CN102337410A - Method for recycling vanadium from dephosphorization base flow residues - Google Patents
Method for recycling vanadium from dephosphorization base flow residues Download PDFInfo
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- CN102337410A CN102337410A CN2011103180816A CN201110318081A CN102337410A CN 102337410 A CN102337410 A CN 102337410A CN 2011103180816 A CN2011103180816 A CN 2011103180816A CN 201110318081 A CN201110318081 A CN 201110318081A CN 102337410 A CN102337410 A CN 102337410A
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- vanadium
- dephosphorization
- vanadate
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- underflow slag
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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 provides a method for recycling vanadium from dephosphorization base flow residues. The method comprises the following steps of: leaching the dephosphorization base flow residues by using a sulfuric acid solution to obtain acid vanadium-containing leachate; performing dephosphorization treatment on the acid vanadium-containing leachate, precipitating the vanadium, and thus obtaining coarse ammonium polyvanadate; dissolving the coarse ammonium polyvanadate by using a basic solvent to obtain a basic vanadium-containing solution; and performing vanadium precipitation treatment on the basic vanadium-containing solution to obtain ammonium metavanadate or ammonium polyvanadate, deaminating the ammonium metavanadate or the ammonium polyvanadate, performing oxidizing roasting, and thus obtaining vanadium oxide. The method has the advantages that: vanadium elements are recycled from the dephosphorization base flow residues, and the recovery rate of the vanadium elements is not less than 87.3 percent; production operation stability and product stability are high; and processes are shortened, and the cost is reduced.
Description
Technical field
The present invention relates to the recovery and utilization technology field of v element in the slag, more particularly, relate to a kind of method that reclaims vanadium in the dephosphorization underflow slag.
Background technology
The traditional technology of producing vanadium oxide comprises operations such as vanadium raw materials, sodium roasting, water logging, purification, precipitation, deamination are provided in order.In the water logging process of sodium roasting operation gained grog, except v element got in the solution, impurity elements such as silicon, phosphorus together got into solution.For deposition rate and the quality product that improves vanadium, obtain high vanadium oxide (for example, the V of purity
2O
3Or V
2O
5) product, must remove impurity elements such as silicon in the leach liquor, phosphorus.
The method of removing impurity element such as silicon, phosphorus in the leach liquor usually is in above-mentioned solution, to add an amount of calcium chloride solution.When adding calcium chloride solution, excessive or local excessive calcium chloride and the v element in the leach liquor form insoluble vanadic acid calcium, and this insoluble vanadic acid calcium forms dephosphorization underflow slag with other throw out.Usually, the content of v element is approximately 10%～20% by weight percentage in the said dephosphorization underflow slag.
At present, the processing overwhelming majority to dephosphorization underflow slag carries out re-baking through it being returned sodium roasting workshop section.The obvious deficiency of this treatment process is: the one, because the calcium contents in the dephosphorization underflow slag is high,, cause the total yield of v element low so the vanadium transformation efficiency is lower in the sodium roasting process; The 2nd, because impurity such as the part silicon in the dephosphorization underflow slag, phosphorus can get into leach liquor once more in leaching process, thereby needing to cause further removal of impurities; The 3rd, this treatment process operation is long, cost is high.
The patented claim that disclosed publication number was CN101182037 on May 21st, 2008 discloses a kind of method that from dephosphorization underflow slag, reclaims vanadium oxide; This method directly leaches dephosphorization underflow slag with carbonate aqueous solutions such as volatile salt or bicarbonate of ammonia, and precipitation behind the leach liquor silica removal, deamination are produced the vanadium oxide product.Yet, when adopting carbonate aqueous solution to leach, exist two aspects not enough at least: the one, the vanadium leaching yield is unstable; Specifically, under alkaline leaching condition, be prone to form the ammonium meta-vanadate deposition when vanadium, ammonium salt coexistence; Form the how much relevant of ammonium meta-vanadate with solution temperature; And in commercial process, system temperature can not get abundant guarantee, soaks the poor stability of rate thereby can cause vanadium to change; The 2nd, it is relatively low that vanadium changes the rate of soaking, and under all preferable condition of each processing parameter, it is 85%～86% that vanadium changes the rate of soaking.
Summary of the invention
To the deficiency that prior art exists, the invention provides a kind of method that can improve vanadium in the high recovery dephosphorization underflow slag of vanadium recovery and stability.
The invention provides a kind of method that reclaims vanadium in the dephosphorization underflow slag.Said method comprises step: A, leach dephosphorization underflow slag with sulphuric acid soln, obtain acidity and contain vanadium leachate; B, acidity contained vanadium leachate and carries out dephosphorization and handle after, precipitation obtains thick ammonium poly-vanadate; C, dissolve thick ammonium poly-vanadate, obtain alkalescence and contain vanadium solution with basic solvent; D, alkalescence is contained vanadium solution carry out precipitation and handle, obtain ammonium meta-vanadate or ammonium poly-vanadate, ammonium meta-vanadate or ammonium poly-vanadate make barium oxide behind deamination, oxidizing roasting.
Compared with prior art, beneficial effect of the present invention comprises: v element has been reclaimed in (1) from dephosphorization underflow slag, and the recovery of v element high (for example, being not less than 87.3%); (2) production operation and good stability of products; (3) shorten operation, reduced cost.
Embodiment
Hereinafter, with combining exemplary embodiment to specify the method for vanadium in the recovery dephosphorization underflow slag of the present invention.
The method of vanadium comprises step in the recovery dephosphorization underflow slag of the present invention: A, leach dephosphorization underflow slag with sulphuric acid soln, obtain acidity and contain vanadium leachate; B, acidity contained vanadium leachate and carries out dephosphorization and handle after, precipitation obtains thick ammonium poly-vanadate; C, dissolve thick ammonium poly-vanadate, obtain alkalescence and contain vanadium solution with basic solvent; D, alkalescence is contained vanadium solution carry out precipitation and handle, obtain ammonium meta-vanadate or ammonium poly-vanadate, ammonium meta-vanadate or ammonium poly-vanadate make barium oxide behind deamination, oxidizing roasting.
In the present invention, said dephosphorization underflow slag is meant at the slag that solution in the preparation vanadium oxide technology, that obtain through sodium roasting and water logging is carried out form when removal of impurities is handled.Generally, contain impurity elements such as a certain amount of v element (for example, about by weight percentage 10%～20%) and manganese, magnesium, silicon, phosphorus in this dephosphorization underflow slag.
In one embodiment of the invention, dephosphorization among the said step B is handled can adopt to contain to said acidity and is added ferric sulfate, Tai-Ace S 150 or polymeric aluminum sulfate silicate iron in the vanadium leachate as dephosphorization agent, so that the phosphoric that said acidity contains in the vanadium leachate forms deposition.Preferably, the add-on of said dephosphorization agent can be 4.0～5.0 to calculate according to the weight ratio that said dephosphorization agent and said acidity contain the phosphoric in the vanadium leachate.
In one embodiment of the invention, the basic solvent among the said step C is preferably sodium hydroxide solution or sodium carbonate solution.
In one embodiment of the invention, said steps A also can be included in sulphuric acid soln and leach before the dephosphorization underflow slag, and dephosphorization underflow slag is mixed with water, stirs then and heats, with the raising leaching efficiency.
In one embodiment of the invention, said when leaching dephosphorization underflow slag with sulphuric acid soln pH be preferably 2.0～3.0.When using sulphuric acid soln to leach dephosphorization underflow slag, if the pH of the system of leaching greater than 3.0, then can the little vanadium leaching yield that causes reduce because of the main thing phase vanadic acid calcium solubleness in the dephosphorization underflow slag; If the pH of the system of leaching less than 2.0, can not increase because of the main thing phase vanadic acid calcium in the dephosphorization underflow slag has fully dissolved the vanadium leaching yield, but impurity such as the phosphorus in the solution, iron, manganese can increase because of the reduction of pH.
The time of leaching in the said steps A in one embodiment of the invention, can be 30～60min.
In one embodiment of the invention, said step D can add ammonium salt and obtains ammonium meta-vanadate with deposition through directly containing in the vanadium solution to said alkalescence, perhaps can contain vanadium solution to acid back and adds the ammonium salt deposition and obtain ammonium poly-vanadate through regulating said alkalescence.
In one embodiment of the invention, the pH that the dephosphorization among the said step B is handled is preferably 2.0～3.0, and the time that dephosphorization is handled can be 30～60min.
The principle of the method for vanadium comprises in the recovery dephosphorization underflow slag of the present invention: (1) utilizes and (for example mainly contains vanadium thing phase in the dephosphorization underflow slag; Vanadic acid calcium) be soluble in sour character; Form acidity with the vanadium in the sulfuric acid dissolution dephosphorization underflow slag and contain vanadium solution, impurity elements such as while part manganese, magnesium, silicon, phosphorus also get into acidity together and contain vanadium solution.(2) oxytropism contains and adds the phosphate radical that ferric sulfate, Tai-Ace S 150 or polymeric aluminum sulfate silicate iron etc. and acidity contains in the vanadium solution in the vanadium solution and form depositions such as tertiary iron phosphate or phosphagel phosphaljel; Contain the part phosphorus in the vanadium solution to remove acidity; Here, acidity contains phosphorus content in the vanadium solution and reduces the precipitation rate when can improve acid precipitation largely.(3) acidity after the dephosphorization being contained vanadium solution carries out precipitation and handles and can remove impurity elements such as most phosphorus, silicon, manganese, magnesium; For example, the acidity after the dephosphorization contains vanadium solution and carries out the acid ammonium salt precipitation and handle to obtain thick ammonium poly-vanadate, here; In acid ammonium salt precipitation process; The selective binding of vanadic acid radical ion and ammonium radical ion can force rate manganese, magnesium is strong, and the vanadic acid radical ion combines with the ammonium radical ion to form and precipitates and manganese, magnesium are stayed in the solution, thereby the realization vanadium separates with manganese, the magnesium of the overwhelming majority; When precipitation, the phosphorus, silicon that few part only arranged parcel, absorption etc. when forming the ammonium poly-vanadate particle are former thereby get in the ammonium poly-vanadate, and other overwhelming majority is stayed in the solution, thereby the realization vanadium separates with the overwhelming majority of phosphorus, silicon.(4) come to dissolve the thick ammonium poly-vanadate that obtains through above-mentioned precipitation processing again with basic soln (for example, sodium hydroxide or yellow soda ash), contain vanadium solution to obtain alkalescence, at this moment, the manganese in the thick ammonium poly-vanadate, magnesium are because of forming Mn (OH)
2, Mg (OH)
2Deposition; And vanadium gets into solution because of dissolving, thereby thoroughly realizes separating of vanadium and impurity elements such as manganese, magnesium, and thoroughly remove silicon, impurity elements such as manganese, magnesium; And (the solution phosphorus content is not higher than 0.30g/L when for example, precipitating ammonium meta-vanadate can the content of phosphoric to be controlled at acceptability limit; Phosphorus content after thick ammonium poly-vanadate heavily dissolves generally is lower than 0.10g/L), even the underproof situation of phosphorus concentration occurs accidentally, under alkaline condition, phosphoric is also very easily removed (for example, making phosphate radical form calcium phosphate precipitation through adding calcium chloride).(5) said alkalescence is contained vanadium solution and carry out precipitation and handle and to obtain ammonium meta-vanadate or ammonium poly-vanadate, then ammonium meta-vanadate or ammonium poly-vanadate are carried out deamination, oxidizing roasting, can make qualified Vanadium Pentoxide in FLAKES.
In addition, the method for vanadium also can realize through following technical scheme in the recovery dephosphorization underflow slag of the present invention:
(1) with dephosphorization underflow slag making beating and be heated to 30～60 ℃, regulate slurry pH=2.0～3.0 with sulfuric acid and leach, leach reaction 30～90min after-filtration, washing, obtain acidity and contain vanadium leachate.
(2) acidity contains and adds the ammonium salt precipitation after the vanadium leachate dephosphorization and produce thick ammonium poly-vanadate, and thick ammonium poly-vanadate heavily dissolves after-filtration with basic solvent, obtains alkalescence and contains vanadium solution.
(3) alkalescence contains and adds ammonium salt deposition ammonium poly-vanadate after vanadium solution directly adds ammonium salt deposition ammonium meta-vanadate or is adjusted to acidity, and ammonium meta-vanadate or ammonium poly-vanadate obtain Vanadium Pentoxide in FLAKES through the deamination oxidizing roasting.
To combine concrete example to come the present invention is done further elaboration below.Following example only is used to explain the present invention, rather than limits the present invention by any way.
Example 1
(its composition (below, also be designated as wt%) is by weight percentage counted: V 10.08%, and Si 5.69% with dephosphorization underflow slag 200g; P 2.68%; Ca 16.98%, Mn 6.17%, Mg 2.10%, and the O element of surplus and other trace impurity) join in the 400mL water; Stirring to be forming slurry, and slurry is heated to 30 ℃.Then; Using volumetric concentration is that 50% sulphuric acid soln is regulated slurry to its pH=2.0～2.2; Leach then, behind the leaching reaction 30min, filter, wash; Obtain 576mL acidity and contain vanadium leachate (be also referred to as acidity and contain vanadium solution, and wherein contain the V of 32.24g/L, the Si of 0.68g/L, the P of 0.96g/L, the Mn of 6.71g/L, the Mg of 0.77g/L) and residue 188.32g (V that wherein contains 0.85wt%).It is thus clear that the leaching yield of vanadium is 92.1wt%.
Contain the polymeric aluminum sulfate silicate iron that adds 2.48g in the vanadium leachate to said acidity and carry out dephosphorization, stirring reaction 30min after-filtration.Regulate filtrating pH value to 1.8 with the vitriol oil, add ammonium sulfate 22.28g post-heating to 95 ℃, reaction 60min under agitation condition, is dried and is obtained thick ammonium poly-vanadate at filtration.Using the 350mL mass concentration is that 8% sodium hydroxide solution dissolves thick ammonium poly-vanadate; Filter; Obtain 348mL filtrating (wherein contain Si, the 0.04g/L of V, the 0.08g/L of 51.37g/L P,＜Mn of 0.01g/L, the Mg of 0.02g/L); In filtrating, add 55g ammonium sulfate and carry out the precipitation processing, to obtain ammonium meta-vanadate.Ammonium meta-vanadate is calcined the 3h deaminations, acquisition Vanadium Pentoxide in FLAKES 32.02g, its V in 500 ℃ in retort furnace
2O
5Content is 98.70wt%.
Example 2
(its composition is by weight percentage: V 10.08%, and Si 5.69%, P2.68% with dephosphorization underflow slag 100g; Ca 16.98%; Mn 6.17%, Mg 2.10%, and the O element of surplus and other trace impurity) join in the 200mL water, stir and slurry is heated to 60 ℃.Then; Using volumetric concentration is that 50% sulphuric acid soln is regulated slurry to its pH=2.8～3.0; Leach then; After leaching reaction 90min, filter, wash, obtain 336mL acidity and contain vanadium leachate (wherein containing the V of 27.27g/L, the Si of 0.63g/L, the P of 0.77g/L, the Mn of 4.36g/L, the Mg of 0.54g/L) and residue 94.8g (wherein containing V 0.97wt%).It is thus clear that the leaching yield of vanadium is 90.9%.
Contain the ferric sulfate that adds 1.16g in the vanadium leachate to said acidity and carry out dephosphorization, stirring reaction 60min after-filtration.Regulate filtrating pH value to 1.8 with the vitriol oil, add ammonium sulfate 11.00g post-heating to 95 ℃, reaction 60min under agitation condition, is dried and is obtained thick ammonium poly-vanadate at filtration.Using the 320mL mass concentration is that 5% sodium hydroxide solution dissolves thick ammonium poly-vanadate, filters, obtain 318mL filtrating (wherein contain Si, the 0.02g/L of V, the 0.05g/L of 27.96g/L P,＜Mn of 0.01g/L, the Mg of 0.02g/L); Using the vitriol oil that filtrating is adjusted to its pH value then is 2, then in filtrating, adds 11.00g ammonium sulfate and carries out the precipitation processing, to obtain ammonium poly-vanadate.Ammonium poly-vanadate is calcined the 3h deaminations, acquisition Vanadium Pentoxide in FLAKES 15.87g, its V in 500 ℃ in retort furnace
2O
5Content is 99.02wt%.
Example 3
(its composition is by weight percentage: V 10.08%, and Si 5.69%, P2.68% with dephosphorization underflow slag 100g; Ca 16.98%; Mn 6.17%, Mg 2.10%, and the O element of surplus and other trace impurity) join in the 200mL water, stir and slurry is heated to 40 ℃.Then; Using volumetric concentration is that 50% sulphuric acid soln is regulated slurry to its pH=2.5～2.7; Leach then; After leaching reaction 60min, filter, wash, obtain acidity and contain vanadium leachate (wherein containing the V of 26.78g/L, the Si of 0.65g/L, the P of 0.82g/L, the Mn of 4.28g/L, the Mg of 0.52g/L) and residue 94.2g (V that wherein contains 0.85wt%).It is thus clear that the leaching yield of vanadium is 91.4%.
Contain the Tai-Ace S 150 that adds 1.12g in the vanadium leachate to said acidity and carry out dephosphorization, stirring reaction 60min after-filtration.Regulate filtrating pH value to 1.8 with the vitriol oil, add ammonium sulfate 11.00g post-heating to 95 ℃, reaction 60min under agitation condition, is dried and is obtained thick ammonium poly-vanadate at filtration.Using the 320mL mass concentration is that 10% sodium carbonate solution dissolves thick ammonium poly-vanadate, filters, obtain 318mL filtrating (wherein contain Si, the 0.03g/L of V, the 0.06g/L of 49.92g/L P,＜Mn of 0.01g/L, the Mg of 0.02g/L).Then, in filtrating, add 33.00g ammonium sulfate precipitation ammonium meta-vanadate.Ammonium meta-vanadate is calcined the 3h deaminations, acquisition Vanadium Pentoxide in FLAKES 15.91g, its V in 500 ℃ in retort furnace
2O
5Content is 98.92wt%.
In sum, the method for vanadium can stably be recycled the v element in the dephosphorization underflow slag in the recovery dephosphorization underflow slag of the present invention, and has characteristics such as vanadium recovery height, technical process weak point, stable operation.
Although combined exemplary embodiment to describe method of the present invention in detail, it will be apparent to those skilled in the art that under the situation of spirit that does not break away from claim and limited and scope, can make amendment to embodiment.
Claims (10)
1. a method that reclaims vanadium in the dephosphorization underflow slag is characterized in that, said method comprises step:
A, leach dephosphorization underflow slag, obtain acidity and contain vanadium leachate with sulphuric acid soln;
B, acidity contained vanadium leachate and carries out dephosphorization and handle after, precipitation obtains thick ammonium poly-vanadate;
C, dissolve thick ammonium poly-vanadate, obtain alkalescence and contain vanadium solution with basic solvent;
D, alkalescence is contained vanadium solution carry out precipitation and handle, obtain ammonium meta-vanadate or ammonium poly-vanadate, ammonium meta-vanadate or ammonium poly-vanadate make barium oxide behind deamination, oxidizing roasting.
2. the method for vanadium is characterized in that in the recovery dephosphorization underflow slag according to claim 1, and said dephosphorization underflow slag is meant at the slag that solution in the preparation vanadium oxide technology, that obtain through sodium roasting and water logging is carried out form when removal of impurities is handled.
3. the method for vanadium in the recovery dephosphorization underflow slag according to claim 1; It is characterized in that; Dephosphorization processing employing among the said step B contains to said acidity and adds ferric sulfate, Tai-Ace S 150 or polymeric aluminum sulfate silicate iron in the vanadium leachate as dephosphorization agent, so that the phosphoric that said acidity contains in the vanadium leachate forms deposition.
4. the method for vanadium is characterized in that in the recovery dephosphorization underflow slag according to claim 3, and the add-on of said dephosphorization agent is 4.0～5.0 calculating according to the weight ratio that said dephosphorization agent and said acidity contain the phosphoric in the vanadium leachate.
5. the method for vanadium is characterized in that in the recovery dephosphorization underflow slag according to claim 1, and the basic solvent among the said step C is sodium hydroxide solution or sodium carbonate solution.
6. the method for vanadium is characterized in that in the recovery dephosphorization underflow slag according to claim 1, and said steps A also is included in before the sulphuric acid soln leaching dephosphorization underflow slag, dephosphorization underflow slag is mixed with water, and stir and heating.
7. according to the method for vanadium in claim 1 or the 6 described recovery dephosphorization underflow slags, it is characterized in that pH was 2.0～3.0 when said use sulphuric acid soln leached dephosphorization underflow slag.
8. the method for vanadium is characterized in that in the recovery dephosphorization underflow slag according to claim 1, and the time of leaching in the said steps A is 30～60min.
9. the method for vanadium in the recovery dephosphorization underflow slag according to claim 1; It is characterized in that; Said step D adds ammonium salt and obtains ammonium meta-vanadate with deposition through directly containing in the vanadium solution to said alkalescence, perhaps contains vanadium solution to acid back and adds the ammonium salt deposition and obtain ammonium poly-vanadate through regulating said alkalescence.
10. the method for vanadium is characterized in that in the recovery dephosphorization underflow slag according to claim 1, and the pH that the dephosphorization among the said step B is handled is 2.0～3.0, and the time that dephosphorization is handled is 30～60min.
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Cited By (6)
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| CN103397209A (en) * | 2013-07-16 | 2013-11-20 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for extracting vanadium from high-calcium and high-phosphorus vanadium slag |
| CN105950877A (en) * | 2016-05-27 | 2016-09-21 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for recovering vanadium in impurity removing slag by using vanadium precipitation waste water |
| CN110042248A (en) * | 2019-04-30 | 2019-07-23 | 攀钢集团钒钛资源股份有限公司 | The method for preparing ferric vandate as raw material using dephosphorization mud |
| CN110951970A (en) * | 2019-11-28 | 2020-04-03 | 攀钢集团钒钛资源股份有限公司 | Method for recovering vanadium from vanadium-containing underflow slag |
| CN111003701A (en) * | 2019-12-20 | 2020-04-14 | 大连博融新材料有限公司 | Method for producing vanadium-doped lithium iron phosphate from vanadium industrial wastewater and vanadium-doped lithium iron phosphate |
| 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 |
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| CN102051486A (en) * | 2010-11-12 | 2011-05-11 | 攀钢集团钢铁钒钛股份有限公司 | Method for preparing low-phosphorus vanadium liquid by using wastewater subjected to vanadium precipitation |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103397209A (en) * | 2013-07-16 | 2013-11-20 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for extracting vanadium from high-calcium and high-phosphorus vanadium slag |
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| CN105950877A (en) * | 2016-05-27 | 2016-09-21 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for recovering vanadium in impurity removing slag by using vanadium precipitation waste water |
| CN110042248A (en) * | 2019-04-30 | 2019-07-23 | 攀钢集团钒钛资源股份有限公司 | The method for preparing ferric vandate as raw material using dephosphorization mud |
| CN110951970A (en) * | 2019-11-28 | 2020-04-03 | 攀钢集团钒钛资源股份有限公司 | Method for recovering vanadium from vanadium-containing underflow slag |
| CN111003701A (en) * | 2019-12-20 | 2020-04-14 | 大连博融新材料有限公司 | Method for producing vanadium-doped lithium iron phosphate from vanadium industrial wastewater and vanadium-doped lithium iron phosphate |
| 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 |
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