CN102864318B - Method for recycling vanadium from acid vanadium-containing solution containing silicon and phosphorus - Google Patents
Method for recycling vanadium from acid vanadium-containing solution containing silicon and phosphorus Download PDFInfo
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Abstract
The invention discloses a method for recycling vanadium from an acid vanadium-containing solution containing silicon and phosphorus. The method includes that a pH value of an acid vanadium-containing solution is adjusted in a range from 1.0 to 2.5, the acid vanadium-containing solution with an adjusted pH value passes through weak-base anion-exchange resins or strong-base anion exchange resins to be absorbed, a strong alkali solution is used to desorb the weak-base anion-exchange resins or the strong-base anion exchange resins after adsorption, soluble magnesium salt and/or calcium salt is used to purify a desorption solution after desorption and silicon to remove phosphorus in the solution, ammonium salt is used to perform vanadium precipitation on a purified solution obtained after purification, vanadium-containing precipitation obtained after vanadium precipitation is calcined, and high- purity vanadium-containing products are recycled. The method has the advantages that the technological process is simple, the operation is convenient, the energy consumption is low, the impurity removing effect is good, the product quality is high and the like.
Description
Technical field
The invention belongs to chemical industry metallurgical technical field, relate in particular to a kind of from the method containing reclaiming vanadium vanadium solution.
Background technology
Industrial from stone coal mine, clay vanadium mineral, take wet method as main containing vanadium solid waste etc. containing the method for extracting vanadium vanadium resource and calcining matter thereof, mostly adopt acid leaching agent (as sulfuric acid, hydrochloric acid, nitric acid etc.) to leach, this take out with acidleach high containing foreign matter content in vanadium solution (acid containing vanadium solution), especially silicon in solution, phosphorus content are higher, this not only directly affects carrying out smoothly of follow-up process for extracting vanadium, and affects the quality of final vanadium product.For example, when silicon in solution, phosphorus content are higher, the enrichment stage can be caused the obstruction of spe medium generation emulsification and ion exchange column, makes vanadium extracting process be difficult to carry out; The precipitation stage can be reduced precipitation rate, directly affects the yield of vanadium; And silicon in product, phosphorus is except affecting the purity of vanadium product, also can be to subsequent product as the mass formation negative influence of vanadium iron, vanadium nitride etc.Therefore, before producing vanadium product, the impurity such as silicon, phosphorus must be removed as far as possible.
Publication number is a kind of method that the Chinese patent literature of CN102251113A discloses purifying vanadium leaching solution, the sodium vanadium-contained clinker leaching liquor temperature that is 8.0～11.0 by pH value is controlled between 60 ℃ to 100 ℃, add dephosphorization scavenging agent magnesium sulfate and ammonium sulfate, after reaction 10min～20min, with sulfuric acid, pH is adjusted to 5.0～8.0, add silica removal scavenging agent aluminum sulfate aqueous solution, then react after 10min～20min, cooling, standing filtration, obtains the solution that silicon phosphorus content is lower.This technical scheme is divided into two stages by purification and impurity removal and removes respectively silicon, phosphorus, and temperature is controlled at 60 ℃ to 100 ℃, and process is comparatively complicated, and energy consumption is higher.
Publication number is that the Chinese patent literature of CN101724757A discloses a kind of method of producing low-silicon and low-phosphorous vanadium liquid, mainly to add scavenging agent dephosphorization, silica removal in the leaching process of vanadium bearing slag (alkaline additive roasting material) or the dissolution process of thick vanadium product, specifically the temperature of leaching or dissolution process is controlled between 60 ℃ to 100 ℃, with acid or alkali, regulate vanadium liquid system pH value to 8.0～12.0, then add at least one in aluminium salt, molysite or magnesium salts to purify silica removal, dephosphorization, after question response completes, solution is cooling, filtration obtains low-silicon and low-phosphorous vanadium liquid.Although the method can a step be removed silicon, phosphorus, process temperature is controlled at 60 ℃ to 100 ℃ equally, and energy consumption is also higher.
The low-grade vanadium slag of the high silicon high calcium of < < extracts research > > (the < < rare metal > > of Vanadium Pentoxide in FLAKES, 2011,35 (5): 747-752), described a kind of method of extracting Vanadium Pentoxide in FLAKES from the low-grade vanadium slag of high silicon high calcium.The method is after vanadium slag fragmentation, to add sodium carbonate roasting 2.5h at 700 ℃, make silicon and phosphorus be separately converted to sodium phosphate and water glass, then adopt the method for water logging, make sodium phosphate, water glass and the reaction of vanadic acid calcium generate insoluble Calucium Silicate powder and calcium phosphate, thereby the silicon in leach liquor and phosphorus are removed.Be not difficult to find out, the method is only applicable to the vanadium resource of some particular type.
In sum, the existing method that reclaims vanadium from simultaneously contain the solution of silicon, phosphorus, vanadium, is all after adding silica removal, dephosphorization reagent that silicon, phosphorus are removed under alkaline condition substantially, then carries out follow-up vanadium extraction work.Because silica removal under acid system, dephosphorization are more difficult, thus from contain the acidic solution of silicon, phosphorus, vanadium simultaneously by silicon, the phosphorus impurities method separated with vanadium, rare report.
Summary of the invention
The technical problem to be solved in the present invention is to overcome the deficiencies in the prior art, provide that a kind of technological process is simple, easy to operate, energy consumption is little, Impurity removal is effective, quality product is high from the acidity of siliceous, phosphorus containing the method that reclaims vanadium vanadium solution.
For solving the problems of the technologies described above, the technical scheme that the present invention proposes be a kind of from the acidity of siliceous, phosphorus containing the method that reclaims vanadium vanadium solution, comprise the following steps:
(1) described acidity is adjusted to 1.0～2.5 containing the pH value of vanadium solution; In this step, the acid pH value containing vanadium solution is less than 1.0 o'clock available bases (preferred Na
2cO
3, NaOH or ammoniacal liquor) adjustment of acidity is containing the pH value of vanadium solution, alkali can add by solid form, also can aqueous solution form add;
(2) acidity after adjust pH is adsorbed to (adsorption process can be carried out at normal temperatures) containing flow through weak base anion-exchange resin or strongly basic anion exchange resin of vanadium solution;
(3) with strong base solution, weak base anion-exchange resin or the strongly basic anion exchange resin after to step (2) carries out desorb;
(4) with solubility magnesium salts and/or calcium salt, the stripping liquid after to step (3) purifies, and removes silicon, phosphorus (the pH value in scavenging process is preferably controlled at 8.0～10.0) wherein;
(5) scavenging solution obtaining after to step (4) with ammonium salt carries out precipitation processing; The pH value that front scavenging solution is processed in precipitation is preferably controlled at 8.0～10.0;
(6), by calcining containing vanadium precipitation of obtaining after step (5), reclaim and obtain the highly purified vanadium product that contains.
Above-mentioned contains from acidity siliceous, phosphorus the method that reclaims vanadium vanadium solution, and preferred, described acidity is containing the mass ratio SiO of silicon-dioxide in vanadium solution and Vanadium Pentoxide in FLAKES
2/ V
2o
5≤ 1.0.
Above-mentioned contains from acidity siliceous, phosphorus the method that reclaims vanadium vanadium solution, in described step (2), described strongly basic anion exchange resin is preferably 201 resins or D201 resin, and described weak base anion-exchange resin is preferably D301 resin, D311 resin or D314 resin.
Above-mentioned contains from acidity siliceous, phosphorus the method that reclaims vanadium vanadium solution, and in described step (3), described strong base solution preferably refers to that concentration is the NaOH solution of 50g/L～150g/L.
Above-mentioned contains from acidity siliceous, phosphorus the method that reclaims vanadium vanadium solution, and in described step (3), temperature during desorb is preferably controlled at 20 ℃～65 ℃, is more preferably at 20 ℃～55 ℃ or 30 ℃～40 ℃ and carries out.
Above-mentioned contains from acidity siliceous, phosphorus the method that reclaims vanadium vanadium solution, and in described step (4), described magnesium salts is preferably magnesium chloride, magnesium sulfate, magnesium sulfate hydrate or magnesium chloride hydrate; Described calcium salt is preferably calcium chloride or calcium chloride hydrate; The addition of described magnesium salts or calcium salt is preferably silicon, the required theoretical amount of phosphorus in precipitation stripping liquid 1.0～1.5 times.
Above-mentioned contains from acidity siliceous, phosphorus the method that reclaims vanadium vanadium solution, and in described step (5), described ammonium salt is preferably ammonium chloride.
Compared with prior art, the invention has the advantages that: the present invention directly utilizes ion exchange resin to adsorb containing vanadium, silicon, phosphorus in vanadium solution acidity simultaneously, then with alkali, ion exchange resin is carried out to desorb, in stripping liquid, utilize chemical precipitation method to remove silicon, phosphorus, finally by calcining, can obtain containing vanadium product Vanadium Pentoxide in FLAKES.First method of the present invention has simplified process for extracting vanadium process, has improved process efficiency; Because sorption and desorption process all can be carried out at a lower temperature, this has not only reduced energy consumption, and has solved smoothly the problem of phosphate crystal obstruction exchange column in desorption process.The Vanadium Pentoxide in FLAKES product that the present invention finally obtains is purity high (can reach more than 99%) not only, and the rate of recovery of vanadium is high.
Accompanying drawing explanation
Fig. 1 is process flow sheet of the present invention.
Embodiment
Below in conjunction with Figure of description, the invention will be further described with concrete preferred embodiment, but protection domain not thereby limiting the invention.
embodiment 1:
The acidity from siliceous, phosphorus as shown in Figure 1, containing reclaiming a method for vanadium vanadium solution, comprises the following steps:
(1) get and contain SiO
21.8g/L, P 2.89g/L, V
2o
5the acidity that 3.52g/L and pH value are 0.8, containing vanadium solution 2.5L, is used solid Na under agitation condition
2cO
3regulate this acidity containing the pH value to 1.5 of vanadium solution;
(2) acidity after adjust pH is adsorbed containing the vanadium solution weak base anion-exchange resin (D301 resin) of flowing through, absorption duration of contact is that 10min(adsorption process can be carried out at normal temperatures), after testing, V
2o
5adsorption rate is 98.6%, SiO
2adsorption rate is that 30.1%, P adsorption rate is 27.3%;
(3) the D301 resin of the NaOH solution that is 150g/L by concentration after to step (2) carries out desorb, and temperature during desorb is controlled at 35 ℃; After testing, V
2o
5desorption efficiency be 99.3%, V in stripping liquid
2o
5concentration be 75.2g/L, SiO
2concentration be that the concentration of 11.8g/L, P is 16.5g/L; The pH value of stripping liquid is 9.2;
(4) with solubility magnesium salts MgCl
26H
2the stripping liquid of O after to step (3) purifies, and removes silicon, phosphorus wherein; MgCl
26H
2the addition of O is 1.0 times of silicon, the required theoretical amount of phosphorus in precipitation stripping liquid, and in scavenging process, with NaOH, controlling pH value is 8.0～10.0, stirs 1.0h, filters to obtain scavenging solution; After testing, V in scavenging process
2o
5the rate of recovery is 99.5%, and silicon clearance is 98.8%, and tp removal rate is 99.6%;
(5) scavenging solution obtaining after to step (4) with ammonium salt carries out precipitation processing; The pH value that front scavenging solution is processed in precipitation is controlled at 8.0～10.0; Scavenging solution adds NH by the amount of 80g/L
4after Cl, stir 1.0h, ageing 12.0h, filters V in precipitation treating processes
2o
5deposition rate is 99.6%;
(6) by being dried containing vanadium filter cake of obtaining after step (5), then be placed in 550 ℃ of temperature lower calcination 2.0h, after recovery, obtain grade and be 99.3% golden yellow powdery Vanadium Pentoxide in FLAKES product.
embodiment 2:
The acidity from siliceous, phosphorus as shown in Figure 1, containing reclaiming a method for vanadium vanadium solution, comprises the following steps:
(1) get and contain SiO
21.8g/L, P 2.89g/L, V
2o
5the acidity that 3.52g/L and pH value are 0.8, containing vanadium solution 2.5L, is used solid Na under agitation condition
2cO
3regulate this acidity containing the pH value to 1.8 of vanadium solution;
(2) acidity after adjust pH is adsorbed containing the vanadium solution weak base anion-exchange resin (D314 resin) of flowing through, absorption duration of contact is that 10min(adsorption process can be carried out at normal temperatures), after testing, V
2o
5adsorption rate is 99.0%, SiO
2adsorption rate is that 27.2%, P adsorption rate is 28.0%;
(3) the D314 resin of the NaOH solution that is 135g/L by concentration after to step (2) carries out desorb, and temperature during desorb is controlled at 40 ℃; After testing, V
2o
5desorption efficiency is 99.2%, V in stripping liquid
2o
5concentration be 73.5g/L, SiO
2concentration be that the concentration of 10.33g/L, P is 17.01g/L; The pH value of stripping liquid is 9.0;
(4) with solubility magnesium salts MgCl
26H
2the stripping liquid of O after to step (3) purifies, and removes silicon, phosphorus wherein; MgCl
26H
2the addition of O is 1.2 times of silicon, the required theoretical amount of phosphorus in precipitation stripping liquid, and in scavenging process, with NaOH, controlling pH value is 8.0～10.0, stirs 1.0h, filters to obtain scavenging solution; After testing, V in scavenging process
2o
5the rate of recovery is 99.6%, and silicon clearance is 98.9%, and tp removal rate is 99.6%;
(5) scavenging solution obtaining after to step (4) with ammonium salt carries out precipitation processing; The pH value that front scavenging solution is processed in precipitation is controlled at 8.0～10.0; Scavenging solution adds NH by the amount of 80g/L
4after Cl, stir 1.0h, ageing 12.0h, filters V in precipitation treating processes
2o
5deposition rate is 99.4%;
(6) by being dried containing vanadium filter cake of obtaining after step (5), then be placed in 550 ℃ of temperature lower calcination 2.0h, after recovery, obtain grade and be 99.4% golden yellow powdery Vanadium Pentoxide in FLAKES product.
embodiment 3:
The acidity from siliceous, phosphorus as shown in Figure 1, containing reclaiming a method for vanadium vanadium solution, comprises the following steps:
(1) get and contain SiO
20.60g/L, P 4.82g/L, V
2o
5the acidity that 4.20g/L and pH value are 0.5, containing vanadium solution 2.5L, regulates this acidity containing the pH value to 2.0 of vanadium solution with solid NaOH under agitation condition;
(2) acidity after adjust pH is adsorbed containing the vanadium solution strongly basic anion exchange resin (D201 resin) of flowing through, absorption duration of contact is that 15min(adsorption process can be carried out at normal temperatures), after testing, V
2o
5adsorption rate is 99.2%, SiO
2adsorption rate is that 20.1%, P adsorption rate is 28.5%;
(3) the D201 resin of the NaOH solution that is 120g/L by concentration after to step (2) carries out desorb, and temperature during desorb is controlled at 40 ℃; After testing, V
2o
5desorption efficiency is 99.2%, V in stripping liquid
2o
5concentration be 65.30g/L, SiO
2concentration be that the concentration of 1.82g/L, P is 18.74g/L; The pH value of stripping liquid is 9.0;
(4) with solubility magnesium salts MgSO
47H
2the stripping liquid of O after to step (3) purifies, and removes silicon, phosphorus wherein; MgSO
47H
2the addition of O is 1.1 times of silicon, the required theoretical amount of phosphorus in precipitation stripping liquid, and in scavenging process, with NaOH, controlling pH value is 8.0～10.0, stirs 1.0h, filters to obtain scavenging solution; After testing, V in scavenging process
2o
5the rate of recovery is 99.6%, and silicon clearance is 98.5%, and tp removal rate is 99.5%;
(5) scavenging solution obtaining after to step (4) with ammonium salt carries out precipitation processing; The pH value that front scavenging solution is processed in precipitation is controlled at 8.0～10.0; Scavenging solution adds NH by the amount of 80g/L
4after Cl, stir 1.0h, ageing 12.0h, filters V in precipitation treating processes
2o
5deposition rate is 99.5%;
(6) by being dried containing vanadium filter cake of obtaining after step (5), then be placed in 550 ℃ of temperature lower calcination 2.0h, after recovery, obtain grade and be 99.2% golden yellow powdery Vanadium Pentoxide in FLAKES product.
embodiment 4:
The acidity from siliceous, phosphorus as shown in Figure 1, containing reclaiming a method for vanadium vanadium solution, comprises the following steps:
(1) get and contain SiO
20.60g/L, P 4.82g/L, V
2o
5the acidity that 4.20g/L and pH value are 0.5, containing vanadium solution 2.5L, regulates this acidity containing the pH value to 2.2 of vanadium solution with solid NaOH under agitation condition;
(2) acidity after adjust pH is adsorbed containing the vanadium solution strongly basic anion exchange resin (201 resin) of flowing through, absorption duration of contact is that 15min(adsorption process can be carried out at normal temperatures), after testing, V
2o
5adsorption rate is 99.2%, SiO
2adsorption rate is that 19.8%, P adsorption rate is 28.6%;
(3) 201 resins of the NaOH solution that is 100g/L by concentration after to step (2) carry out desorb, and temperature during desorb is controlled at 55 ℃; After testing, V
2o
5desorption efficiency is 99.2%, V in stripping liquid
2o
5concentration be 70.4g/L, SiO
2concentration be that the concentration of 2.02g/L, P is 23.24g/L; The pH value of stripping liquid is 9.5;
(4) use soluble solids CaCl
2stripping liquid after step (3) is purified, remove silicon, phosphorus wherein; CaCl
2addition be silicon, the required theoretical amount of phosphorus in precipitation stripping liquid 1.2 times, stir 1.0h, filter to obtain scavenging solution; After testing, V in scavenging process
2o
5the rate of recovery is 99.0%, and silicon clearance is 98.2%, and tp removal rate is 99.6%;
(5) scavenging solution obtaining after to step (4) with ammonium salt carries out precipitation processing; The pH value that front scavenging solution is processed in precipitation is controlled at 8.0～10.0; Scavenging solution adds NH by the amount of 80g/L
4after Cl, stir 1.0h, ageing 12.0h, filters V in precipitation treating processes
2o
5deposition rate is 99.6%;
(6) by being dried containing vanadium filter cake of obtaining after step (5), then be placed in 550 ℃ of temperature lower calcination 2.0h, after recovery, obtain grade and be 99.3% golden yellow powdery Vanadium Pentoxide in FLAKES product.
Claims (7)
1. from acidity siliceous, phosphorus, contain a method that reclaims vanadium vanadium solution, comprise the following steps:
(1) described acidity is less than 1.0 containing the pH value of vanadium solution, and described acidity is adjusted to 1.0～2.5 containing the pH value of vanadium solution; Described acidity is containing the mass ratio SiO of silicon-dioxide in vanadium solution and Vanadium Pentoxide in FLAKES
2/ V
2o
5≤ 1.0;
(2) acidity after adjust pH is adsorbed containing flow through weak base anion-exchange resin or strongly basic anion exchange resin of vanadium solution;
(3) with strong base solution, weak base anion-exchange resin or the strongly basic anion exchange resin after to step (2) carries out desorb; Temperature during desorb is controlled at 30 ℃～40 ℃;
(4) with solubility magnesium salts and/or calcium salt, the stripping liquid after to step (3) purifies, and removes silicon, phosphorus wherein;
(5) scavenging solution obtaining after to step (4) with ammonium salt carries out precipitation processing;
(6), by calcining containing vanadium precipitation of obtaining after step (5), reclaim and obtain the highly purified vanadium product that contains.
2. the acidity from siliceous, phosphorus according to claim 1, containing reclaiming the method for vanadium vanadium solution, is characterized in that: in described step (1), be to adopt Na
2cO
3, NaOH or ammoniacal liquor carries out the adjustment of pH value.
3. the acidity from siliceous, phosphorus according to claim 1 is containing reclaiming the method for vanadium vanadium solution, it is characterized in that: in described step (2), described strongly basic anion exchange resin is 201 resins or D201 resin, and described weak base anion-exchange resin is D301 resin, D311 resin or D314 resin.
4. the acidity from siliceous, phosphorus according to claim 1, containing reclaiming the method for vanadium vanadium solution, is characterized in that: in described step (3), described strong base solution refers to that concentration is the NaOH solution of 50g/L～150g/L.
According to the acidity from siliceous, phosphorus described in any one in claim 1～4 containing reclaiming the method for vanadium vanadium solution, it is characterized in that: in described step (4), described magnesium salts is magnesium chloride, magnesium sulfate, magnesium sulfate hydrate or magnesium chloride hydrate; Described calcium salt is calcium chloride or calcium chloride hydrate; The addition of described magnesium salts or calcium salt is 1.0～1.5 times of silicon, the required theoretical amount of phosphorus in precipitation stripping liquid.
According to the acidity from siliceous, phosphorus described in any one in claim 1～4 containing reclaiming the method for vanadium vanadium solution, it is characterized in that: in described step (5), the scavenging solution before precipitation is processed is first adjusted to 8.0～10.0 by its pH value.
7. the acidity from siliceous, phosphorus according to claim 6, containing reclaiming the method for vanadium vanadium solution, is characterized in that: in described step (5), described ammonium salt is ammonium chloride.
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| CN104046799B (en) * | 2013-12-03 | 2015-07-08 | 攀钢集团攀枝花钢铁研究院有限公司 | Dephosphorization agent, and preparation method and application thereof |
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| CN113481389A (en) * | 2021-06-02 | 2021-10-08 | 四川星明能源环保科技有限公司 | Method for removing phosphorus from vanadium-containing solution with high phosphorus content |
| CN114959308B (en) * | 2022-05-11 | 2023-10-27 | 西安西北有色地质研究院有限公司 | Ion exchange vanadium extraction method for high-iron low-vanadium solution |
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| CN101838749A (en) * | 2010-06-10 | 2010-09-22 | 中南大学 | Ion exchange extraction vanadium method of vanadium-containing solution |
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