CN105567964B - Method for selectively reducing, separating and recycling vanadium and chrome from solution containing vanadium and chrome - Google Patents
Method for selectively reducing, separating and recycling vanadium and chrome from solution containing vanadium and chrome Download PDFInfo
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- CN105567964B CN105567964B CN201510995884.3A CN201510995884A CN105567964B CN 105567964 B CN105567964 B CN 105567964B CN 201510995884 A CN201510995884 A CN 201510995884A CN 105567964 B CN105567964 B CN 105567964B
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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
- C22B3/46—Treatment or purification of solutions, e.g. obtained by leaching by chemical processes by substitution, e.g. by cementation
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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
-
- 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
- C22B34/30—Obtaining chromium, molybdenum or tungsten
- C22B34/32—Obtaining chromium
-
- 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 selectively reducing, separating and recycling vanadium and chrome from a solution containing vanadium and chrome. The method is characterized by comprising the steps that a compound of V(IV) or/and V(III) and a solution of the compound serve as a reducing agent, Cr(VI) in the solution is selectively reduced into Cr(III), and then polyvanadic acid or ammonium polyorthovanadate are precipitated out from the solution; after the obtained polyvanadic acid or the ammonium polyorthovanadate is calcined, a vanadium pentoxide product is obtained; and a vanadium precipitation solution hydrates chromic oxide through hydrolytic precipitation after being subjected to purification and impurity removal, or NH4Cr(SO4)2 is precipitated out of the vanadium precipitation solution under the action of ammonium salt, hydrated chromic oxide is obtained after the NH4Cr(SO4)2 is transformed, and after the hydrated chromic oxide is calcined, a chromic oxide product is obtained. The method has the advantages that the vanadium-chrome separation effect is good, the technological process is short, the treatment cost is low, operation is easy, environmental friendliness is achieved, and the method is suitable for industrialized application.
Description
Technical field
The present invention relates to a kind of method that containing vanadium and chromium solution-selective Reduced separating reclaims vanadium and chromium.
Background technology
Vanadium is similar with chromium property, nature they generally in the way of symbiosis preservation in mineral.China's Flos Bombacis Malabarici, west
The vanadium titano-magnetite of the ground such as prosperous, Chengde paneling is exactly the Typical Representative of this kind of mineral.What v-bearing titanomagnetite smelting process was produced
Vanadium slag is the primary raw material of vanadic anhydride production.Vanadium slag Jing sodium roastings~water logging, vanadium chromium is respectively with vanadate and chromate
Form enter solution.Additionally, the containing vanadium and chromium material that chemical industry metallurgical technical process is produced, such as containing vanadium and chromium waste liquid precipitate reduction slag
Sodium roasting-water logging is also obtained the solution of containing vanadium and chromium hydrochlorate.
The solution chemistry of vanadium chromium is similar, and the vanadium and chromium separated and recovered in solution is a global difficult problem.It is right both at home and abroad
It has carried out substantial amounts of research, the method that vanadium and chromium are separated and recovered in various solution from containing vanadium and chromium is developed, including molten
Agent extraction, ion exchange and the electronation sedimentation method.Can be realized in solution using the compound amine extraction of primary amine, quaternary amine or brothers
The separation of vanadium and chromium, but extract and separate vanadium and chromium high cost, process conditions are difficult to control to.Exchanged using weak base and strong alkali anion
The difference of the anion exchange gesture that resin is formed in aqueous to Cr VI and pentavalent vanadium, by saturation absorption vanadium and chromium are realized
Separation, directly obtain the product of vanadium and chromium, but ion exchange is only suitable for the process of low concentration solution, the vanadate to Gao Ge
For solution, the capacity of ion exchange resin is too little, has a strong impact on production efficiency.The electronation sedimentation method include ferrous sulfate or
Iron reduction method, sulfur dioxide and Arbiso process, iron anode electrolysis etc., vanadium that these methods can be in purified solution and
Chromium, but obtain is all the industrial residue (green mud) containing vanadium and chromium, needs further to separate and recover vanadium and chromium from green mud.China
Patent CN103602819A is gone back respectively using first adding reducing agent by the pentavalent vanadium and Cr VI in solution under the conditions of suitable pH
It is former then to precipitate tetravalence vanadium and trivalent chromium into tetravalence vanadium and trivalent chromium, then alkali is respectively adopted leaches and separate with the mode of Ore Leaching
Reclaim vanadium and chromium；The method good separating effect, it is simple to operate, but long flow path is there is also, the problem of high cost.
The content of the invention
It is an object of the invention to overcome prior art deficiency and a kind of technological process is provided short, simple to operate, vanadium chromium
Good separating effect, processing cost is low, the method that eco-friendly containing vanadium and chromium solution-selective Reduced separating reclaims vanadium and chromium.
The method that a kind of containing vanadium and chromium solution-selective Reduced separating of the present invention reclaims vanadium and chromium, comprises the following steps：
The first step：Selective reduction chromium
Adjust containing vanadium and chromium solution ph to 0.1~3.5, then Cr is reduced into by Cr (VI) by the chromium in containing vanadium and chromium solution
(III) 1~1.5 times of addition reducing agent of theoretical amount, selective reduction chromium therein, liquid after must reducing；
Second step：Precipitate and separate vanadium
, to 1.5~3.5, Direct precipitation separates out many vanadic acid, or adjusts liquid pH after reduction to adjust liquid pH value after first step gained reduction
Ammonium salt, Precipitation ammonium poly-vanadate is added to filter liquid after much vanadic acid or ammonium poly-vanadate and precipitation while value to 1.5~3.5,
Many vanadic acid or ammonium poly-vanadate calcine to obtain vanadic anhydride；
3rd step：Precipitate and separate chromium
Adjust liquid pH value after the precipitation obtained by second step to adjust pH value to 4.5~9.5 again to 3.5~4.0 purification and impurity removals, precipitate
Hydrated chromium oxide, or ammonia or ammonium salt are added in liquid after precipitation, then at a temperature of -15~45 DEG C, crystallization separates out NH4Cr
(SO4)2Crystal, NH4Cr(SO4)2Crystal makes the transition to obtain hydrated chromium oxide, and hydrated chromium oxide calcines to obtain chromic oxide；Ammonia or ammonium salt
Addition press Cr3+/NH4 +Mol ratio 1:1~3 determines.
The method that a kind of containing vanadium and chromium solution-selective Reduced separating of the present invention reclaims vanadium and chromium, in the first step, the reduction
Compound or solution of the agent selected from V (IV) or/and V (III).
The method that a kind of containing vanadium and chromium solution-selective Reduced separating of the present invention reclaims vanadium and chromium, the V (IV) or/and V
(III) compound is selected from VO2、V2O3、Na2VO3、Na2V2O5、NaVO2、(NH4)2O·2V2O4、VCl4、VCl3、VOCl2、
VOCl、VOSO4、V2(SO4)3In one or more；The solution of the V (IV) or/and V (III) is selected from V (IV) or/and V
(III) one kind in acid solution, alkaline solution, the aqueous solution of compound is obtained by reducing the solution containing pentavalent vanadium
.
The method that a kind of containing vanadium and chromium solution-selective Reduced separating of the present invention reclaims vanadium and chromium, in the first step, selectivity is also
Former process conditions are：Reaction temperature is 5~115 DEG C, and the response time is 0.5~6 hour.
The method that a kind of containing vanadium and chromium solution-selective Reduced separating of the present invention reclaims vanadium and chromium, in second step, Precipitation
The process conditions of many vanadic acid are：Reaction temperature 60-110 DEG C, 1~6 hour time；The process conditions of Precipitation ammonium poly-vanadate
For：Reaction temperature 50-110 DEG C, 1~6 hour time.
The method that a kind of containing vanadium and chromium solution-selective Reduced separating of the present invention reclaims vanadium and chromium, in second step, many vanadic acid or
Ammonium poly-vanadate calcines 0.5-5 hours at 450~600 DEG C, obtains vanadic anhydride.
The method that a kind of containing vanadium and chromium solution-selective Reduced separating of the present invention reclaims vanadium and chromium, in the 3rd step, NH4Cr
(SO4)2Crystal make the transition hydrated chromium oxide technical process is：NH4Cr(SO4)2Crystal first presses solid-to-liquid ratio 1:2-10 adds water stirring, plus
Enter ammonia or ammonia and adjust pH to 4.5-8.5,25~115 DEG C of stirring 0.5-3.5 hours, filter after hydrated chromium oxide and transition
Liquid, liquid returns NH after transition4Cr(SO4)2Crystallization Procedure is recycled, or evaporating, concentrating and crystallizing obtains ammonium sulfate product.
The method that a kind of containing vanadium and chromium solution-selective Reduced separating of the present invention reclaims vanadium and chromium, in the 3rd step, aqua oxidation
Chromium calcines 0.5-6 hours and obtains chromic oxide at 700-900 DEG C.
The method that a kind of containing vanadium and chromium solution-selective Reduced separating of the present invention reclaims vanadium and chromium, the first step, second step, the 3rd
In step, system pH is adjusted using acid or alkali, one or more of acid in hydrochloric acid, nitric acid, sulphuric acid, carbonic acid；Alkali
Selected from CaO, CaOH, CaCO3、NaOH、NaHCO3、Na2CO3、KOH、KHCO3、K2CO3、One or more in ammonia.
The method that a kind of containing vanadium and chromium solution-selective Reduced separating of the present invention reclaims vanadium and chromium, in second step, the 3rd step, plus
At least one of the ammonium salt for entering in ammonium sulfate, ammonium chloride, ammonium nitrate.
It is of the invention compared with existing technology with advantages below and effect：
The present invention is cleverly using E in acid condition0 Cr(III)/Cr(VI)With E0 V(IV)/V(V)The difference that current potential is present, with V
(IV) or/and V (III) compound and its solution as reducing agent, by Cr (VI) selective reductions in solution into Cr
(III), the then many vanadic acid of Precipitation or ammonium poly-vanadate, therefrom separate and recover vanadium, and institute is much after vanadic acid or ammonium poly-vanadate calcining
Obtain vanadic anhydride product；After precipitation after the purified remove impurity of liquid, then liquid is direct after hydrolytic precipitation hydrated chromium oxide or precipitation
The Precipitation NH in the presence of ammonium salt4Cr(SO4)2, separate and recover chromium therein, gained NH4Cr(SO4)2Water is obtained Jing after transition
Chromium oxide is closed, after hydrated chromium oxide calcining chromic oxide product is obtained.
The present invention has vanadium chromium good separating effect, and technological process is short, and processing cost is low, is simple to operate and friendly to environment, and is adapted to
The advantages of industrial applications.
Specific embodiment
With reference to embodiment, the invention will be further described.It is right that following examples are intended to illustrate rather than
The further restriction of the present invention.
Embodiment 1
The 35.1g/L containing V that 10L vanadium slags are obtained Jing after sodium roasting~water logging is taken, the solution of Cr 5.6g/L adds sulphuric acid
PH value of solution is adjusted to 1.8, is heated and solution is kept into boiling 2.5 hours, filtered, obtain liquid after many vanadic acid and precipitation, many vanadic acid take off
Calcine after sodium purity be 98.3% vanadic anhydride product, after precipitation liquid crystallization Natrii Sulfas after return calcining leach operation circulation
Use.
Embodiment 2
5L 34.8g/L containing V, the solution of Cr 11.1g/L are taken, the solution is the sodium chloride crystal mother solution obtained with embodiment 1
Leach the solution that vanadium slag calcining is obtained.Sulfuric acid regulation solution pH to 0.5 is added in solution, is gone back by Cr (VI) by the chromium in solution
Former 1.2 times of addition VO into Cr (III) theoretical amount2Solution made by sulphuric acid is dissolved in, 70 DEG C are reacted 4 hours；Add sodium hydroxide
PH value of solution is adjusted to 2.5, then stoichiometric 1.3 times as needed for precipitation 85 DEG C add ammonium sulfate precipitation to separate out ammonium poly-vanadate, mistake
Filter, obtains liquid after ammonium poly-vanadate and precipitation, and the calcining 2 hours of 550 DEG C of ammonium poly-vanadate obtains the vanadic anhydride that purity is 99.3% and produces
Product；Liquid presses Cr after precipitation3+/NH4 +Mol ratio 1:1.1 add 25 DEG C of crystallizations of ammonium sulfate to separate out NH4Cr(SO4)2Crystal；NH4Cr
(SO4)2By solid-to-liquid ratio 1:3 add water wiring solution-forming, are subsequently adding ammonia and adjust pH value of solution to 6.5 Precipitation hydrated chromium oxides, mistake
Filter to obtain liquid after hydrated chromium oxide and heavy chromium；Hydrated chromium oxide is calcined 2 hours at 850 DEG C, obtains the Cr that purity is 99.5%2O3Product；
Liquid evaporating, concentrating and crystallizing obtains ammonium sulfate after heavy chromium.
Embodiment 3
Take obtain after 10L green muds sodium roasting~water logging containing V12.5g/L, the solution of Cr 20.1g/L adds hydrochloric acid to adjust
Section pH value of solution is reduced into 1.1 times of addition VCl of Cr (III) theoretical amount by Cr (VI) to 1.5 by the chromium in solution3, 50 DEG C of reactions
3 hours；Again stoichiometric 1.5 times as needed for precipitation 95 DEG C add chloride precipitation to separate out ammonium poly-vanadate, filter, much vanadic acid
Liquid after ammonium and precipitation, 500 DEG C of ammonium poly-vanadate calcining 3 hours obtains the vanadic anhydride product that purity is 98.9%；Liquid adds after precipitation
Enter the purification and impurity removals of sodium carbonate regulating solution pH to 3.5, add in sodium hydroxide and the Precipitation hydrated chromium oxides of pH to 6.0,
Gained hydrated chromium oxide is calcined 2 hours at 850 DEG C, obtains the Cr that purity is 98.3%2O3Product.
Embodiment 4
The 35.1g/L containing V that 5L vanadium slags are obtained Jing after sodium roasting~water logging is taken, the solution of Cr 5.6g/L adds sulphuric acid
PH value of solution is adjusted to 1.8, is heated and solution is kept into boiling 2.5 hours, filtered, much liquid after vanadic acid and precipitation.Many vanadic acid are molten
To enter pressurize in the acid solution that pH value is 0.2 to be passed through sulphur dioxide reduction and must contain the solution of Low Valent Vanadium.
Embodiment 5
The 25.8g/L containing V obtained after the high chrome alum slag sodium roasting~water loggings of 10L is taken, the solution of Cr 45.6g/L is added
Sulfuric acid regulation solution pH to 1.0, by the chromium in solution 1.3 times of addition embodiments 4 of Cr (III) theoretical amount are reduced into by Cr (VI)
In the solution containing Low Valent Vanadium, 90 DEG C react 2 hours；Again stoichiometric 1.5 times as needed for precipitation 95 DEG C add ammonium sulfate to sink
Precipitation goes out ammonium poly-vanadate, filters, and obtains liquid after ammonium poly-vanadate and precipitation, and five oxidations that purity is 99.3% are obtained after ammonium poly-vanadate calcining
Two vanadium products；Liquid adds the purification and impurity removals of sodium carbonate regulating solution pH to 3.6 after precipitation, adds in sodium hydroxide and pH to 5.5
Precipitation hydrated chromium oxide, obtains the Cr that purity is 98.6% after hydrated chromium oxide calcining2O3Product.
Claims (9)
1. a kind of method that containing vanadium and chromium solution-selective Reduced separating reclaims vanadium and chromium, comprises the following steps：
The first step：Selective reduction chromium
Adjust containing vanadium and chromium solution ph to 0.1~3.5, then Cr (III) reasons are reduced into by Cr (VI) by the chromium in containing vanadium and chromium solution
1~1.5 times of addition reducing agent of stoichiometric, selective reduction chromium therein, liquid after must reducing；The reducing agent selected from V (IV) or/
With the compound or solution of V (III)；
Second step：Precipitate and separate vanadium
Liquid pH value is adjusted after first step gained reduction to 1.5~3.5, Direct precipitation separates out many vanadic acid, or adjust after reduction liquid pH value extremely
Ammonium salt, Precipitation ammonium poly-vanadate is added to filter liquid after much vanadic acid or ammonium poly-vanadate and precipitation, many vanadium while 1.5~3.5
Acid or ammonium poly-vanadate calcine to obtain vanadic anhydride；
3rd step：Precipitate and separate chromium
Liquid pH value after the precipitation obtained by second step is adjusted to adjust pH value to 4.5~9.5 again to 3.5~4.0 purification and impurity removals, precipitation is hydrated
Chromium oxide, or ammonia or ammonium salt are added in liquid after precipitation, then at a temperature of -15~45 DEG C, crystallization separates out NH4Cr(SO4)2It is brilliant
Body, NH4Cr(SO4)2Crystal makes the transition to obtain hydrated chromium oxide, and hydrated chromium oxide calcines to obtain chromic oxide；The addition of ammonia or ammonium salt
By Cr3+/NH4 +Mol ratio 1:1~3 determines.
2. the method that a kind of containing vanadium and chromium solution-selective Reduced separating according to claim 1 reclaims vanadium and chromium, its feature
It is：The compound of the V (IV) or/and V (III) is selected from VO2、V2O3、Na2VO3、Na2V2O5、NaVO2、(NH4)2O·
2V2O4、VCl4、VCl3、VOCl2、VOCl 、VOSO4、V2 (SO4)3In one or more；The V (IV) or/and V (III)
One kind in acid solution, alkaline solution, the aqueous solution of the compound of V (IV) or/and V (III) of solution or by also
The former solution containing pentavalent vanadium is obtained.
3. the method that a kind of containing vanadium and chromium solution-selective Reduced separating according to claim 2 reclaims vanadium and chromium, its feature
In being the first step, the process conditions of selective reduction are：Reaction temperature is 5~115 DEG C, and the response time is 0.5~6 hour.
4. the method that a kind of containing vanadium and chromium solution-selective Reduced separating according to claim 1 reclaims vanadium and chromium, its feature
It is：In second step, the process conditions of many vanadic acid of Precipitation are：Reaction temperature 60-110 DEG C, 1~6 hour time；Precipitation analysis
The process conditions for going out ammonium poly-vanadate are：Reaction temperature 50-110 DEG C, 1~6 hour time.
5. the method that a kind of containing vanadium and chromium solution-selective Reduced separating according to claim 4 reclaims vanadium and chromium, its feature
It is：In second step, many vanadic acid or ammonium poly-vanadate calcine 0.5-5 hours at 450 ~ 600 DEG C, obtain vanadic anhydride.
6. the method that a kind of containing vanadium and chromium solution-selective Reduced separating according to claim 1 reclaims vanadium and chromium, its feature
It is：In 3rd step, NH4Cr(SO4)2Crystal make the transition hydrated chromium oxide technical process is：NH4Cr(SO4)2Crystal first presses solid-liquid
Than 1:2-10 adds water stirring, adds ammonia or ammonia to adjust pH to 4.5-8.5,25~115 DEG C of stirring 0.5-3.5 hours to filter
Liquid after hydrated chromium oxide and transition, liquid returns NH after transition4Cr(SO4)2Crystallization Procedure is recycled, or evaporating, concentrating and crystallizing is obtained
Ammonium sulfate product.
7. the method that a kind of containing vanadium and chromium solution-selective Reduced separating according to claim 6 reclaims vanadium and chromium, its feature
It is：In 3rd step, hydrated chromium oxide calcines 0.5-6 hours and obtains chromic oxide at 700-900 DEG C.
8. a kind of containing vanadium and chromium solution-selective Reduced separating according to any one of claim 1- 7 reclaims vanadium and chromium
Method, it is characterised in that：In the first step, second step, the 3rd step, system pH is adjusted using acid or alkali, acid is selected from salt
One or more in acid, nitric acid, sulphuric acid, carbonic acid；Alkali is selected from CaO, CaOH, CaCO3、NaOH、NaHCO3、Na2CO3、KOH、
KHCO3、K2CO3、One or more in ammonia.
9. a kind of containing vanadium and chromium solution-selective Reduced separating according to any one of claim 1- 7 reclaims vanadium and chromium
Method, it is characterised in that：In second step, the 3rd step, the ammonium salt of addition is selected from ammonium sulfate, ammonium chloride, ammonium nitrate at least one
Kind.
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| CN105950865B (en) * | 2016-05-17 | 2019-01-04 | 沈阳理工大学 | A method of the separation and Extraction vanadium chromium from high-chromic vanadium leachate |
| CN106916950B (en) * | 2017-03-06 | 2018-08-21 | 中信锦州金属股份有限公司 | A method of producing low chromium ammonium poly-vanadate |
| CN110317961A (en) * | 2019-08-07 | 2019-10-11 | 攀钢集团攀枝花钢铁研究院有限公司 | The method for preparing vanadic anhydride containing vanadium solution |
| CN110629047B (en) * | 2019-10-25 | 2020-10-30 | 中南大学 | Method for separating and extracting vanadium and chromium from vanadium and chromium-containing solution |
| CN112646972B (en) * | 2020-11-13 | 2021-12-24 | 北京科技大学 | Method for separating vanadium and chromium from vanadium and chromium-containing material through chlorination-selective oxidation |
| CN113416847B (en) * | 2021-07-05 | 2022-05-31 | 昆明理工大学 | Method for recycling, reducing and harmlessly treating vanadium extraction tailings |
| CN114408972A (en) * | 2022-01-26 | 2022-04-29 | 重庆科技学院 | Method for comprehensively recovering vanadium and chromium from sodium salt roasting water leaching solution of vanadium-containing steel slag |
| CN115404361B (en) * | 2022-09-02 | 2023-09-29 | 成都先进金属材料产业技术研究院股份有限公司 | Method for preparing high-purity vanadyl sulfate solution from industrial vanadium slag sodium roasting water leaching solution |
| CN117185351A (en) * | 2023-09-07 | 2023-12-08 | 有研资源环境技术研究院(北京)有限公司 | Superfine high-purity chromium oxide and preparation method thereof |
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| CN102041377B (en) * | 2010-11-11 | 2012-04-18 | 武钢集团昆明钢铁股份有限公司 | Method for recovering iron, vanadium and chromium in vanadium-titanium magnetite concentrate |
| CN103849765B (en) * | 2012-12-04 | 2016-02-24 | 中国科学院过程工程研究所 | A kind of precipitate and separate and the method reclaiming vanadium and chromium in vanadium chromium solution |
| JP6183788B2 (en) * | 2014-04-18 | 2017-08-23 | 住友金属鉱山株式会社 | Method for hydrometallizing nickel oxide ore |
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