CN105925821A - Impurity removal and vanadium recycle method for high-acid-concentration vanadium-containing solution - Google Patents
Impurity removal and vanadium recycle method for high-acid-concentration vanadium-containing solution Download PDFInfo
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- CN105925821A CN105925821A CN201610524900.5A CN201610524900A CN105925821A CN 105925821 A CN105925821 A CN 105925821A CN 201610524900 A CN201610524900 A CN 201610524900A CN 105925821 A CN105925821 A CN 105925821A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B34/00—Obtaining refractory metals
- C22B34/20—Obtaining niobium, tantalum or vanadium
- C22B34/22—Obtaining vanadium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/44—Treatment or purification of solutions, e.g. obtained by leaching by chemical processes
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Abstract
The invention discloses an impurity removal and vanadium recycle method for a high-acid-concentration vanadium-containing solution. The vanadium-containing solution with the acid concentration, calculated by sulfuric acid, ranging from 0.1% to 20% is added to a certain amount of alkali liquor, the pH value of a system is kept being 2 to 8, a stirring reaction is performed for 0.5 h to 6 h at the temperature ranging from 20 DEG C to 100 DEG C, filtration is conducted after the reaction ends, and filter residues and vanadium-containing filtrate are obtained; the filter residues are washed with acid liquor or alkali liquor at least four times, all wash water obtained through filtration and the vanadium-containing filtrate are mixed, the pH value is regulated to 1.5 to 9, stirring is conducted for 1 h to 48 h at the temperature ranging from 20 DEG C to 95 DEG C, vanadium pentoxide and ammonium polyvanadate or ammonium metavanadate precipitate are obtained, and vanadium pentoxide and ammonium polyvanadate or ammonium metavanadate products are obtained through filtering and drying.
Description
Technical field
Embodiments of the present invention relate to chemical field, more specifically, embodiments of the present invention relate to one
The method that high phosphorus, high ferro, Gao Meng, high acid concentration reclaim vanadium containing vanadium solution.
Background technology
Vanadium is important strategic element, all has been widely used at metallurgical and chemical field.Leaching of Vanadium from Vanadium slag is main
It is as additive with sodium salt (sodium carbonate, sodium chloride, sodium sulfate etc.), obtains containing vanadium molten by roasting-water logging
Liquid, solution through dephosphorization, except silica purge after carry out ammonium salt precipitation again and obtain ammonium poly-vanadate, make the most further
Various vanadium products.Traditional sodium roasting vanadium-extracting is faced with leachate phosphorus, impurity levels is high, waste water circulation is sharp
The problems such as, tailings sodium content height comprehensive utilization difficulty high with cost.
At present, vanadium slag calcification baking vanadium extraction and extracting vanadium from stone coal are all to use acid leaching process, and it has roasting process
Do not produce harmful gas, waste water can the advantages such as low cost recycles, tailings can comprehensively utilize.But, calcium
Salt roasting clinker and bone coal often make substantial amounts of entrance of the impurity elements such as phosphorus, ferrum, manganese leach during acidleach
Liquid, it is necessary to qualified vanadium product can be obtained after being purified by impurity.Purging by crystallization, extracting and purifying are formed
Purify, with ion exchange, the purification technique waited containing vanadic acid immersion, but said method often exists vanadium and loses big, raw
Produce the shortcomings such as cost is high, flow process is complicated.The precipitation method of purification is the method studying more, and it has and operated
The advantages such as journey is simple, dust removal rate is high, reagent consuming cost is low, but high acid concentration is contained in vanadium solution by it
Impurity clean-up effect extreme difference.Therefore, new technique need to be developed for high acid concentration containing purifying of vanadic acid immersion
Flow process.
Summary of the invention
The problem existed for prior art, the present invention provides a kind of clean containing impurity vanadium solution from high acid concentration
The method changed, reclaim vanadium, it is therefore intended that solve high acid concentration and purify containing impurity such as phosphorus, ferrum, manganese in vanadium solution
Difficulty, the vanadium big problem of loss, have easy and simple to handle, production cost is low, vanadium recovery advantages of higher.
For solving above-mentioned technical problem, one embodiment of the present invention by the following technical solutions:
A kind of high acid concentration purifies containing vanadium solution impurity, the method for recovery vanadium, and it comprises the following steps:
(1) by with the acid concentration of sulphur acid meter be 0.1%～20% join a certain amount of alkali liquor containing vanadium solution
In, the pH value of maintenance system is 2～8, under conditions of temperature is 20～100 DEG C stirring reaction 0.5～
6h, reaction is filtered after terminating, is obtained filtering residue and the filtrate Han vanadium；
(2) by described filtering residue acid solution or alkali liquid washing at least four times, every time the solid-to-liquid ratio of washing be 0.5～
The all washings being filtrated to get are merged by 3:1 with the described filtrate containing vanadium；
(3) pH value containing vanadium filtrate after merging with washings regulates to 1.5～9, when in step (1)
When alkali liquor used is non-ammonium salt solution, after pH value regulates, add ammonium salt, then temperature be 20～
1～48h is stirred, it is thus achieved that vanadic anhydride, ammonium poly-vanadate or ammonium metavanadate precipitate, mistake under conditions of 95 DEG C
Filter, be dried to obtain vanadic anhydride, ammonium poly-vanadate or ammonium metavanadate product.The addition of ammonium salt in this step
For: ammonium salt be 0.5～5:1 with the vanadic anhydride metering mass ratio containing the content of vanadium in vanadium solution.
Above-mentioned high acid concentration purifies containing vanadium solution impurity, reclaims in the method for vanadium, and step (1) described alkali liquor is
Sodium hydroxide solution, sodium carbonate liquor, sodium bicarbonate solution, ammonia, sal volatile, ammonium hydrogen carbonate are molten
Any one of liquid.Preferably sodium carbonate liquor, ammonia, sal volatile, ammonium bicarbonate soln.Alkali liquor
Consumption remains 2～7 for containing pH value of reaction system after vanadium solution adds.
Above-mentioned high acid concentration purifies containing vanadium solution impurity, reclaims in the method for vanadium, and step (2) described acid solution is
The sulfuric acid solution of pH=0.2～5, described alkali liquor is the sodium carbonate of pH=8～12, sodium hydroxide, ammonia, carbon
Acid ammonium or the saturated solution of ammonium hydrogen carbonate.
Above-mentioned high acid concentration purifies containing vanadium solution impurity, reclaims in the method for vanadium, the pH that step (3) uses
Value regulation reagent be acid solution or alkali liquor, acid solution be aqueous sulfuric acid, aqueous hydrochloric acid solution, aqueous solution of nitric acid or
Any one in carbonate aqueous solution, preferably sulfuric acid aqueous solution；Alkali liquor is that sodium hydroxide solution, sodium carbonate are molten
Liquid, sodium bicarbonate solution, ammonia, sal volatile, ammonium bicarbonate soln any one, preferably carbonic acid
Sodium solution, ammonia, sal volatile, ammonium bicarbonate soln.
Above-mentioned high acid concentration purifies containing vanadium solution impurity, reclaims in the method for vanadium, and step (1) is described molten containing vanadium
Liquid be vanadium concentration be 1～50g/L, phosphorus concentration be 0.05～2.5g/L, concentration of iron be 0.5～3.5g/L, manganese dense
Degree is 1～25g/L, and acid concentration is the solution of 0.1%～20%.
Above-mentioned high acid concentration purifies containing vanadium solution impurity, reclaims in the method for vanadium, described ammonium poly-vanadate and inclined vanadium
Acid ammonium carries out calcining and prepares vanadic anhydride.
Compared with prior art, one of beneficial effects of the present invention is: the present invention uses containing high acid concentration
Vanadium solution adds in aqueous slkali, coordinates the mode of residue washing, can realize the deep purifying of impurity, and will
The eluting of the vanadium overwhelming majority carried secretly in ferrum, manganese, phosphorus precipitate, it is ensured that obtain high vanadium yield, vanadium yield
Reaching more than 98%, the purity of vanadium product also reaches more than 98%.During precipitation can by hydrolysis precipitation or
Ammonium salt precipitation obtains hydration vanadic anhydride or ammonium poly-vanadate, ammonium metavanadate product, also can be further by forging
Firing standby vanadic anhydride product, the recovery of vanadium product is easy, efficient, various.Therefore, this method has stream
Journey is short, low cost, the response rate high, be applicable to the advantages such as large-scale industrial production.
Detailed description of the invention
In order to make the purpose of the present invention, technical scheme and advantage clearer, below in conjunction with embodiment,
The present invention is further elaborated.Should be appreciated that specific embodiment described herein only in order to
Explain the present invention, be not intended to limit the present invention.
Embodiment 1
Take 1L containing 25g/L V, phosphorus concentration be 2.5g/L, concentration of iron be 3.5g/L, manganese concentration be 23.6g/L, acid
Concentration be 9.6% (with sulphur acid meter) containing vanadium solution, join in appropriate sodium carbonate liquor and make reaction system
PH value maintain to 8.0, at 85 DEG C stirring reaction 2h.Filter, obtain filtering residue and the filtrate Han vanadium.Filtering residue is through 50mL
Saturated sodium carbonate solution washs four times, is merged with the filtrate containing vanadium by washings, and its pH value is 8.7.
To obtain containing in vanadium solution add 75g ammonium chloride, at 25 DEG C stir 48h, obtain white inclined vanadium
Acid ammonium precipitation.Filter, be dried, obtain the ammonium metavanadate product that purity is 99.1%.Technical process vanadium is total entirely
The response rate is 98.6%.
Embodiment 2
Take 1L containing 50g/L V, phosphorus concentration be 0.05g/L, concentration of iron be 0.75g/L, manganese concentration be 1.5g/L, acid
Concentration be 0.1% (with sulphur acid meter) containing vanadium solution, join in appropriate ammonium bicarbonate soln and make reactant
The pH value of system maintains to 3, stirring reaction 4h at 60 DEG C.Filter, obtain filtering residue and the filtrate Han vanadium.Filtering residue is through 60mL
Unsaturated carbonate hydrogen ammonium salt solution washs four times, is merged with the filtrate containing vanadium by washings.
Regulate pH to 2.2 to obtain containing addition concentrated sulphuric acid in vanadium solution, at 95 DEG C, stir 2h, obtain orange
The ammonium poly-vanadate precipitation of color.Filter, be dried, after 520 DEG C of calcining 1h, obtain five oxidations two that purity is 99.4%
Vanadium product.The overall recovery of full technical process vanadium is 99.5%.
Embodiment 3
Take 1L containing 6g/L V, phosphorus concentration be 0.95g/L, concentration of iron be 1.5g/L, manganese concentration be 10.3g/L, acid
Concentration be 3% (with sulphur acid meter) containing vanadium solution, join in appropriate sodium carbonate liquor and make reaction system
PH value maintains to 6.5, stirring reaction 6h at 25 DEG C.Filter, obtain filtering residue and the filtrate Han vanadium.Filtering residue is through 40mL
Saturated sodium carbonate solution washs four times, is merged with the filtrate containing vanadium by washings.
To obtain containing in vanadium solution add 8g ammonium sulfate, regulation pH value be 2.1, at 85 DEG C stir 2.5h,
Obtain saffron ammonium poly-vanadate precipitation.Filtering, be dried, obtaining purity after 510 DEG C of calcining 1h is 99.6%
Vanadic anhydride product.The overall recovery of full technical process vanadium is 99.1%.
Embodiment 4
Take 1L containing 20g/L V, phosphorus concentration be 0.15g/L, concentration of iron be 0.56g/L, manganese concentration be 5.6g/L, acid
Concentration be 5% (with sulphur acid meter) containing vanadium solution, join and appropriate ammonia make the pH value of reaction system tie up
Hold to 5, stirring reaction 2h at 80 DEG C.Filter, obtain filtering residue and the filtrate Han vanadium.Filtering residue is through 80mL ammonia scrubbing
Four times, washings are merged with the filtrate containing vanadium.
Regulate pH to 1.6 to obtain containing addition concentrated sulphuric acid in vanadium solution, at 95 DEG C, stir 2h, obtain redness
Hydration vanadic anhydride precipitation.Filter, be dried, obtain the vanadic anhydride product that purity is 98.8%.Entirely
The overall recovery of technical process vanadium is 98.1%.
Embodiment 5
Take 1L containing 35g/L V, phosphorus concentration be 2.15g/L, concentration of iron be 3.23g/L, manganese concentration be 22.5g/L,
Acid concentration be 7% (with sulphur acid meter) containing vanadium solution, join in appropriate sodium hydroxide solution and make reactant
The pH value of system maintains to 4, stirring reaction 2h at 100 DEG C.Filter, obtain filtering residue and the filtrate Han vanadium.Filtering residue warp
The saturated sodium hydroxide solution of 20mL washs four times, is merged with the filtrate containing vanadium by washings.
To obtain containing in vanadium solution add 50g ammonium sulfate, regulation pH value be 2.3, at 95 DEG C stir 1h,
Obtain saffron ammonium poly-vanadate precipitation.Filtering, be dried, obtaining purity after 510 DEG C of calcining 1h is 99.3%
Vanadic anhydride product.The overall recovery of full technical process vanadium is 99.5%.
Embodiment 6
Take 1L containing 15g/L V, phosphorus concentration be 1.15g/L, concentration of iron be 2.75g/L, manganese concentration be 10.2g/L,
Acid concentration be 1% (with sulphur acid meter) containing vanadium solution, join in appropriate sal volatile and make reaction system
PH value maintain to 7, at 50 DEG C stirring reaction 3h.Filter, obtain filtering residue and the filtrate Han vanadium.Filtering residue is through 50mL
Unsaturated carbonate ammonium salt solution washs four times, is merged with the filtrate containing vanadium by wash water, and its pH value is 8.8.
Gained is stirred 48h containing vanadium solution at 25 DEG C, obtains the ammonium metavanadate precipitate of white.Filter, be dried,
Obtain the ammonium metavanadate product that purity is 99.2%.The overall recovery of full technical process vanadium is 98.0%.
Comparative example 1
Taking same as in Example 2 containing vanadium solution, unlike embodiment 2 feed postition, the present embodiment will
The pH value that appropriate sodium hydroxide solution adds containing making reaction system in vanadium solution maintains to 5, and at 60 DEG C, stirring is anti-
Answer 4h.Filter, obtain filtering residue and the filtrate Han vanadium.Filtering residue washs four times through the saturated sodium hydroxide solution of 30mL,
Washings are merged with the filtrate containing vanadium.
Regulate pH to 2.3 to obtain containing addition concentrated sulphuric acid in vanadium solution, at 95 DEG C, stir 2h, obtain orange
The ammonium poly-vanadate precipitation of color.Filter, be dried, after 520 DEG C of calcining 1h, obtain five oxidations two that purity is 99.1%
Vanadium product.The overall recovery of full technical process vanadium is 52.8%.
Comparative example 2
Taking same as in Example 2 containing vanadium solution, unlike embodiment 2 feed postition, the present embodiment will
The pH value that appropriate ammonium bicarbonate soln adds containing making reaction system in vanadium solution maintains to 3, and at 60 DEG C, stirring is anti-
Answer 4h.Filter, obtain filtering residue and the filtrate Han vanadium.Filtering residue washs four times through 50mL unsaturated carbonate hydrogen ammonium salt solution,
Washings are merged with the filtrate containing vanadium.
Regulate pH to 2.2 to obtain containing addition concentrated sulphuric acid in vanadium solution, at 95 DEG C, stir 2h, obtain orange
The ammonium poly-vanadate precipitation of color.Filter, be dried, after 520 DEG C of calcining 1h, obtain five oxidations two that purity is 96.8%
Vanadium product.The overall recovery of full technical process vanadium is 68.5%.
Although reference be made herein to invention has been described for the explanatory embodiment of the present invention, however, it should reason
Solving, those skilled in the art can be designed that a lot of other amendments and embodiment, these amendments and enforcement
Mode will fall within spirit disclosed in the present application and spirit.More specifically, disclosed in the present application
In the range of, the building block of theme composite configuration and/or layout can be carried out multiple modification and improvement.Except
The modification that building block and/or layout are carried out and improve outside, to those skilled in the art, other
Purposes also will be apparent from.
Claims (6)
1. the method that a high acid concentration purifies containing vanadium solution impurity, reclaims vanadium, it is characterised in that it includes following
Step:
(1) by with the acid concentration of sulphur acid meter be 0.1%～20% join a certain amount of alkali liquor containing vanadium solution
In, the pH value of maintenance system is 2～8, under conditions of temperature is 20～100 DEG C stirring reaction 0.5～
6h, reaction is filtered after terminating, is obtained filtering residue and the filtrate Han vanadium；
(2) by described filtering residue acid solution or alkali liquid washing at least four times, every time the solid-to-liquid ratio of washing be 0.5～
The all washings obtained are merged by 3:1 with the described filtrate containing vanadium；
(3) pH value containing vanadium filtrate after merging with washings regulates to 1.5～9, when in step (1)
When alkali liquor used is non-ammonium salt solution, after pH value regulates, add ammonium salt, then temperature be 20～
1～48h is stirred, it is thus achieved that vanadic anhydride, ammonium poly-vanadate or ammonium metavanadate precipitate under conditions of 95 DEG C,
Filter, be dried to obtain vanadic anhydride, ammonium poly-vanadate or ammonium metavanadate product.
The method that high acid concentration the most according to claim 1 purifies containing vanadium solution impurity, reclaims vanadium, it is special
Levy be step (1) described alkali liquor be sodium hydroxide solution, sodium carbonate liquor, sodium bicarbonate solution,
Ammonia, sal volatile, ammonium bicarbonate soln any one.
The method that high acid concentration the most according to claim 1 purifies containing vanadium solution impurity, reclaims vanadium, it is special
Levy the sulfuric acid solution being that step (2) described acid solution is pH=0.2～5, described alkali liquor be pH=8～
The saturated solution of sodium carbonate, sodium hydroxide, ammonia, ammonium carbonate or the ammonium hydrogen carbonate of 12.
The method that high acid concentration the most according to claim 1 purifies containing vanadium solution impurity, reclaims vanadium, it is special
Levy and be that the pH value regulation reagent that step (3) uses is acid solution or alkali liquor, acid solution be aqueous sulfuric acid,
Any one in aqueous hydrochloric acid solution, aqueous solution of nitric acid or carbonate aqueous solution, alkali liquor is sodium hydroxide
Solution, sodium carbonate liquor, sodium bicarbonate solution, ammonia, sal volatile, ammonium bicarbonate soln
Any one.
The method that high acid concentration the most according to claim 1 purifies containing vanadium solution impurity, reclaims vanadium, it is special
Levy be step (1) described containing vanadium solution be vanadium concentration be 1～50g/L, phosphorus concentration be 0.05～
2.5g/L, concentration of iron are 0.5～3.5g/L, manganese concentration is 1～25g/L, and acid concentration is 0.1%～20%
Solution.
The method that high acid concentration the most according to claim 1 purifies containing vanadium solution impurity, reclaims vanadium, it is special
Levy and be that described ammonium poly-vanadate and ammonium metavanadate carry out calcining and can prepare vanadic anhydride.
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Cited By (1)
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|---|---|---|---|---|
| CN112391537A (en) * | 2020-10-29 | 2021-02-23 | 攀枝花市山青钒业有限公司 | Method for extracting vanadium by using hydrochloric acid, sulfuric acid and vanadium-containing high-calcium high-phosphorus slag |
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| CN112391537A (en) * | 2020-10-29 | 2021-02-23 | 攀枝花市山青钒业有限公司 | Method for extracting vanadium by using hydrochloric acid, sulfuric acid and vanadium-containing high-calcium high-phosphorus slag |
| CN112391537B (en) * | 2020-10-29 | 2021-07-06 | 攀枝花市山青钒业有限公司 | Method for extracting vanadium by using hydrochloric acid, sulfuric acid and vanadium-containing high-calcium high-phosphorus slag |
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Address after: 610306 Chengdu City, Chengdu, Sichuan, China (Sichuan) free trade test zone, Chengdu City, Qingbaijiang District, xiangdao Boulevard, Chengxiang Town, No. 1509 (room 13, A District, railway port mansion), room 1319 Patentee after: Chengdu advanced metal material industry technology Research Institute Co.,Ltd. Address before: 610306 Chengdu City, Chengdu, Sichuan, China (Sichuan) free trade test zone, Chengdu City, Qingbaijiang District, xiangdao Boulevard, Chengxiang Town, No. 1509 (room 13, A District, railway port mansion), room 1319 Patentee before: CHENGDU ADVANCED METAL MATERIAL INDUSTRIAL TECHNOLOGY RESEARCH INSTITUTE Co.,Ltd. |