CN105087933A - Method for separating vanadium and chromium from vanadium and chromium mixed solution - Google Patents
Method for separating vanadium and chromium from vanadium and chromium mixed solution Download PDFInfo
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- CN105087933A CN105087933A CN201510614831.2A CN201510614831A CN105087933A CN 105087933 A CN105087933 A CN 105087933A CN 201510614831 A CN201510614831 A CN 201510614831A CN 105087933 A CN105087933 A CN 105087933A
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- vanadium
- chromium
- resin
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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 discloses a method for separating vanadium and chromium from a vanadium and chromium mixed solution. The method includes the steps that A, the pH value of the mixed solution is adjusted to 3.0-4.0, vanadium and chromium in the mixed solution are adsorbed through an ion exchange resin adsorption method, and resin containing vanadium and chromium is obtained; B, a 3-4% sulfuric acid-ethanol elution solution is used for eluting the resin containing vanadium and chromium, and resin containing vanadium and a solution containing chromium are obtained; C, the resin containing vanadium is desorbed so that a desorbing solution containing vanadium can be obtained, and vanadium precipitation processing is performed on the desorbing solution containing vanadium so that vanadate can be obtained; D, the vanadate is calcinated so that vanadium pentoxide can be obtained; E, the pH of the solution containing chromium is adjusted for neutralization, chromium is precipitated in the manner of hydrate precipitate Cr(OH)3.nH2O, and chromium trioxide is prepared through calcination processing. The method is simple in technological process, easy to operate, low in cost and beneficial to separation and recycling of vanadium and chromium resources.
Description
Technical field
The present invention relates to the technical field recycling vanadium, chromium, more particularly, relate to a kind of spent ion exchange resin method and be separated and reclaim the method containing vanadium, chromium in vanadium, chromium mixed solution.
Background technology
Vanadium is a kind of important strategic materials, is widely used in the industries such as iron and steel, alloy, chemical industry, pottery, medicine.The vanadium iron magnetite association of China's Panxi Diqu has metallic element chromium, and ore is bessemerized the vanadium slag obtained and is enriched elemental vanadium and chromium.Because vanadium is similar to the character of chromium, therefore, in the process of Leaching of Vanadium from Vanadium slag, vanadium and chromium are oxidized to high price leaching in aqueous phase simultaneously, leach liquor is after ammonium salt precipitation, containing metal V (V) and Cr (VI) in vanadium wastewater liquid, in solution, V (V) and Cr (VI) is valuable metal and toxic substance, need process further.
In current solution, vanadium chromium separation method mainly contains: direct precipitation method, extraction process, ion exchange method.Direct precipitation method is the most most economical method, but the metavanadate that precipitation obtains or vanadate all can contain impurity element.Ning Pengge etc. adopt primary amine N-1923 extraction agent separation and extraction vanadium, chromium, and technical process is fairly simple, can obtain the product of the higher vanadium of purity and chromium, and shortcoming is that the capacity of extraction agent is low, easily produces emulsion in extraction process.Fan Yeye have studied and is separated and extracts vanadium and chromium with D314 anionite-exchange resin by twin columns absorption method, and the method is simple to operate and cost is lower, but absorption adds technique required time again.
Summary of the invention
For prior art above shortcomings, the object of the present invention is to provide and a kind ofly effectively can be separated and reclaim the method containing vanadium, vanadium in chromium mixed solution, chromium element, present method is simple, easy to operate.
Technical scheme of the present invention is achieved in that
From vanadium, chromium mixed solution, be separated a method for vanadium, chromium, comprise the steps:
The pH value of A, adjustment mixed solution is 3.0-4.0, and the vanadium in spent ion exchange resin absorption method absorption mixed solution and chromium, obtain containing vanadium, chromium resin;
B, use 3%-4% sulfuric acid-ethanolic soln wash-out, containing vanadium, chromium resin, obtain containing vanadium resin and chromium-containing solution;
C, desorb obtain containing vanadium stripping liquid containing vanadium resin, carry out precipitation process to obtain vanadate to containing vanadium stripping liquid;
D, calcination processing is carried out to vanadate, obtain Vanadium Pentoxide in FLAKES;
E, chromium-containing solution regulate pH to neutralize, and chromium is with hydrate deposition Cr (OH)
3nH
2the form of O is separated out, and produces chromium sesquioxide through calcination process.
Wherein, steps A ion-exchange absorption adopts dynamic adsorption test method, and the ion exchange resin used is Dex-V weak base anion-exchange resin.
Wherein, step C containing vanadium resin, obtains containing vanadium stripping liquid with 3%-4%NaOH solution stripping, obtains ammonium metavanadate precipitate to containing adding ammonium chloride in vanadium stripping liquid; The calcining temperature of step D is 550-600 DEG C.
Wherein, the calcining temperature of step e is 1000-1150 DEG C, calcination time 2.5-3.0h.
The invention provides and a kind ofly effectively can be separated and reclaim containing vanadium, the method for vanadium, chromium in chromium mixed solution.The method, by using vanadium, the chromium in anion-exchange resin method absorption vanadium, chromium mixed solution, then adopts stepwise elution thus separately reclaims chromium, vanadium.Compared with prior art, technical process is simple, easy handling, cost are low, is conducive to the Separation and Recovery of vanadium chromium resource for method of the present invention.
Embodiment
The present invention, from containing the method being separated vanadium, chromium vanadium, chromium mixed solution, comprises the steps:
The pH value of A, adjustment mixing solutions is 3.0-4.0, with the vanadium in Dex-V macroreticular weakly base Anion-adsorption solution and chromium, obtains containing vanadium, chromium resin; Ion-exchange absorption adopts dynamic adsorption test method; The form that vanadium chromium exists under different pH value is in the solution different, and resin is different to multi-form ion adsorption capacity.Through static test research, Dex-V resin is respectively 98.35%, 99.26% to the adsorption efficiency of V (V), Cr (VI) ion in pH value range 3.0-4.0.Therefore in order to ensure that resin absorption ability reaches the highest, therefore to choose pH value be 3.0-4.0.
B, use 3%-4% sulfuric acid-ethanolic soln wash-out, containing vanadium, chromium resin, obtain containing vanadium resin and chromium-containing solution; Preferably 4% sulfuric acid-ethanolic soln, 4% represents the volume fraction of sulfuric acid at this solution, and the reaction mechanism equation of this eluant solution is as follows:
C, obtaining containing vanadium stripping liquid with 3%-4%NaOH solution stripping containing vanadium resin, obtaining ammonium metavanadate precipitate to containing adding ammonium chloride in vanadium stripping liquid;
D, carry out calcination processing to ammonium meta-vanadate, obtain Vanadium Pentoxide in FLAKES, calcining temperature is 550-600 DEG C;
E, chromium-containing solution regulate pH to neutralize, and chromium is with hydrate deposition Cr (OH)
3nH
2the form of O is separated out, and produces chromium sesquioxide through calcination process.Calcining temperature is 1000-1150 DEG C, calcination time 2.5-3h.
The present invention is used for the bronsted lowry acids and bases bronsted lowry of adjust ph and is respectively H
2sO
4and NaOH.
Below in conjunction with embodiment, be described in further detail the present invention, following examples are intended to the present invention instead of limitation of the invention are described.
Embodiment 1
2000mL is contained mixing solutions sodium hydroxide solution or the sulphur acid for adjusting pH to 3.0 of pentavalent vanadium (100mg/L) and sexavalent chrome (100mg/L).Carry out dress post dynamic experiment with Dex-V macroporous weakly basic anion exchange resin, post layer height is filled to 10cm.2000mLV (V), Cr (VI) mixing solutions are flowed through ion exchange column with the flow velocity of 10mL/min and adsorb, obtains containing vanadium, chromium resin.After adsorption equilibrium, reach balance with 4% sulfuric acid-ethanolic soln wash-out containing vanadium, chromium resin, obtain containing vanadium resin and containing chromium stripping liquid.Now, vanadium is adsorbed on resin with anion radical form, and chromium is with Cr
3+form is present in stripping liquid.
Regulate above-mentioned containing chromium stripping liquid pH to 8.2, chromium is with hydrate deposition Cr (OH)
3nH
2the form of O is separated out, and at 1000 DEG C, calcination 3h obtains Cr
2o
3powder.Obtain vanadium stripping liquid containing vanadium resin 3%NaOH solution stripping, in stripping liquid, add ammonium chloride obtain ammonium metavanadate precipitate, obtain V 550 DEG C of these precipitations of calcination
2o
5powder.By analysis, the total yield of vanadium and chromium is respectively 82.63% and 95.42%.
Embodiment 2
2000mL is contained mixing solutions sodium hydroxide solution or the sulphur acid for adjusting pH to 3.0 of pentavalent vanadium (100mg/L) and sexavalent chrome (100mg/L).Carry out dress post dynamic experiment with Dex-V macroporous weakly basic anion exchange resin, post layer height is filled to 20cm.2000mLV (V), Cr (VI) mixing solutions are flowed through ion exchange column with the flow velocity of 10mL/min and adsorb, obtains containing vanadium, chromium resin.After adsorption equilibrium, reach balance with 4% sulfuric acid-ethanolic soln wash-out containing vanadium, chromium resin, obtain containing vanadium resin and containing chromium stripping liquid.Now, vanadium is adsorbed on resin with anion radical form, and chromium is with Cr
3+form is present in stripping liquid.
Regulate above-mentioned containing chromium stripping liquid pH to 8.2, chromium is with hydrate deposition Cr (OH)
3nH
2the form of O is separated out, and at 1000 DEG C, calcination 3h obtains Cr
2o
3powder.Obtain vanadium stripping liquid containing vanadium resin 3%NaOH solution stripping, in stripping liquid, add ammonium chloride obtain ammonium metavanadate precipitate, obtain V 550 DEG C of these precipitations of calcination
2o
5powder.By analysis, the total yield of vanadium and chromium is respectively 88.47% and 96.26%.
Embodiment 3
2000mL is contained mixing solutions sodium hydroxide solution or the sulphur acid for adjusting pH to 3.0 of pentavalent vanadium (100mg/L) and sexavalent chrome (100mg/L).Carry out dress post dynamic experiment with Dex-V macroporous weakly basic anion exchange resin, post layer height is filled to 30cm.2000mLV (V), Cr (VI) mixing solutions are flowed through ion exchange column with the flow velocity of 10mL/min and adsorb, obtains containing vanadium, chromium resin.After adsorption equilibrium, reach balance with 4% sulfuric acid-ethanolic soln wash-out containing vanadium, chromium resin, obtain containing vanadium resin and containing chromium stripping liquid.Now, vanadium is adsorbed on resin with anion radical form, and chromium is with Cr
3+form is present in stripping liquid.
Regulate above-mentioned containing chromium stripping liquid pH to 8.2, chromium is with hydrate deposition Cr (OH)
3nH
2the form of O is separated out, and at 1000 DEG C, calcination 3h obtains Cr
2o
3powder.Obtain vanadium stripping liquid containing vanadium resin 3%NaOH solution stripping, in stripping liquid, add ammonium chloride obtain ammonium metavanadate precipitate, obtain V 550 DEG C of these precipitations of calcination
2o
5powder.By analysis, the total yield of vanadium and chromium is respectively 90.37% and 96.52%.
Finally it should be noted that, above embodiment is only in order to illustrate technical scheme of the present invention and unrestricted, although applicant's reference preferred embodiment is to invention has been detailed description, those of ordinary skill in the art is to be understood that, technical scheme of the present invention is modified or equivalent replacement, and do not depart from aim and the scope of the technical program, all should be encompassed in the middle of right of the present invention.
Claims (4)
1. from vanadium, chromium mixed solution, be separated a method for vanadium, chromium, it is characterized in that: comprise the steps:
The pH value of A, adjustment mixed solution is 3.0-4.0, and the vanadium in spent ion exchange resin absorption method absorption mixed solution and chromium, obtain containing vanadium, chromium resin;
B, use 3%-4% sulfuric acid-ethanolic soln wash-out, containing vanadium, chromium resin, obtain containing vanadium resin and chromium-containing solution;
C, desorb obtain containing vanadium stripping liquid containing vanadium resin, carry out precipitation process to obtain vanadate to containing vanadium stripping liquid;
D, calcination processing is carried out to vanadate, obtain Vanadium Pentoxide in FLAKES;
E, chromium-containing solution regulate pH to neutralize, and chromium is with hydrate deposition Cr (OH)
3nH
2the form of O is separated out, and produces chromium sesquioxide through calcination process.
2. the method being separated vanadium, chromium from vanadium, chromium mixed solution according to claim 1, is characterized in that, steps A ion-exchange absorption adopts dynamic adsorption test method, and the ion exchange resin used is Dex-V weak base anion-exchange resin.
3. the method being separated vanadium, chromium from vanadium, chromium mixed solution according to claim 1, is characterized in that, step C containing vanadium resin, obtains containing vanadium stripping liquid with 3%-4%NaOH solution stripping, obtains ammonium metavanadate precipitate to containing adding ammonium chloride in vanadium stripping liquid; The calcining temperature of step D is 550-600 DEG C.
4. the method being separated vanadium, chromium from vanadium, chromium mixed solution according to claim 1, is characterized in that, the calcining temperature of step e is 1000-1150 DEG C, calcination time 2.5-3.0h.
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| CN105087933B CN105087933B (en) | 2017-08-25 |
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Cited By (5)
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| CN105714131A (en) * | 2016-03-26 | 2016-06-29 | 云南广隆有色环保科技发展有限公司 | Method for separating and extracting vanadium and chromium from same solution |
| CN105753219A (en) * | 2016-04-18 | 2016-07-13 | 湖南永清环保研究院有限责任公司 | Process for purifying and treating vanadium-containing wastewater in advanced manner and process for recycling vanadium and chromium |
| CN107190155A (en) * | 2017-05-19 | 2017-09-22 | 重庆大学 | Vanadium, the method for chromium are extracted in a kind of mixed liquor from containing vanadium and chromium |
| CN109022828A (en) * | 2018-07-03 | 2018-12-18 | 开封大学 | The extracting method of vanadium in spent vanadium catalyst |
| CN116334414A (en) * | 2023-03-16 | 2023-06-27 | 核工业北京化工冶金研究院 | Method for selectively separating vanadium and chromium from vanadium-chromium solution |
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| CN102676810A (en) * | 2012-05-22 | 2012-09-19 | 中南大学 | Method for separating and recycling vanadium and chromium from vanadate-chromate-containing solution |
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| US20040244537A1 (en) * | 2003-06-05 | 2004-12-09 | Runyon Dale Leroy | Processing coal combustion products (CCP), ore, or other material using functionally electrolyzed water (FEW) |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105714131A (en) * | 2016-03-26 | 2016-06-29 | 云南广隆有色环保科技发展有限公司 | Method for separating and extracting vanadium and chromium from same solution |
| CN105753219A (en) * | 2016-04-18 | 2016-07-13 | 湖南永清环保研究院有限责任公司 | Process for purifying and treating vanadium-containing wastewater in advanced manner and process for recycling vanadium and chromium |
| CN107190155A (en) * | 2017-05-19 | 2017-09-22 | 重庆大学 | Vanadium, the method for chromium are extracted in a kind of mixed liquor from containing vanadium and chromium |
| CN109022828A (en) * | 2018-07-03 | 2018-12-18 | 开封大学 | The extracting method of vanadium in spent vanadium catalyst |
| CN109022828B (en) * | 2018-07-03 | 2020-09-11 | 开封大学 | Method for extracting vanadium from waste vanadium catalyst |
| CN116334414A (en) * | 2023-03-16 | 2023-06-27 | 核工业北京化工冶金研究院 | Method for selectively separating vanadium and chromium from vanadium-chromium solution |
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|---|---|
| CN105087933B (en) | 2017-08-25 |
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