CN101418385A - Method for extracting vanadium pentoxide from vanadium-containing steel slag - Google Patents
Method for extracting vanadium pentoxide from vanadium-containing steel slag Download PDFInfo
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- CN101418385A CN101418385A CNA200810305929XA CN200810305929A CN101418385A CN 101418385 A CN101418385 A CN 101418385A CN A200810305929X A CNA200810305929X A CN A200810305929XA CN 200810305929 A CN200810305929 A CN 200810305929A CN 101418385 A CN101418385 A CN 101418385A
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- steel slag
- vanadium
- bearing steel
- flakes
- extraction
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- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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Abstract
The invention belongs to the technical field of vanadium-contained steel slag recovery and vanadium extraction, and provides a method for extracting vanadium pentoxide from the vanadium-contained steel slag with a higher recovery rate. The method comprises the following steps: a. immersing the vanadium-contained steel slag into sulphuric acid solution; b. adding iron powder into the leach solution obtained from step a, and regulating the pH value to 1.50 to 2.0 after reaction; c. extracting the solution obtained from step b with di(2-Ethylhexyl) phosphate with the concentration of 10 to 15 percent, and collecting the extract at the upper layer; d. extracting the solution obtained from step c with 2M to 3M of sulphuric acid, collecting the extract at the lower layer, regulating the pH value to 6.0 to 6.1, adding sodium chlorate which is 1.5 times of the total weight of the vanadium in the extract into the extract, and carrying out oxidation for 1 hour at 60 to 70 DEG C; and e. regulating the pH value of the solution obtained from step d to 2 to 2.1, and filtrating, washing and drying the solution after boiling to obtain vanadium. The vanadium product obtained by the method contains more than 65 percent of V2O5 and can be directly used for smelting vanadium iron.
Description
Technical field
The invention belongs to v-bearing steel slag and reclaim the vanadium extraction technical field, be specifically related to a kind of method of from v-bearing steel slag, extracting Vanadium Pentoxide in FLAKES.
Background technology
The utilization ratio of v-bearing steel slag China only 50% is bigger with the developed country gap.Treated construction material and the phosphate fertilizer such as metallurgical raw material, cement, roadbed material of can be used as of common slag.V-bearing steel slag contains V
2O
5Be 1～2%,, will cause the very big wasting of resources, the particularly loss of high added value element V if directly handle in the mode of handling common slag.Prior art method of vanadium extraction from v-bearing steel slag is mainly sodium-salt calcination one water logging technology, the molten vanadium extracting method of acidleach alkali and solvent extraction vanadium extracting method.First method energy consumption and sodium salt consumption are big, contaminate environment.The molten vanadium extracting method of acidleach alkali utilizes the acidleach v-bearing steel slag earlier, makes wherein vanadium with VO
2+, VO
2+Form leach, add the alkali neutralization, under weak basic condition, make vanadium become 5 valency ions (as VO with oxygenant
3 -, [H
2VO
4]
-), and make the impurity coprecipitations such as hydrous oxide of vanadium and iron, get thick vanadium with the alkali infuse again, thick vanadium is through the sodium salt of the molten generation 5 valency vanadium of alkali, and removes impurity silicon, and the back gets ammonium meta-vanadate with the precipitation of ammonium salt secondary, obtains V through roasting
2O
5The solvent extraction vanadium extracting method is to change the vanadium in the v-bearing steel slag into the water-soluble or acid soluble vanadium ion group that contains with means such as acidleach, the back extracts with extraction agent, and generation negatively charged ion or cationic exchange, because other metal ion mostly can not enter into organic phase, thereby realize that vanadium separates with the metallic impurity ionic.Use extraction agent (as NH again through the organic solution that extraction obtains
4Cl, ammoniacal liquor) back extraction, make vanadium change water over to from organic phase, adjust the pH value then, vanadium is precipitated out with the form of ammonium poly-vanadate or ammonium meta-vanadate, the calcination throw out promptly gets V
2O
5But the recovery rate of next two kinds of method vanadium is lower, is difficult to realize the efficient recovery of vanadium, and the consumption of acid is big.Therefore, the method that does not also occur the vanadium extraction from v-bearing steel slag that step is easy, the rate of recovery is high, pollution is little at present.
Summary of the invention
Technical problem to be solved by this invention provides the high method of extracting Vanadium Pentoxide in FLAKES from v-bearing steel slag of a kind of rate of recovery.
The technical scheme that the present invention solves the problems of the technologies described above specifically may further comprise the steps:
A, v-bearing steel slag add acidleach in the sulphuric acid soln;
B, step a leach liquor add iron powder reaction back and regulate pH to 1.50～2.0;
The solution concentration that c, step b obtain is 10%～15% di-(2-ethylhexyl)phosphoric acid extraction, collects upper layer of extraction liquid;
The extraction liquid concentration that d, step c collect is the sulfuric acid extraction of 2M～3M, collects lower floor's extraction liquid and regulates pH to 6.0～6.1, adds sodium chlorate in 60～70 ℃ of oxidations;
The solution that e, steps d make is regulated pH to 2～2.1, boils after-filtration, washing, and calcining promptly.
Further, need pre-treatment before the described v-bearing steel slag acidleach: v-bearing steel slag elder generation granularity after 1～3 grade of magnetic separation reaches below the 8mm, and metal Ferrum content is less than 1% (weight percent); Further grinding is extremely crossed 200 mesh sieves again.
The described sulphuric acid soln weight percent concentration of step a is 18%～22%, is preferably 20%, and the sulphuric acid soln consumption is 4.5～6 times of v-bearing steel slag weight; Sulphuric acid soln is specially and adopts concentration formulated greater than 96% analytical pure sulfuric acid, or adopts the sulfur waste acid of sulfate process titanium dioxide formulated.
Step a slowly joins pretreated v-bearing steel slag in the sulphuric acid soln, adds the back and fully stirs 1h～1.5h, filters by plate-and-frame filter press and obtains leach liquor.
Step b iron powder add-on is 1%～2% of a v-bearing steel slag gross weight; The reagent of regulating pH is NaOH.
Step c extraction agent once used amount is extraction agent: leach liquor=1:1.5～2.
Steps d extraction agent once used amount is leach liquor: extraction agent=1:4～8; The sodium chlorate consumption is 1.5 times of vanadium gross weight in the extraction liquid, and adding the sodium chlorate rear oxidation time is 1h.
The reagent that step e regulates pH is the ammoniacal liquor and/or the solid NaOH of weight concentration 25%.
The inventive method v-bearing steel slag adopts the direct acidleach of sulfuric acid and does not need roasting, makes vanadium change water-soluble or acid soluble vanadium ion into, and with the extraction agent extraction, the realization vanadium separates with metallic impurity.Extraction liquid is used the reverse-extraction agent back extraction again, makes vanadium change water over to from organic phase, adjusts pH value and makes the vanadium post precipitation calcine throw out promptly to get and contain V
2O
5Vanadium product greater than 65%.
The inventive method combines molten vanadium extracting method of acidleach alkali and solvent extraction vanadium extracting method, not only can reclaim the V that contains in the vanadium bessemer furnace slag
2O
5Product, the rate of recovery of raising vanadium resource also by the comprehensive processing method of the treatment of wastes with processes of wastes against one another, reduces the spent acid processing cost of sulfate process titanium dioxide, reduces the consumption of eo-acid, has the remarkable environmental benefit.
Embodiment
The invention will be further elaborated below in conjunction with embodiment.Embodiment only is used to illustrate the present invention, rather than limits the present invention by any way.
Embodiment 1
1, contain the pre-treatment of vanadium bessemer furnace slag: contain the vanadium bessemer furnace slag through 3 grades of magnetic separation after, obtain that 5mm is following, metallic iron (MFe) content is the steel-making slag powder of 0.5%～1% (weight percent), then further grinding to crossing 200 mesh sieves.
2. acidleach: contain vanadium bessemer furnace slag 300kg slowly to join concentration be in 20% the sulfuric acid pretreated, be as the criterion not splash, solvent and solute weight ratio is 5:1, fully stir 1h after, filter out leach liquor by plate-and-frame filter press.
3. contain the purification of vanadium leachate:, use the pH to 1.5 of NaOH regulator solution again with 3kg iron powder reducing leach liquor 1h.
4. extraction: step 3 receive the solution di-(2-ethylhexyl)phosphoric acid extraction agent that adds concentration 15% carry out 3 grades of extractions, each extraction agent consumption is extraction agent: leach liquor=1:1.5, collects, merges upper layer of extraction liquid.
5. strip: step 4 receive solution concentration be that the sulfuric acid of 2M carries out 3 grades of extractions, each extraction agent consumption is extraction agent: leach liquor=4:1, collects, merges lower floor's extraction liquid, and with NaOH adjusting pH to 6.0～6.1.
6. vanadium solution purifying, precipitation, calcining: in the solution that step 5 makes, add the sodium chlorate oxidation of vanadium gross weight 150% in the solution, in oxidation 1h more than 60 ℃.Add concentration then and be 25% ammoniacal liquor and NaOH regulator solution pH to 2, finish precipitation behind the heated and boiled 1h, filter and with clear water washing precipitation 4 times, promptly get grade after the throw out calcination and be 75% Vanadium Pentoxide in FLAKES, can be directly used in smelting ferrovanadium.
Embodiment 2
1. contain the pre-treatment of vanadium bessemer furnace slag: contain the vanadium bessemer furnace slag through 3 grades of magnetic separation after, obtain that 5mm is following, metallic iron (MFe) content is less than 1% steel-making slag powder, more further grinding to crossing 200 mesh sieves.
2. acidleach: with the pretreated vanadium bessemer furnace slag 2.2kg that contains, slowly join (sulfuric acid concentration is 20%) in the titanium white waste acid solution, be as the criterion not splash, liquid-solid ratio is 6:1, fully stir 1.5h after, filter out leach liquor by plate-and-frame filter press.
3. contain the purification of vanadium leachate:, use the pH to 1.5 of NaOH regulator solution again with 44g iron powder reducing leach liquor 1h.
4. extraction: step 3 receive solution concentration be that 15% di-(2-ethylhexyl)phosphoric acid extraction agent carries out 3 grades of extractions, each extraction agent consumption is extraction agent: leach liquor=1:1.7, collects, the merging upper layer of extraction liquid.
5. strip: step 4 receive solution concentration be that the sulfuric acid of 2M carries out 3 grades of extractions, each extraction agent consumption is extraction agent: leach liquor=4:1, collects, merges lower floor's extraction liquid, and with NaOH adjusting pH to 6.0～6.1.
6. vanadium solution purifying, precipitation, calcining: in the solution that step 5 makes, add the sodium chlorate oxidation of vanadium gross weight 150% in the solution, in oxidation 1h more than 65 ℃.Add concentration then and be 25% ammoniacal liquor and NaOH regulator solution pH to 2.1, finish precipitation behind the heated and boiled 1h, filter and, obtain throw out ammonium poly-vanadate 11.35g, V with clear water washing precipitation 3 times
2O
5Content〉65%.Ammonium poly-vanadate obtains content and is 75% V behind the calcining deamination
2O
5, can be directly used in smelting ferrovanadium.The total yield that contains vanadium bessemer furnace slag vanadium is 35%.
The inventive method can be operated at normal temperatures, and power and energy consumption is little, and has improved the rate of recovery of vanadium resource greatly.Can utilize the spent acid leaching v-bearing steel slag that produces in the production process of titanium pigment in addition, can reduce the processing cost of titanium white waste acid, reduce the pollution of environment.
Claims (8)
- [claim 1] a kind of method of extracting Vanadium Pentoxide in FLAKES from v-bearing steel slag is characterized in that: may further comprise the steps:A, v-bearing steel slag add acidleach in the sulphuric acid soln;B, step a leach liquor add iron powder reaction back and regulate pH to 1.50～2.0;The solution concentration that c, step b obtain is 10%～15% di-(2-ethylhexyl)phosphoric acid extraction, collects upper layer of extraction liquid;The solution concentration that d, step c collect is the sulfuric acid extraction of 2M～3M, collects lower floor's extraction liquid and regulates pH to 6.0～6.1, adds sodium chlorate in 60～70 ℃ of oxidations;The solution that e, steps d make is regulated pH to 2～2.1, boils after-filtration, washing, and calcining promptly.
- [claim 2] method of extracting Vanadium Pentoxide in FLAKES from v-bearing steel slag according to claim 1, it is characterized in that: the described sulphuric acid soln weight percent concentration of step a is 18%～22%.
- [claim 3] method of extracting Vanadium Pentoxide in FLAKES from v-bearing steel slag according to claim 1 is characterized in that: step a acidleach condition is for stirring 1h～1.5h in 20 ℃～30 ℃.
- [claim 4] method of extracting Vanadium Pentoxide in FLAKES from v-bearing steel slag according to claim 1, it is characterized in that: step b iron powder add-on is 1%～2% of a v-bearing steel slag gross weight.
- [claim 5] method of extracting Vanadium Pentoxide in FLAKES from v-bearing steel slag according to claim 1, it is characterized in that: step c extraction agent once used amount is extraction agent: leach liquor=1:1.5～2.
- [claim 6] method of extracting Vanadium Pentoxide in FLAKES from v-bearing steel slag according to claim 1, it is characterized in that: steps d extraction agent once used amount is leach liquor: extraction agent=1:4～8.
- [claim 7] method of extracting Vanadium Pentoxide in FLAKES from v-bearing steel slag according to claim 1 is characterized in that: steps d sodium chlorate consumption is 1.5 times of vanadium gross weight in the extraction liquid, and adding the sodium chlorate rear oxidation time is 1h.
- [claim 8] method of from v-bearing steel slag, extracting Vanadium Pentoxide in FLAKES according to claim 1, it is characterized in that: pretreatment process is before the v-bearing steel slag acidleach: granularity is less than 8mm after 1～3 grade of magnetic separation for v-bearing steel slag, and the metallic iron weight percent content is less than 1%; Further grinding is extremely crossed 200 mesh sieves again.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200810305929XA CN101418385B (en) | 2008-12-03 | 2008-12-03 | Method for extracting vanadium pentoxide from vanadium-containing steel slag |
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|---|---|---|---|
| CN200810305929XA CN101418385B (en) | 2008-12-03 | 2008-12-03 | Method for extracting vanadium pentoxide from vanadium-containing steel slag |
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|---|---|
| CN101418385A true CN101418385A (en) | 2009-04-29 |
| CN101418385B CN101418385B (en) | 2010-09-15 |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102121068A (en) * | 2011-04-08 | 2011-07-13 | 北京矿冶研究总院 | Method for preparing vanadium pentoxide |
| CN102430266A (en) * | 2010-09-29 | 2012-05-02 | 攀钢集团钢铁钒钛股份有限公司 | Method for purifying liquid with vanadium and method for preparing ammonium metavanadate and vanadium oxide |
| CN103952560A (en) * | 2014-04-23 | 2014-07-30 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for extracting vanadium from vanadium slag |
| CN104164571A (en) * | 2014-08-12 | 2014-11-26 | 东北大学 | Method for recovering valuable metal elements in converter vanadium slag |
| RU2748195C1 (en) * | 2020-10-21 | 2021-05-20 | Федеральное государственное бюджетное учреждение науки Институт химии твердого тела Уральского отделения Российской академии наук | Vanadium extraction method |
| CN113549769A (en) * | 2021-07-30 | 2021-10-26 | 攀枝花钢城集团有限公司 | Method for enriching vanadium in vanadium-containing steel slag |
-
2008
- 2008-12-03 CN CN200810305929XA patent/CN101418385B/en not_active Expired - Fee Related
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102430266A (en) * | 2010-09-29 | 2012-05-02 | 攀钢集团钢铁钒钛股份有限公司 | Method for purifying liquid with vanadium and method for preparing ammonium metavanadate and vanadium oxide |
| CN102430266B (en) * | 2010-09-29 | 2014-12-10 | 攀钢集团钢铁钒钛股份有限公司 | Method for purifying liquid with vanadium and method for preparing ammonium metavanadate and vanadium oxide |
| CN102121068A (en) * | 2011-04-08 | 2011-07-13 | 北京矿冶研究总院 | Method for preparing vanadium pentoxide |
| CN102121068B (en) * | 2011-04-08 | 2014-06-11 | 北京矿冶研究总院 | Method for preparing vanadium pentoxide |
| CN103952560A (en) * | 2014-04-23 | 2014-07-30 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for extracting vanadium from vanadium slag |
| CN103952560B (en) * | 2014-04-23 | 2016-05-11 | 攀钢集团攀枝花钢铁研究院有限公司 | A kind of method of Leaching of Vanadium from Vanadium slag |
| CN104164571A (en) * | 2014-08-12 | 2014-11-26 | 东北大学 | Method for recovering valuable metal elements in converter vanadium slag |
| CN104164571B (en) * | 2014-08-12 | 2017-03-29 | 东北大学 | The recovery method of valuable metal element in a kind of Converter Vanadium-bearing Slag |
| RU2748195C1 (en) * | 2020-10-21 | 2021-05-20 | Федеральное государственное бюджетное учреждение науки Институт химии твердого тела Уральского отделения Российской академии наук | Vanadium extraction method |
| CN113549769A (en) * | 2021-07-30 | 2021-10-26 | 攀枝花钢城集团有限公司 | Method for enriching vanadium in vanadium-containing steel slag |
| CN113549769B (en) * | 2021-07-30 | 2022-09-27 | 攀枝花钢城集团有限公司 | Method for enriching vanadium in vanadium-containing steel slag |
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|---|---|
| CN101418385B (en) | 2010-09-15 |
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