A (en) * | 2019-10-30 | 2020-01-03 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for extracting vanadium from blast furnace slag by boiling chlorination |
| CN110642294A (en) * | 2019-10-30 | 2020-01-03 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for preparing vanadium oxychloride from blast furnace slag through low-temperature chlorination |
| CN111286632A (en) * | 2020-03-31 | 2020-06-16 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for recovering vanadium from alkaline vanadium liquid dephosphorization residues |
| CN112142107A (en) * | 2020-09-29 | 2020-12-29 | 攀钢集团研究院有限公司 | Method for preparing high-purity vanadium oxychloride from vanadium-containing refined tailings |
| CN112410569A (en) * | 2020-10-30 | 2021-02-26 | 攀钢集团研究院有限公司 | Method for recovering vanadium from acidic vanadium-containing underflow slag |
| CN112708773A (en) * | 2020-12-23 | 2021-04-27 | 青岛惠城环保科技股份有限公司 | Treatment method of petroleum coke hydrogen production ash |
| CN114606539A (en) * | 2022-01-18 | 2022-06-10 | 河钢承德钒钛新材料有限公司 | Preparation method of vanadium chloride molten salt |
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| CN110643837A (en) * | 2019-10-30 | 2020-01-03 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for extracting vanadium from blast furnace slag by chlorination |
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| CN112410569A (en) * | 2020-10-30 | 2021-02-26 | 攀钢集团研究院有限公司 | Method for recovering vanadium from acidic vanadium-containing underflow slag |
| CN112708773A (en) * | 2020-12-23 | 2021-04-27 | 青岛惠城环保科技股份有限公司 | Treatment method of petroleum coke hydrogen production ash |
| CN112708773B (en) * | 2020-12-23 | 2023-04-07 | 青岛惠城环保科技集团股份有限公司 | Treatment method of petroleum coke hydrogen production ash |
| CN114606539A (en) * | 2022-01-18 | 2022-06-10 | 河钢承德钒钛新材料有限公司 | Preparation method of vanadium chloride molten salt |
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Application publication date: 20190827 |