CN105714131A - Method for separating and extracting vanadium and chromium from same solution - Google Patents
Method for separating and extracting vanadium and chromium from same solution Download PDFInfo
- Publication number
- CN105714131A CN105714131A CN201610177241.2A CN201610177241A CN105714131A CN 105714131 A CN105714131 A CN 105714131A CN 201610177241 A CN201610177241 A CN 201610177241A CN 105714131 A CN105714131 A CN 105714131A
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- China
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- chromium
- vanadium
- ion exchange
- exchange resin
- chelating ion
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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
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- Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
- Treatment Of Water By Ion Exchange (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention provides a method for separating and extracting vanadium and chromium from the same solution. Mineral acid or NaOH is added to the solution containing vanadium and chromium to adjust the pH value, then the solution flows through a chelated ion exchange resin column till the chelated ion exchange resin column fully adsorbs vanadate radicals to be saturated, the saturated chelated ion exchange resin column is subjected to vanadium dissolution and absorption through a sodium hydroxide or ammonium hydroxide solution, and a vanadate product is prepared through vanadium dissolving liquid; and chromium-containing tail liquid flowing out of the adsorption process is subjected to resin exchange to enrich chromium or used for preparing a chromate product directly through evaporative crystallization. By the adoption of the method, two types of metal can be deeply purified and separated, the use amount of resin is small, the vanadium recycling rate is high, the production efficiency is high, equipment is simple, operation is convenient, no pollution is generated in the production process, and economic benefits are good.
Description
Technical field
The present invention relates to metallurgical technology field, be specially a kind of method of separation and Extraction vanadium chromium from the same solution containing vanadium chromium.
Background technology
At present, all the time, all there is vanadium chromium attendant phenomenon in vanadic salts industry and Chrome Salt Industry great majority in process of production.Owing to vanadium chromium physics, chemical property are close, therefore in industrial processes, two kinds of metals separate the difficult problem being always up puzzlement industrial production technology.Conventional great majority are all adopt the sedimentation method to reclaim two kinds of metals, but the two kinds of salt purity being difficult to be completely separated and obtain are not high.
Summary of the invention
Technical problem solved by the invention is in that to provide a kind of method of separation and Extraction vanadium chromium from same solution, thus the problem solved in above-mentioned background technology.
Technical problem solved by the invention realizes by the following technical solutions:
A kind of method of separation and Extraction vanadium chromium from same solution, by the solution of containing vanadium and chromium after adding mineral acid or NaOH adjustment pH value, flow through chelating ion exchange resin post, until abundant adsorption of vanadium acid group is to saturated in chelating ion exchange resin post, then by saturated chelating ion exchange resin post sodium hydroxide or ammonia spirit desorbing vanadium, solve vanadium liquid and prepare vanadate product；Adsorption process flows out adopt resins exchange enrichment chromium containing chromium tail washings after or directly adopt evaporative crystallization to produce chromate product.
In the present invention, as the preferred technical scheme of one, the solution of containing vanadium and chromium is adjusted PH is 6～8.
In the present invention, as the preferred technical scheme of one, the chelating ion exchange resin post after desorbing adopts mineral acid to add corresponding salt and realizes regeneration.
In the present invention, as the preferred technical scheme of one, adopt following detailed step:
(1) in leaching tanks, add the distilled water of 10-15 weight portion, the then containing vanadium and chromium waste residue (dry slag) of 2-4 weight portion, then add 2～3 weight portion sodium bicarbonate, be warming up to more than 85 DEG C after stirring, be incubated 3-4 hour；
(2) utilizing pressure filter to carry out solid-liquid separation the material in leaching tanks, liquid adds mineral acid or NaOH adjustment pH is 6-8, then stands 2-4 hour；
(3) transport pump is utilized to adsorb to chelating ion exchange resin post the liquid that step (2) obtains, until chelating ion exchange resin post adsorption of vanadium is saturated, chelating ion exchange resin post utilize NaOH or ammonia carry out resin desorption, chelating ion exchange resin post after desorbing adopts mineral acid to add corresponding salt and realizes regeneration, solves vanadium liquid and is used for producing vanadate product；
(4) adsorption process flows out adopt resins exchange enrichment chromium containing chromium tail washings after or directly adopt evaporative crystallization to produce chromate product.
Owing to have employed above technical scheme, the method have the advantages that
For being completely separated two kinds of metals, deep purifying, the present invention adopts two kinds of metals of Strong acid ion-exchanger.The solution of containing vanadium and chromium is flowed through chelating ion exchange resin post (PH6～8) after adding mineral acid or NaOH adjustment pH value, vanadium exists with negative valency vanadic acid radical ion, chromium exists with chromate ion), first vanadium chromium is adsorbed simultaneously, along with constantly carrying out of absorption, the chromate of early stage resin absorption is replaced by vanadic acid root gradually, and chromate can not replace the vanadic acid root in resin.So that two kinds of metals realize separating with acid group form.Loaded resin sodium hydroxide or ammonia spirit desorbing vanadium, finally with mineral acid (adding corresponding salt) regenerating resin.Resins exchange method can also be adopted what adsorption process flowed out to realize reclaiming containing chromium tail washings simultaneously, produce corresponding chromic salts goods.
Energy deep purifying of the present invention separates two kinds of metals, and resin demand is few, and vanadium recovery is high, and production efficiency is high, and equipment is simple, and easy to operate, production process is pollution-free, good in economic efficiency.Particularly suitable navajoite or containing vanadium and chromium tailings separate ore deposit class (it is even higher that vanadium chromium ratio can reach 1:1) containing the difficulty that chromium is high, also can be applied containing vanadium, chromium purification of water field simultaneously.
The method adopting the present invention, metal overall recovery: vanadium: > 99% chromium: > 98.5%；Product purity: vanadic anhydride: 99.45% chromic salts: 97%.
Accompanying drawing explanation
Fig. 1 is present invention process schematic flow sheet.
Detailed description of the invention
For the technological means making the present invention realize, creation characteristic, reach purpose and effect and be easy to understand, below in conjunction with specific embodiment, the present invention is expanded on further.
As shown in Figure 1, a kind of method of separation and Extraction vanadium chromium from same solution, by the solution of containing vanadium and chromium after adding mineral acid or NaOH adjustment pH value, flow through chelating ion exchange resin post, until abundant adsorption of vanadium acid group is to saturated in chelating ion exchange resin post, then by saturated chelating ion exchange resin post sodium hydroxide or ammonia spirit desorbing vanadium, solve vanadium liquid and prepare vanadate product；Adsorption process flows out adopt resins exchange enrichment chromium containing chromium tail washings after or directly adopt evaporative crystallization to produce chromate product.
Embodiment 1
A kind of method of separation and Extraction vanadium chromium from same solution, adopts following detailed step:
(1) in leaching tanks, add the distilled water of 10 weight portions, then the containing vanadium and chromium waste residue (dry slag) of 2 weight portions, then add 2 weight portion sodium bicarbonate, be warming up to 85 DEG C after stirring, be incubated 3 hours；
(2) utilizing pressure filter to carry out solid-liquid separation the material in leaching tanks, it is 6 that liquid adds mineral acid adjustment pH, then stands 2 hours；
(3) transport pump is utilized to adsorb to chelating ion exchange resin post the liquid that step (2) obtains, until chelating ion exchange resin post adsorption of vanadium is saturated, NaOH is utilized to carry out resin desorption on chelating ion exchange resin post, chelating ion exchange resin post after desorbing adopts mineral acid to add corresponding salt and realizes regeneration, solves vanadium liquid and is used for producing vanadate product；
(4) after the employing resins exchange containing chromium tail washings flowed out in adsorption process is enriched with chromium, then evaporative crystallization is adopted to produce chromate product.
The material component obtained such as following table:
One, former slag Main Ingredients and Appearance
Two, leached mud main component
Three, leachate
Four, stripping liquid analysis of components
Five, vanadic anhydride product analysis
Product complies fully with country's GB3283-87 vanadic anhydride standard after chemically examining by analysis.
Embodiment 2
A kind of method of separation and Extraction vanadium chromium from same solution, adopts following detailed step:
(1) in leaching tanks, add the distilled water of 15 weight portions, then the containing vanadium and chromium waste residue (dry slag) of 4 weight portions, then add 3 weight portion sodium bicarbonate, be warming up to 85 DEG C after stirring, be incubated 4 hours；
(2) utilizing pressure filter to carry out solid-liquid separation the material in leaching tanks, liquid adds mineral acid or NaOH adjustment pH is 8, then stands 4 hours；
(3) transport pump is utilized to adsorb to chelating ion exchange resin post the liquid that step (2) obtains, until chelating ion exchange resin post adsorption of vanadium is saturated, ammonia is utilized to carry out resin desorption on chelating ion exchange resin post, chelating ion exchange resin post after desorbing adopts mineral acid to add corresponding salt and realizes regeneration, solves vanadium liquid and is used for producing vanadate product；
(4) what flow out in adsorption process directly adopts evaporative crystallization to produce chromate product containing chromium tail washings.
The material component obtained such as following table:
One, former slag Main Ingredients and Appearance
Two, leached mud main component
Three, leachate
Four, stripping liquid analysis of components
Five, vanadic anhydride product analysis
Product complies fully with country's GB3283-87 vanadic anhydride standard after chemically examining by analysis.
Embodiment 3
A kind of method of separation and Extraction vanadium chromium from same solution, adopts following detailed step:
(1) in leaching tanks, add the distilled water of 10 tons, the then containing vanadium and chromium waste residue (dry slag) of 3 tons, then add 2.5 tons of sodium bicarbonate, be warming up to 87 DEG C after stirring, be incubated 3.5 hours；
(2) utilizing pressure filter to carry out solid-liquid separation the material in leaching tanks, liquid adds mineral acid or NaOH adjustment pH is 7, then stands 3 hours；
(3) transport pump is utilized to adsorb to chelating ion exchange resin post the liquid that step (2) obtains, until chelating ion exchange resin post adsorption of vanadium is saturated, ammonia is utilized to carry out resin desorption on chelating ion exchange resin post, chelating ion exchange resin post after desorbing adopts mineral acid to add corresponding salt and realizes regeneration, solves vanadium liquid and is used for producing vanadate product；
(4) after the employing resins exchange containing chromium tail washings flowed out in adsorption process is enriched with chromium, then evaporative crystallization is adopted to produce chromate product.
The material component obtained such as following table:
One, former slag Main Ingredients and Appearance
Two, leached mud main component
Three, leachate
Four, stripping liquid analysis of components
Five, vanadic anhydride product analysis
Product complies fully with country's GB3283-87 vanadic anhydride standard after chemically examining by analysis.
Embodiment 4
A kind of method of separation and Extraction vanadium chromium from same solution, adopts following detailed step:
(1) in leaching tanks, add the distilled water of 10 weight portions, then the containing vanadium and chromium waste residue (dry slag) of 4 weight portions, then add 2 weight portion sodium bicarbonate, be warming up to 85 DEG C after stirring, be incubated 4 hours；
(2) utilizing pressure filter to carry out solid-liquid separation the material in leaching tanks, liquid adds mineral acid or NaOH adjustment pH is 7, then stands 2 hours；
(3) transport pump is utilized to adsorb to chelating ion exchange resin post the liquid that step (2) obtains, until chelating ion exchange resin post adsorption of vanadium is saturated, chelating ion exchange resin post utilize NaOH or ammonia carry out resin desorption, chelating ion exchange resin post after desorbing adopts mineral acid to add corresponding salt and realizes regeneration, solves vanadium liquid and is used for producing vanadate product；
(4) the employing resins exchange containing chromium tail washings flowed out in adsorption process adopts evaporative crystallization to produce chromate product after being enriched with chromium.
The material component obtained such as following table:
One, former slag Main Ingredients and Appearance
Two, leached mud main component
Three, leachate
Four, stripping liquid analysis of components
Five, vanadic anhydride product analysis
Product complies fully with country's GB3283-87 vanadic anhydride standard after chemically examining by analysis.
Embodiment 5
A kind of method of separation and Extraction vanadium chromium from same solution, adopts following detailed step:
(1) in leaching tanks, add the distilled water of 12 weight portions, then the containing vanadium and chromium waste residue (dry slag) of 2 weight portions, then add 3 weight portion sodium bicarbonate, be warming up to 85 DEG C after stirring, be incubated 4 hours；
(2) utilizing pressure filter to carry out solid-liquid separation the material in leaching tanks, liquid adds mineral acid or NaOH adjustment pH is 6, then stands 2 hours；
(3) transport pump is utilized to adsorb to chelating ion exchange resin post the liquid that step (2) obtains, until chelating ion exchange resin post adsorption of vanadium is saturated, chelating ion exchange resin post utilize NaOH or ammonia carry out resin desorption, chelating ion exchange resin post after desorbing adopts mineral acid to add corresponding salt and realizes regeneration, solves vanadium liquid and is used for producing vanadate product；
(4) adsorption process flows out adopt resins exchange enrichment chromium containing chromium tail washings after or directly adopt evaporative crystallization to produce chromate product.
The material component obtained such as following table:
One, former slag Main Ingredients and Appearance
Two, leached mud main component
Three, leachate
Four, stripping liquid analysis of components
Five, vanadic anhydride product analysis
Product complies fully with country's GB3283-87 vanadic anhydride standard after chemically examining by analysis.
The ultimate principle of the present invention and principal character and advantages of the present invention have more than been shown and described.Skilled person will appreciate that of the industry; the present invention is not restricted to the described embodiments; described in above-described embodiment and description is that principles of the invention is described; without departing from the spirit and scope of the present invention; the present invention also has various changes and modifications, and these changes and improvements both fall within the claimed scope of the invention.Claimed scope is defined by appending claims and equivalent thereof.
Claims (4)
1. the method for separation and Extraction vanadium chromium from same solution, it is characterized in that: by the solution of containing vanadium and chromium after adding mineral acid or NaOH adjustment pH value, flow through chelating ion exchange resin post, until abundant adsorption of vanadium acid group is to saturated in chelating ion exchange resin post, then by saturated chelating ion exchange resin post sodium hydroxide or ammonia spirit desorbing vanadium, solve vanadium liquid and prepare vanadate product；Adsorption process flows out adopt resins exchange enrichment chromium containing chromium tail washings after or directly adopt evaporative crystallization to produce chromate product.
2. a kind of method of separation and Extraction vanadium chromium from same solution as claimed in claim 1, it is characterised in that: the solution of containing vanadium and chromium is adjusted PH is 6～8.
3. a kind of method of separation and Extraction vanadium chromium from same solution as claimed in claim 1, it is characterised in that: the chelating ion exchange resin post after desorbing adopts mineral acid to add corresponding salt and realizes regeneration.
4. a kind of method of separation and Extraction vanadium chromium from same solution as described in any one of claim 1-3, it is characterised in that: adopt following detailed step:
(1) in leaching tanks, add the distilled water of 10-15 weight portion, the then containing vanadium and chromium waste residue of 2-4 weight portion, then add 2～3 weight portion sodium bicarbonate, be warming up to more than 85 DEG C after stirring, be incubated 3-4 hour；
(2) utilizing pressure filter to carry out solid-liquid separation the material in leaching tanks, liquid adds mineral acid or NaOH adjustment pH is 6-8, then stands 2-4 hour；
(3) transport pump is utilized to adsorb to chelating ion exchange resin post the liquid that step (2) obtains, until chelating ion exchange resin post adsorption of vanadium is saturated, chelating ion exchange resin post utilize NaOH or ammonia carry out resin desorption, chelating ion exchange resin post after desorbing adopts mineral acid to add corresponding salt and realizes regeneration, solves vanadium liquid and is used for producing vanadate product；
(4) adsorption process flows out adopt resins exchange enrichment chromium containing chromium tail washings after or directly adopt evaporative crystallization to produce chromate product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610177241.2A CN105714131A (en) | 2016-03-26 | 2016-03-26 | Method for separating and extracting vanadium and chromium from same solution |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610177241.2A CN105714131A (en) | 2016-03-26 | 2016-03-26 | Method for separating and extracting vanadium and chromium from same solution |
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| CN105714131A true CN105714131A (en) | 2016-06-29 |
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| CN201610177241.2A Pending CN105714131A (en) | 2016-03-26 | 2016-03-26 | Method for separating and extracting vanadium and chromium from same solution |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN102876895A (en) * | 2012-10-09 | 2013-01-16 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for recycling vanadium and chromium from low-concentration pentavalent vanadium and hexavalent chromium mixed liquor |
| CN105087933A (en) * | 2015-09-24 | 2015-11-25 | 重庆大学 | Method for separating vanadium and chromium from vanadium and chromium mixed solution |
-
2016
- 2016-03-26 CN CN201610177241.2A patent/CN105714131A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN102876895A (en) * | 2012-10-09 | 2013-01-16 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for recycling vanadium and chromium from low-concentration pentavalent vanadium and hexavalent chromium mixed liquor |
| CN105087933A (en) * | 2015-09-24 | 2015-11-25 | 重庆大学 | Method for separating vanadium and chromium from vanadium and chromium mixed solution |
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Application publication date: 20160629 |
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