CN105219976A - Improve the method for vanadium slag calcification baking grog leaching yield - Google Patents
Improve the method for vanadium slag calcification baking grog leaching yield Download PDFInfo
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- CN105219976A CN105219976A CN201510811210.3A CN201510811210A CN105219976A CN 105219976 A CN105219976 A CN 105219976A CN 201510811210 A CN201510811210 A CN 201510811210A CN 105219976 A CN105219976 A CN 105219976A
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- leaching
- sulfuric acid
- calcification baking
- vanadium slag
- baking grog
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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
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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Abstract
The invention belongs to field of hydrometallurgy, specifically, relate to a kind of method improving vanadium slag calcification baking grog leaching yield.Improve the method for vanadium slag calcification baking grog leaching yield, control sulfuric acid leaching operation as follows: in calcification baking grog, add sulfuric acid, count in time starting to add sulfuric acid, the pH value adding the mixed slurry that sulfuric acid makes calcification baking grog/sulfuric acid be formed in 10 ~ 15min under rapid stirring state reaches 2.8 ~ 3.2; Wherein, rapid stirring state accuses that stirring intensity processed makes the upset speed >=16 time/min of slurry in leaching vat; The pH of slurry to be mixed is stabilized in 2.8 ~ 3.2, reduce stirring intensity make the upset speed of slurry in leaching vat at 5.5 ~ 8 times/min, and control pH constant in 2.8 ~ 3.2 until sulfuric acid leaching operation terminates.The method of raising vanadium slag calcification baking grog leaching yield of the present invention, achieves the object (its leaching yield Absorbable organic halogens reaches more than 97%) of the leaching yield improving its vanadium.
Description
Technical field
The invention belongs to field of hydrometallurgy, specifically, relate to a kind of method improving vanadium slag calcification baking grog leaching yield.
Background technology
" vanadium oxide process for cleanly preparing " (hereinafter referred to as " novel process ") successively experienced by laboratory test research, 10t/aV
2o
5the gordian technique of extension test breaks through, and 0.5kt/aV
2o
5clean vanadium extraction pilot scale line production test, obtains huge technological breakthrough, solves the technical barrier produced high quality vanadium oxide product and waste water, waste residue economic circulation and utilize, realizes industrialization produce in 2012 at Xichang steel vanadium.
Novel process is different from traditional sodium sinter process, adopts the technical process of vanadium slag " calcification baking---sulfuric acid leaching---acidic precipitation ".Along with an on-the-spot novel process roasting technology difficult problem is captured, roasting conversion rate brings up to more than 88%.But the on-the-spot leaching yield leaching vanadium in grog when producing is about 92%, especially when every tank leaches clinker quantity and mother liquor volume is larger time, leaching yield is low to moderate 87% especially, greatly constrains the vanadium recovery of roasting-leaching operation.On-the-spot by reducing single tank grog treatment capacity, to reaching good leaching effect, but fail fundamentally to solve the problem that the leaching yield of vanadium in on-the-spot grog is low.
Chinese patent CN200810305601.8 and CN201310329193.0 disclose in calcification vanadium slag sintering cleaner production vanadium oxide vanadium extraction leaching method and vanadium extraction leaching plant, but the Optimal improvements of undeclared leaching process drive-motor and actual effect not match condition.
Summary of the invention
The present invention is directed to above-mentioned defect, a kind of method improving vanadium slag calcification baking grog leaching yield is provided, it is by the stirring intensity in Discrete control sulfuric acid leaching operation, achieve the object (its leaching yield Absorbable organic halogens reaches more than 97%) of the leaching yield improving its vanadium, energy-conservation basis is improved the vanadium yield that vanadium oxide cleans extraction.
Technical scheme of the present invention:
The invention provides a kind of method improving vanadium slag calcification baking grog leaching yield, control sulfuric acid leaching operation as follows:
In calcification baking grog, add sulfuric acid, count when certainly starting to add sulfuric acid, the pH value adding the mixed slurry that sulfuric acid makes calcification baking grog/sulfuric acid be formed in 10 ~ 15min under rapid stirring state reaches 2.8 ~ 3.2; Wherein, rapid stirring state accuses that stirring intensity processed makes the upset speed >=16 time/min of slurry in leaching vat;
The pH of slurry to be mixed is stabilized in 2.8 ~ 3.2, reduce stirring intensity make the upset speed of slurry in leaching vat at 5.5 ~ 8 times/min, and control pH constant in 2.8 ~ 3.2 until sulfuric acid leaching operation terminates.
Further, in aforesaid method, rapid stirring state accuses that stirring intensity processed makes the upset speed of slurry in leaching vat be 16-20 time/min.
Further, in above-mentioned sulfuric acid leaching operation, control liquid-solid ratio is 2:1 ~ 4:1.
Further, in sulfuric acid leaching operation, extraction time controls at 60 ~ 100min.
Further, in sulfuric acid leaching operation, the concentration of sulfuric acid is: the vitriol oil and the volume ratio of water are that 1 ︰ 1 mixes.
Further, in sulfuric acid leaching operation, the agitating vane adopted in leaching vat is: upper strata is three narrow leaves or four wide leaf formulas, and lower floor is straight leaf turbine type or 15 ° of oblique leaf turbine types.
Further, in sulfuric acid leaching operation, the trough body structure of leaching vat is: stirring cell wall has material in the traverse baffle auxiliary tank of 4 leaf 15 ~ 20cm to strengthen flow field.
Further, in sulfuric acid leaching operation, in described calcification baking grog, TV (total content of vanadium) content is 8% ~ 11%, magnetic material content≤3%.
Further, in sulfuric acid leaching operation, the Task-size Controlling of described calcification baking grog is: particle diameter accounts for more than 95% at below 125um, and particle diameter is less than 5% at the need of more than 180um.
When adopting the 30m of φ 3000 × 4500
3when leaching vat and corresponding quick agitator thereof, stir shaft speed is: adding sulfuric acid, to start agitator shaft speed to the time period adding sulfuric acid be 97r/min, and it is 63r/min that sulfuric acid adds rear control agitator shaft speed.
Beneficial effect of the present invention:
Leach after steel basin is Rapid Leaching steel basin by improving, production test data show that the leaching yield of vanadium in calcification baking grog fine powder can reach 97.22%, and the comparatively existing leaching yield of producing vanadium that leaches exceeds 5 percentage points; By its leaching process processing parameter of stability contorting, its leaching yield Absorbable organic halogens reaches more than 97%, and expectation can be created economic benefit and reach 1,500 ten thousand yuan.
Embodiment
The invention provides a kind of method improving vanadium slag calcification baking grog leaching yield, affiliated main technical schemes comprises the following steps:
(1) the newly-increased Rapid Leaching steel basin of field conduct, leaching starts front 10 ~ 15min setting electric machine frequency and ensures that tank inner fluid upset number of times reaches 16 times/min or more, carries out the external diffusion rate-determining steps of calcification grog; Then be reduced to general leaching production driving frequency, the leaching completing calcification grog is produced;
(2) processing parameter of newly-increased Rapid Leaching steel basin is as follows:
1. liquid-solid ratio: 2:1 ~ 4:1;
2. pH value is leached: 2.8 ~ 3.2;
3. extraction time: 60 ~ 100min;
4. sulfuric acid concentration: 1:1 (V:V) ~ vitriol oil, the vitriol oil to be mass concentration be 95% sulfuric acid; Sulfuric acid in the present invention is: density to be the mass concentration of 1.84g/mL be 95% sulfuric acid by the volume ratio of 1:1 and water mixing gained.
5. acid adding controls: acid adding in 10-15min, and pH is reduced to about 3.0;
6. agitating vane: upper strata is three narrow leaves or four wide leaf formulas, lower floor is straight leaf turbine type or 15 ° of oblique leaf turbine types;
7. trough body structure: stirring cell wall has material in the traverse baffle auxiliary tank of 4 leaves ~ 20cm to strengthen flow field
8. stirring intensity: leach and start front 10 ~ 15min and set electric machine frequency and to make in groove materials overturning number of times >=16 time/min, agitator shaft speed is set drive-motor frequency near 97r/min, pH are stabilized in 3.0 after 10min to make agitator shaft speed be 63r/min.
(3) leaching calcification grog of the present invention grinds grog fine powder for meeting processing requirement (-120 order >=95% ,+80 order≤5%, MFe≤3%) through rod milling, and its TV content is 8% ~ 11%.
Room proof test data by experiment, judge that the sulfuric acid leaching process of calcification baking grog is mainly divided into two step of reaction.It is external diffusion Reaction controlling step in the 5-15min that about acid adding starts, at this one-phase, grog vanadium dissolution rate that is outer and middle level is exceedingly fast, and after adding sulfuric acid in 1-2 minute, the viscosity of slip can sharply be elevated to 200-500Pa/s (relevant with temperature) from the viscosity close to water, therefore stirring strongly must be had could to meet the reacting dynamics condition of sulfuric acid and the grog added, avoid the localized acidity that causes not in time because of sulfuric acid blending dispersion too high and the irreversible precipitation reaction that causes simultaneously.And the power of motor of existing batch extractor is only 18.5kw, far can not meet the requirement of this one-phase, therefore need the flashing reactor that newly-increased stirring intensity is very high.About the 20-60min that about acid adding starts, the vanadium stripping in grog skin and middle level, the vanadium of internal layer needs to move to particle surface and could react, at this moment vanadium becomes rate-determining steps from the migration of internal layer outer layers, i.e. internal diffusion rate-determining steps, the stirring intensity demand in this stage is little, as long as solid materials does not obviously sink to the bottom in tank, namely existing batch extractor meets this step requirement.
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.
Embodiment 1:
To 18m
3vanadium concentration be 0 ~ 12g/L containing vanadium leaching solvent (herein terminate after filtration containing vanadium leaching solvent and acidleach, the wash filtrate of gained after washing, leaching solvent during first time acidleach can be process water, can obtain after washing after filtration containing vanadium leaching solvent, recycle for leaching next time, as long as the wash filtrate of its concentration in 12g/L all can be used as containing vanadium leaching solvent) in add 6t and meet processing requirement (namely particle diameter meets: particle diameter accounts for more than 95% at below 125um, particle diameter is less than 5% at the need of more than 180um, magnetic material content≤3%, TV content is 8% ~ 11%) calcification baking grog fine powder, adopt the 30m of φ 3000 × 4500
3leaching vat and corresponding quick agitator thereof, rapid stirring (setting drive-motor agitator shaft speed is 97r/min) in Rapid Leaching steel basin, auto-adjustment control is opened after slip pH to be mixed is stable, adding sulfuric acid (its concentration is: the vitriol oil mixes with the 1:1 by volume of water) in 10 ~ 15min fast makes the pH value of slurry in steel basin be 2.8 ~ 3.2, slip pH to be mixed is stabilized in about 3.0, setting drive-motor agitator shaft speed after 10min is 63r/min, and makes the pH value of slurry be stabilized in 2.8 ~ 3.2 by slowly adding sulfuric acid, after end of processing to be leached, mixed slurry is sent into dashpot, after filtration, washing after obtain leach liquor and leach residue, recording leach liquor mean concns is 27.94g/l, and residue average T V is 1.48%, calculate leaching yield be 98.32%.
Embodiment 2:
To 18m
3vanadium concentration is add the calcification baking grog fine powder that 8t meets processing requirement, rapid stirring in Rapid Leaching steel basin containing in vanadium leaching agent of 0 ~ 12g/L, and setting drive-motor agitator shaft speed is 97r/min; Auto-adjustment control is opened after slip pH to be mixed is stable, add the dilute sulphuric acid that volume ratio is 1:1 fast, when slip pH to be mixed is stabilized in about 3.0, setting drive-motor agitator shaft speed after 10min is 63r/min, keeps its acid adding speed to make mixed slurry pH be stabilized in 2.8 ~ 3.2; After waiting for that leaching process terminates, mixed slurry is sent into dashpot, after filtration, obtain leach liquor and leach residue after washing, leach liquor mean concns is 31.9g/l, and residue average T V is 1.64%, and calculating leaching yield is 97.58%.
Embodiment 3:
To 14m
3vanadium concentration is add the calcification baking grog fine powder that 6t meets processing requirement, rapid stirring in Rapid Leaching steel basin containing in vanadium leaching agent of 0 ~ 12g/L, and setting drive-motor agitator shaft speed is 97r/min; Auto-adjustment control is opened after slip pH to be mixed is stable, add the dilute sulphuric acid that volume ratio is 1:1 fast, when slip pH to be mixed is stabilized in about 3.0, setting drive-motor agitator shaft speed after 10min is 63r/min, keeps its acid adding speed to make mixed slurry pH be stabilized in 2.8 ~ 3.2; After waiting for that leaching process terminates, mixed slurry is sent into dashpot, after filtration, obtain leach liquor and leach residue after washing, leach liquor mean concns is 35.2g/l, and residue average T V is 1.71%, and calculating leaching yield is 97.49%.
Claims (9)
1. improve the method for vanadium slag calcification baking grog leaching yield, it is characterized in that, control sulfuric acid leaching operation as follows:
In calcification baking grog, add sulfuric acid, count when certainly starting to add sulfuric acid, the pH value adding the mixed slurry that sulfuric acid makes calcification baking grog/sulfuric acid be formed in 10 ~ 15min under rapid stirring state reaches 2.8 ~ 3.2; Wherein, rapid stirring state accuses that stirring intensity processed makes the upset speed >=16 time/min of slurry in leaching vat;
The pH of slurry to be mixed is stabilized in 2.8 ~ 3.2, reduce stirring intensity make the upset speed of slurry in leaching vat at 5.5 ~ 8 times/min, and control pH constant in 2.8 ~ 3.2 until sulfuric acid leaching operation terminates.
2. the method for raising vanadium slag calcification baking grog leaching yield according to claim 1, is characterized in that, rapid stirring state accuses that stirring intensity processed makes the upset speed of slurry in leaching vat be 16 ~ 20 times/min.
3. the method for raising vanadium slag calcification baking grog leaching yield according to claim 1 and 2, is characterized in that, in sulfuric acid leaching process, controlling liquid-solid ratio is 2 ︰ 1 ~ 4 ︰ 1.
4. the method for the raising vanadium slag calcification baking grog leaching yield according to any one of claims 1 to 3, it is characterized in that, in described calcification baking grog, TV content is 8% ~ 11%, magnetic material content≤3%.
5. the method for the raising vanadium slag calcification baking grog leaching yield according to any one of Claims 1 to 4, it is characterized in that, the Task-size Controlling of described calcification baking grog is: particle diameter accounts for more than 95% at below 125um, and particle diameter is less than 5% at the need of more than 180um.
6. the method for the raising vanadium slag calcification baking grog leaching yield according to any one of Claims 1 to 5, it is characterized in that, in sulfuric acid leaching operation, extraction time controls at 60 ~ 100min.
7. the method for the raising vanadium slag calcification baking grog leaching yield according to any one of claim 1 ~ 6, it is characterized in that, the concentration of sulfuric acid is: the vitriol oil and the volume ratio of water are that 1 ︰ 1 mixes.
8. the method for the raising vanadium slag calcification baking grog leaching yield according to any one of claim 1 ~ 7, it is characterized in that, in sulfuric acid leaching operation, the agitating vane adopted in leaching vat is: upper strata is three narrow leaves or four wide leaf formulas, and lower floor is straight leaf turbine type or 15 ° of oblique leaf turbine types.
9. the method for the raising vanadium slag calcification baking grog leaching yield according to any one of claim 1 ~ 8, it is characterized in that, in sulfuric acid leaching operation, the trough body structure of leaching vat is: stirring cell wall has material in the traverse baffle auxiliary tank of 4 leaf 15 ~ 20cm to strengthen flow field.
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Cited By (7)
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| CN106987716A (en) * | 2017-06-05 | 2017-07-28 | 攀钢集团研究院有限公司 | The continuous acidic leaching method of vanadium slag calcification baking clinker |
| CN107475518A (en) * | 2017-10-11 | 2017-12-15 | 攀钢集团钒业有限公司 | A kind of method that vanadium classification is leached |
| CN107723483A (en) * | 2017-10-11 | 2018-02-23 | 攀钢集团钒钛资源股份有限公司 | The method for controlling vanadium slag calcification baking and its clinker sulfuric acid leaching technological parameter |
| CN107723482A (en) * | 2017-10-11 | 2018-02-23 | 攀钢集团钒钛资源股份有限公司 | The method for controlling vanadium slag calcification baking clinker sulfuric acid leaching technological parameter |
| CN109097567A (en) * | 2018-10-10 | 2018-12-28 | 攀钢集团钒钛资源股份有限公司 | The secondary pickling technique of vanadium slag calcification baking clinker |
| CN109252047A (en) * | 2018-10-31 | 2019-01-22 | 攀钢集团钒钛资源股份有限公司 | Calcification clinker acidleach method |
| CN114350982A (en) * | 2021-11-30 | 2022-04-15 | 攀钢集团研究院有限公司 | Method for extracting vanadium by using calcified roasting clinker and recycling leaching washing liquid |
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| CN106987716A (en) * | 2017-06-05 | 2017-07-28 | 攀钢集团研究院有限公司 | The continuous acidic leaching method of vanadium slag calcification baking clinker |
| CN106987716B (en) * | 2017-06-05 | 2019-03-19 | 攀钢集团研究院有限公司 | The continuous acidic leaching method of vanadium slag calcification baking clinker |
| CN107475518A (en) * | 2017-10-11 | 2017-12-15 | 攀钢集团钒业有限公司 | A kind of method that vanadium classification is leached |
| CN107723483A (en) * | 2017-10-11 | 2018-02-23 | 攀钢集团钒钛资源股份有限公司 | The method for controlling vanadium slag calcification baking and its clinker sulfuric acid leaching technological parameter |
| CN107723482A (en) * | 2017-10-11 | 2018-02-23 | 攀钢集团钒钛资源股份有限公司 | The method for controlling vanadium slag calcification baking clinker sulfuric acid leaching technological parameter |
| CN107475518B (en) * | 2017-10-11 | 2019-02-19 | 攀钢集团钒钛资源股份有限公司 | A kind of method that vanadium classification is leached |
| CN107723483B (en) * | 2017-10-11 | 2022-06-24 | 攀钢集团钒钛资源股份有限公司 | Method for controlling technological parameters of vanadium slag calcification roasting and clinker sulfuric acid leaching |
| CN109097567A (en) * | 2018-10-10 | 2018-12-28 | 攀钢集团钒钛资源股份有限公司 | The secondary pickling technique of vanadium slag calcification baking clinker |
| CN109252047A (en) * | 2018-10-31 | 2019-01-22 | 攀钢集团钒钛资源股份有限公司 | Calcification clinker acidleach method |
| CN114350982A (en) * | 2021-11-30 | 2022-04-15 | 攀钢集团研究院有限公司 | Method for extracting vanadium by using calcified roasting clinker and recycling leaching washing liquid |
| CN114350982B (en) * | 2021-11-30 | 2023-09-15 | 攀钢集团研究院有限公司 | Method for extracting vanadium and recycling leaching washing liquid by calcified roasting clinker |
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Effective date of registration: 20191030 Address after: 615032, Liangshan Yi Autonomous Prefecture of Xichang province Sichuan City Industrial Zone, Panzhihua Steel Group Xichang steel vanadium Co., Ltd. Patentee after: Pangang Group Xichang Steel & Vanadium Co., Ltd. Address before: 615032, Liangshan Yi Autonomous Prefecture of Xichang province Sichuan City Industrial Zone, Panzhihua Steel Group Xichang steel vanadium Co., Ltd. Co-patentee before: Pangang Group Institute Co., Ltd. Patentee before: Pangang Group Xichang Steel & Vanadium Co., Ltd. |
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Effective date of registration: 20210818 Address after: 615000 vanadium and Titanium Industrial Park, Xichang City, Liangshan Yi Autonomous Prefecture, Sichuan Province Patentee after: Panzhihua Iron and Steel Group Xichang vanadium products Technology Co.,Ltd. Address before: 615032 Xichang steel vanadium Co., Ltd. of Panzhihua Iron and Steel Group, Jiuzhai Industrial Park, Xichang City, Liangshan Yi Autonomous Prefecture, Sichuan Province Patentee before: XICHANG STEEL VANADIUM CO., LTD., PANGANG Group |
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