CN102864318A - 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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- CN102864318A CN102864318A CN2012103910156A CN201210391015A CN102864318A CN 102864318 A CN102864318 A CN 102864318A CN 2012103910156 A CN2012103910156 A CN 2012103910156A CN 201210391015 A CN201210391015 A CN 201210391015A CN 102864318 A CN102864318 A CN 102864318A
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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 the chemical industry metallurgical technical field, relate in particular to a kind of method that from contain vanadium solution, reclaims vanadium.
Background technology
Industrial from stone coal mine, clay vanadium mineral, contain vanadium solid waste etc. contain extract vanadium vanadium resource and the calcining matter thereof method take wet method as main, mostly adopt acid leaching agent (such as sulfuric acid, hydrochloric acid, nitric acid etc.) to leach, this foreign matter content height in the vanadium solution (being that acidity contains vanadium solution) that contains with the acidleach taking-up, especially silicon in the 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, silicon in the solution, when phosphorus content is 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 the precipitation rate, directly affects the yield of vanadium; And the silicon in the product, phosphorus is except the purity that affects the vanadium product, also can be to the mass formation negative influence of subsequent product such as vanadium iron, vanadium nitride etc.Therefore, before producing the vanadium product, the impurity such as silicon, phosphorus must be removed as far as possible.
Publication number is the method that the Chinese patent literature of CN102251113A discloses a kind of purifying vanadium leaching solution, be that 8.0～11.0 sodium vanadium-contained clinker leaching liquor temperature is controlled between 60 ℃ to 100 ℃ with the pH value, add dephosphorization scavenging agent sal epsom and ammonium sulfate, behind reaction 10min～20min, with sulfuric acid pH is adjusted to 5.0～8.0, adds silica removal scavenging agent aluminum sulfate aqueous solution, react 10min～20min again after, cool off, leave standstill filtration, obtain the lower solution of silicon phosphorus content.This technical scheme is divided into two stages with 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 be in the dissolution process of the leaching process of vanadium bearing slag (alkaline additive roasting material) or thick vanadium product, to add scavenging agent dephosphorization, silica removal, specifically will leach or the temperature of dissolution process is controlled between 60 ℃ to 100 ℃, regulate vanadium liquid system pH value to 8.0～12.0 with acid or alkali, then add at least a in aluminium salt, molysite or the magnesium salts and purify silica removal, dephosphorization, after question response was finished, solution cooling, filtration obtained 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.
" research that the low-grade vanadium slag of high silicon high calcium extracts Vanadium Pentoxide in FLAKES " (" rare metal ", 2011,35 (5): described a kind of method of from the low-grade vanadium slag of high silicon high calcium, extracting Vanadium Pentoxide in FLAKES 747-752).The method is to add yellow soda ash after the vanadium slag fragmentation at 700 ℃ of lower roasting 2.5h, 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 the leach liquor and phosphorus are removed.Be not difficult to find out that the method is only applicable to the vanadium resource of some particular type.
In sum, the existing method that reclaims vanadium from the solution that contains simultaneously silicon, phosphorus, vanadium all is to add under alkaline condition after silica removal, dephosphorization reagent removes silicon, phosphorus basically, carries out follow-up vanadium extraction work again.Because silica removal, dephosphorization are relatively more difficult under the acid system, so the method for from the acidic solution that contains simultaneously silicon, phosphorus, vanadium silicon, phosphorus impurities being 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, and what provide that a kind of technological process is simple, easy to operate, energy consumption is little, Impurity removal is effective, quality product is high contains the method that reclaims vanadium the vanadium solution from acidity siliceous, phosphorus.
For solving the problems of the technologies described above, the technical scheme that the present invention proposes is a kind ofly to contain the method that reclaims vanadium the vanadium solution from acidity siliceous, phosphorus, may further comprise the steps:
(1) the pH value that described acidity is contained vanadium solution adjusts to 1.0～2.5; In this step, acidity contains the pH value of vanadium solution less than 1.0 o'clock available bases (preferred Na
2CO
3, NaOH or ammoniacal liquor) adjustment of acidity contains the pH value of vanadium solution, alkali can add by solid form, also can aqueous solution form add;
(2) acidity behind the adjust pH is contained flow through weak base anion-exchange resin or strongly basic anion exchange resin of vanadium solution and adsorb (adsorption process can be carried out at normal temperatures);
(3) carry out desorb with weak base anion-exchange resin or the strongly basic anion exchange resin of strong base solution after to step (2);
(4) purify with solubility magnesium salts and/or the calcium salt stripping liquid after to step (3), remove wherein silicon, phosphorus (the pH value in the scavenging process preferably is controlled at 8.0～10.0);
(5) scavenging solution that obtains after to step (4) with ammonium salt carries out precipitation to be processed; The pH value of scavenging solution preferably was controlled at 8.0～10.0 before precipitation was processed;
(6) the vanadium precipitation that contains that obtains after the step (5) is calcined, reclaim and obtain the highly purified vanadium product that contains.
Above-mentioned contain the method that reclaims vanadium the vanadium solution from acidity siliceous, phosphorus, preferred, described acidity contains the mass ratio SiO of silicon-dioxide and Vanadium Pentoxide in FLAKES in the vanadium solution
2/ V
2O
5≤ 1.0.
Above-mentioned contains the method that reclaims vanadium the vanadium solution from acidity siliceous, phosphorus, in the 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 the method that reclaims vanadium the vanadium solution from acidity siliceous, phosphorus, and in the described step (3), described strong base solution refers to that preferably concentration is the NaOH solution of 50g/L～150g/L.
Above-mentioned contains the method that reclaims vanadium the vanadium solution from acidity siliceous, phosphorus, and in the described step (3), the temperature during desorb preferably is controlled at 20 ℃～65 ℃, is more preferably under 20 ℃～55 ℃ or 30 ℃～40 ℃ and carries out.
Above-mentioned contains the method that reclaims vanadium the vanadium solution from acidity siliceous, phosphorus, and in the described step (4), described magnesium salts is preferably magnesium chloride, sal epsom, 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 the precipitation stripping liquid 1.0～1.5 times.
Above-mentioned contains the method that reclaims vanadium the vanadium solution from acidity siliceous, phosphorus, and in the 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 that vanadium, silicon, the phosphorus that acidity contains in the vanadium solution is adsorbed simultaneously, then with alkali ion exchange resin is carried out desorb, in stripping liquid, utilize chemical precipitation method to remove silicon, phosphorus, can obtain containing vanadium product Vanadium Pentoxide in FLAKES finally by calcining.Method of the present invention has at first been simplified the process for extracting vanadium process, has improved process efficiency; Because the 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 the 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.
Description of drawings
Fig. 1 is process flow sheet of the present invention.
Embodiment
The invention will be further described with concrete preferred embodiment below in conjunction with Figure of description, but protection domain not thereby limiting the invention.
Embodiment 1:
A kind of as shown in Figure 1 contain the vanadium solution method that reclaims vanadium from acidity siliceous, phosphorus, may further comprise the steps:
(1) gets and contain SiO
21.8g/L, P 2.89g/L, V
2O
53.52g/L and the pH value is that 0.8 acidity contains vanadium solution 2.5L, uses solid Na under agitation condition
2CO
3Regulate this acidity and contain the pH value to 1.5 of vanadium solution;
(2) acidity behind the adjust pH is contained the vanadium solution weak base anion-exchange resin (D301 resin) of flowing through and adsorb, absorption duration of contact is that the 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) be that the NaOH solution of the 150g/L D301 resin after to step (2) carries out desorb with concentration, the temperature during desorb is controlled at 35 ℃; After testing, V
2O
5Desorption efficiency be 99.3%, V in the 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 wherein silicon, phosphorus; MgCl
26H
2The addition of O is 1.0 times of silicon, the required theoretical amount of phosphorus in the precipitation stripping liquid, and controlling the pH value with NaOH in the scavenging process is 8.0～10.0, stirs 1.0h, filters to get scavenging solution; After testing, V in the scavenging process
2O
5The rate of recovery is 99.5%, and the silicon clearance is 98.8%, and tp removal rate is 99.6%;
(5) scavenging solution that obtains after to step (4) with ammonium salt carries out precipitation to be processed; The pH value of scavenging solution was controlled at 8.0～10.0 before precipitation was processed; The amount that scavenging solution is pressed 80g/L adds NH
4Stir 1.0h behind the Cl, ageing 12.0h filters V in the precipitation treating processes
2O
5Deposition rate is 99.6%;
(6) the vanadium filter cake that contains that obtains after the step (5) is carried out drying, place again 550 ℃ of temperature lower calcination 2.0h, obtain grade after the recovery and be 99.3% golden yellow powdery Vanadium Pentoxide in FLAKES product.
Embodiment 2:
A kind of as shown in Figure 1 contain the vanadium solution method that reclaims vanadium from acidity siliceous, phosphorus, may further comprise the steps:
(1) gets and contain SiO
21.8g/L, P 2.89g/L, V
2O
53.52g/L and the pH value is that 0.8 acidity contains vanadium solution 2.5L, uses solid Na under agitation condition
2CO
3Regulate this acidity and contain the pH value to 1.8 of vanadium solution;
(2) acidity behind the adjust pH is contained the vanadium solution weak base anion-exchange resin (D314 resin) of flowing through and adsorb, absorption duration of contact is that the 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) be that the NaOH solution of the 135g/L D314 resin after to step (2) carries out desorb with concentration, the temperature during desorb is controlled at 40 ℃; After testing, V
2O
5Desorption efficiency is 99.2%, V in the 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 wherein silicon, phosphorus; MgCl
26H
2The addition of O is 1.2 times of silicon, the required theoretical amount of phosphorus in the precipitation stripping liquid, and controlling the pH value with NaOH in the scavenging process is 8.0～10.0, stirs 1.0h, filters to get scavenging solution; After testing, V in the scavenging process
2O
5The rate of recovery is 99.6%, and the silicon clearance is 98.9%, and tp removal rate is 99.6%;
(5) scavenging solution that obtains after to step (4) with ammonium salt carries out precipitation to be processed; The pH value of scavenging solution was controlled at 8.0～10.0 before precipitation was processed; The amount that scavenging solution is pressed 80g/L adds NH
4Stir 1.0h behind the Cl, ageing 12.0h filters V in the precipitation treating processes
2O
5Deposition rate is 99.4%;
(6) the vanadium filter cake that contains that obtains after the step (5) is carried out drying, place again 550 ℃ of temperature lower calcination 2.0h, obtain grade after the recovery and be 99.4% golden yellow powdery Vanadium Pentoxide in FLAKES product.
Embodiment 3:
A kind of as shown in Figure 1 contain the vanadium solution method that reclaims vanadium from acidity siliceous, phosphorus, may further comprise the steps:
(1) gets and contain SiO
20.60g/L, P 4.82g/L, V
2O
54.20g/L and the pH value is that 0.5 acidity contains vanadium solution 2.5L, regulates the pH value to 2.0 that this acidity contains vanadium solution with solid NaOH under agitation condition;
(2) acidity behind the adjust pH is contained the vanadium solution strongly basic anion exchange resin (D201 resin) of flowing through and adsorb, absorption duration of contact is that the 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) be that the NaOH solution of the 120g/L D201 resin after to step (2) carries out desorb with concentration, the temperature during desorb is controlled at 40 ℃; After testing, V
2O
5Desorption efficiency is 99.2%, V in the 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 wherein silicon, phosphorus; MgSO
47H
2The addition of O is 1.1 times of silicon, the required theoretical amount of phosphorus in the precipitation stripping liquid, and controlling the pH value with NaOH in the scavenging process is 8.0～10.0, stirs 1.0h, filters to get scavenging solution; After testing, V in the scavenging process
2O
5The rate of recovery is 99.6%, and the silicon clearance is 98.5%, and tp removal rate is 99.5%;
(5) scavenging solution that obtains after to step (4) with ammonium salt carries out precipitation to be processed; The pH value of scavenging solution was controlled at 8.0～10.0 before precipitation was processed; The amount that scavenging solution is pressed 80g/L adds NH
4Stir 1.0h behind the Cl, ageing 12.0h filters V in the precipitation treating processes
2O
5Deposition rate is 99.5%;
(6) the vanadium filter cake that contains that obtains after the step (5) is carried out drying, place again 550 ℃ of temperature lower calcination 2.0h, obtain grade after the recovery and be 99.2% golden yellow powdery Vanadium Pentoxide in FLAKES product.
Embodiment 4:
A kind of as shown in Figure 1 contain the vanadium solution method that reclaims vanadium from acidity siliceous, phosphorus, may further comprise the steps:
(1) gets and contain SiO
20.60g/L, P 4.82g/L, V
2O
54.20g/L and the pH value is that 0.5 acidity contains vanadium solution 2.5L, regulates the pH value to 2.2 that this acidity contains vanadium solution with solid NaOH under agitation condition;
(2) acidity behind the adjust pH is contained the vanadium solution strongly basic anion exchange resin (201 resin) of flowing through and adsorb, absorption duration of contact is that the 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) be that the NaOH solution of 100g/L 201 resins after to step (2) carry out desorb with concentration, the temperature during desorb is controlled at 55 ℃; After testing, V
2O
5Desorption efficiency is 99.2%, V in the 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 the step (3) is purified, remove wherein silicon, phosphorus; CaCl
2Addition be silicon, the required theoretical amount of phosphorus in the precipitation stripping liquid 1.2 times, stir 1.0h, filter to get scavenging solution; After testing, V in the scavenging process
2O
5The rate of recovery is 99.0%, and the silicon clearance is 98.2%, and tp removal rate is 99.6%;
(5) scavenging solution that obtains after to step (4) with ammonium salt carries out precipitation to be processed; The pH value of scavenging solution was controlled at 8.0～10.0 before precipitation was processed; The amount that scavenging solution is pressed 80g/L adds NH
4Stir 1.0h behind the Cl, ageing 12.0h filters V in the precipitation treating processes
2O
5Deposition rate is 99.6%;
(6) the vanadium filter cake that contains that obtains after the step (5) is carried out drying, place again 550 ℃ of temperature lower calcination 2.0h, obtain grade after the recovery and be 99.3% golden yellow powdery Vanadium Pentoxide in FLAKES product.
Claims (10)
1. one kind contains the vanadium solution method that reclaims vanadium from acidity siliceous, phosphorus, may further comprise the steps:
(1) the pH value that described acidity is contained vanadium solution adjusts to 1.0～2.5;
(2) acidity behind the adjust pH being contained flow through weak base anion-exchange resin or strongly basic anion exchange resin of vanadium solution adsorbs;
(3) carry out desorb with weak base anion-exchange resin or the strongly basic anion exchange resin of strong base solution after to step (2);
(4) purify with solubility magnesium salts and/or the calcium salt stripping liquid after to step (3), remove wherein silicon, phosphorus;
(5) scavenging solution that obtains after to step (4) with ammonium salt carries out precipitation to be processed;
(6) the vanadium precipitation that contains that obtains after the step (5) is calcined, reclaim and obtain the highly purified vanadium product that contains.
2. according to claim 1ly contain the vanadium solution method that reclaims vanadium from acidity siliceous, phosphorus, it is characterized in that: described acidity contains the mass ratio SiO of silicon-dioxide and Vanadium Pentoxide in FLAKES in the vanadium solution
2/ V
2O
5≤ 1.0.
3. according to claim 1ly contain the vanadium solution method that reclaims vanadium from acidity siliceous, phosphorus, it is characterized in that: described acidity contains the pH value of vanadium solution less than 1.0, is employing Na in the described step (1)
2CO
3, NaOH or ammoniacal liquor carries out the adjustment of pH value.
4. according to claim 1ly contain the vanadium solution method that reclaims vanadium from acidity siliceous, phosphorus, it is characterized in that: in the 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.
5. according to claim 1ly contain the vanadium solution method that reclaims vanadium from acidity siliceous, phosphorus, it is characterized in that: in the described step (3), described strong base solution refers to that concentration is the NaOH solution of 50g/L～150g/L.
6. each describedly contains the vanadium solution method that reclaims vanadium from acidity siliceous, phosphorus according to claim 1～4, and it is characterized in that: in the described step (3), the temperature during desorb is controlled at 20 ℃～65 ℃.
7. according to claim 5ly contain the vanadium solution method that reclaims vanadium from acidity siliceous, phosphorus, it is characterized in that: in the described step (3), the temperature during desorb is controlled at 20 ℃～55 ℃.
8. each describedly contains the vanadium solution method that reclaims vanadium from acidity siliceous, phosphorus according to claim 1～4, and it is characterized in that: in the described step (4), described magnesium salts is magnesium chloride, sal epsom, 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 the precipitation stripping liquid.
9. each describedly contains the vanadium solution method that reclaims vanadium from acidity siliceous, phosphorus according to claim 1～4, it is characterized in that: in the described step (5), the scavenging solution before precipitation processed is adjusted to 8.0～10.0 with its pH value first.
10. according to claim 9ly contain the vanadium solution method that reclaims vanadium from acidity siliceous, phosphorus, it is characterized in that: in the described step (5), described ammonium salt is ammonium chloride.
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| CN103613167A (en) * | 2013-11-07 | 2014-03-05 | 河南盛锐钒业集团有限公司 | Infinite cyclic utilization technology of acidic vanadium mother liquor ion exchange tail water |
| CN103787414A (en) * | 2014-01-26 | 2014-05-14 | 贵州义信矿业有限公司 | Method of preparing high-purity vanadium pentoxide from roasting-method vanadium solution |
| CN103803649A (en) * | 2014-02-28 | 2014-05-21 | 重庆大学 | Method for settling vanadium by using acidic vanadium solution |
| CN104046799A (en) * | 2013-12-03 | 2014-09-17 | 攀钢集团攀枝花钢铁研究院有限公司 | Dephosphorization agent, and preparation method and application thereof |
| CN104843789A (en) * | 2015-04-30 | 2015-08-19 | 河北钢铁股份有限公司承德分公司 | Method for purifying vanadium pentoxide |
| WO2015161660A1 (en) * | 2014-04-21 | 2015-10-29 | 中国科学院过程工程研究所 | Method for preparing low-silicon vanadium pentoxide from solution containing vanadium, chromium and silicon |
| CN105331832A (en) * | 2015-11-27 | 2016-02-17 | 攀钢集团攀枝花钢铁研究院有限公司 | Acid-leaching washing method for vanadium-containing roasting clinker |
| CN113106270A (en) * | 2021-03-26 | 2021-07-13 | 西部矿业股份有限公司 | Method for efficiently recovering vanadium based on modified acid leaching of vanadium-containing metallurgical slag |
| 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 |
| CN114959308A (en) * | 2022-05-11 | 2022-08-30 | 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 |
| CN115286038A (en) * | 2022-08-08 | 2022-11-04 | 吉林吉恩镍业股份有限公司 | Method for producing ammonium metavanadate by taking phosphorus removal slag as raw material |
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