CN107739826A - A kind of method of the reduction containing sodium content in vanadium leachate - Google Patents
A kind of method of the reduction containing sodium content in vanadium leachate Download PDFInfo
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- CN107739826A CN107739826A CN201711049523.5A CN201711049523A CN107739826A CN 107739826 A CN107739826 A CN 107739826A CN 201711049523 A CN201711049523 A CN 201711049523A CN 107739826 A CN107739826 A CN 107739826A
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- vanadium
- vanadium leachate
- leachate
- ammonium sulfate
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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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- 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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- 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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Abstract
The invention discloses a kind of method of the reduction containing sodium content in vanadium leachate, belong to field of metallurgy.Sodium content is higher for containing at present in vanadium leachate by the present invention, causes subsequent technique tediously long, the relatively low technical problem of purity of vanadium pentoxide, there is provided a kind of method of the reduction containing sodium content in vanadium leachate, this method comprises the following steps：Ammonium sulfate is added in containing vanadium leachate, stirs, ammonium sulfate is fully dissolved, solution filters after cooling crystallization, contains vanadium leachate after must purifying.The inventive method adds ammonium sulfate in containing vanadium leachate, using the method for crystallisation by cooling, separate out substantial amounts of sodium sulfate crystal in leachate, the content containing sodium in vanadium leachate can effectively be reduced, and lost without vanadium, the progress for being advantageous to subsequent technique containing vanadium leachate after purification, shorten the process cycle of vanadic anhydride.
Description
Technical field
The invention belongs to field of metallurgy, and in particular to a kind of method of the reduction containing sodium content in vanadium leachate.
Background technology
Vanadic anhydride is widely used, and demand is big, as the consumption proportion of VN alloy and vanadium functional material is further
Increase, vanadium cell energy storage technology preliminarily form industrialization, and vanadium product variety will the more seriation, various on the basis of extension
Change, functionalization.The application field scope of vanadium constantly expands, and some vanadium downstreams are high-end, high technology content, deep processed product are to vanadium oxygen
The quality of compound especially vanadic anhydride proposes requirements at the higher level.The mostly important high-end product of vanadium application field includes at present
Aerospace grade vananum, all-vanadium flow battery, luminescent material etc..
PZH vanadic-titanomagnetite is maximum navajoite area of China, is characterized in being associated with Various Complex metal, difficulty be present
The problems such as selecting smelting.At present, the technique of the common vanadium extraction from vanadium slag mainly has vanadium slag sodium to heat up water again leaching and vanadium extraction technique and vanadium slag
Calcification baking process for extracting vanadium both.In vanadium slag sodium roasting produces vanadic anhydride technique, usually with sodium chloride or carbon
Sour sodium is roasting additive, by roasting, trivalent vanadium in clinker is converted into water-soluble sodium salt containing pentavalent vanadium, by clinker water
After leaching, it can must contain vanadium leachate, wherein having the impurity such as sodium, chromium, silicon.Acid ammonium salt is added in containing vanadium leachate afterwards, is made
Ammonium metavanadate precipitate is obtained, the ammonium metavanadate precipitate after drying is calcined, thick vanadic anhydride is made, then is cleaned through alkali soluble, uses ammonium
The secondary precipitation of salt obtains ammonium metavanadate, and obtained purity of vanadium pentoxide is more than 98% after roasting.Impurity content in leachate
Higher is always to cause one of the reason for process duration is longer, cost is higher, therefore urgent need one kind can be effective at present
The method containing sodium content in vanadium leachate of reduction.
The content of the invention
The present invention at present contain vanadium leachate in sodium content it is higher, cause subsequent technique tediously long, purity of vanadium pentoxide
Relatively low technical problem, there is provided a kind of efficiently to reduce the method containing sodium content in vanadium leachate.
A kind of method of the reduction containing sodium content in vanadium leachate, this method comprise the following steps：
A, ammonium sulfate is added in containing vanadium leachate, is stirred, ammonium sulfate is fully dissolved, obtain solution A；
B, solution A filters after cooling crystallization, contains vanadium leachate after must purifying.
Wherein, in the above method, in step a, the vanadium concentration containing vanadium leachate is 20~60g/L, na concn 10
~60g/L.
Wherein, in the above method, in step a, the liquid-solid ratio containing vanadium leachate and ammonium sulfate is 10：3~8；Wherein,
Containing vanadium leachate by volume, ammonium sulfate is in mass.
Wherein, in the above method, in step b, the cooling crystallization is stirring cooling crystallization or stands cooling crystallization.
Wherein, in the above method, in step b, the temperature of the standing is -10 DEG C~0 DEG C.
Wherein, in the above method, in step b, the time of the cooling crystallization is 0.5h~5h.
The beneficial effects of the invention are as follows：
The inventive method creativeness adds ammonium sulfate in containing vanadium leachate, using the method for crystallisation by cooling, makes leaching
Substantial amounts of sodium sulfate crystal separates out in liquid, is advantageous to the progress of subsequent technique, shortens the process cycle of vanadic anhydride, improves
Vanadic anhydride quality；Compared with traditional crystallisation by cooling method, the inventive method significantly reduces sodium content containing vanadium leachate,
Crystallisation step separates out without vanadium ion, vanadium recovery 100%, and the process that cleans is simple；The crystal of precipitation using sodium sulphate as
It is main, secondary operation and utilization can be carried out, reduces the generation of solid waste.
Embodiment
Specifically, a kind of method of the reduction containing sodium content in vanadium leachate, this method comprise the following steps：
A, ammonium sulfate is added in containing vanadium leachate, is stirred, ammonium sulfate is fully dissolved, obtain solution A；
B, solution A filters after cooling crystallization, contains vanadium leachate after must purifying.
After being the roasting of sodium method containing vanadium leachate, gone out by water logging obtained, the pH containing vanadium leachate is generally 9~10, mainly
Impurity element is including Na, K, Ca, Cr, Fe, Si etc., wherein [Na]=10~60g/L, [Cr]=0.5~5g/L, [Si]=0.5
~5g/L, [K]=0.2~1.5g/L, [V]=20~60g/L；The V of technical grade2O5There are strict requirements to sodium content, due to vanadium
Acid group is strong to the binding ability of sodium, needs strictly to control sodium content in preparation process, therefore the present invention is for high sodium content
A kind of method of the reduction containing sodium content in vanadium leachate is proposed containing vanadium leachate, so that meeting life containing vanadium leachate after purification
Production requires.
In the inventive method step a, the liquid-solid ratio containing vanadium leachate and ammonium sulfate is 10：3~10:8；Wherein, contain
By volume, (such as in solid-to-liquid ratio, quality and volume are the unit ratios using ad eundem to ammonium sulfate to vanadium leachate in mass
Compared with, such as quality, in units of g, volume is in units of mL)；The purpose of ammonium sulfate is added in introducing sulfuric acid into leachate
Root, by common-ion effect, sodium sulphate is set to be more easy to separate out；It is few to add volume of ammonium sulfate, sodium sulphate is separated out slowly, except sodium effect is failed to understand
It is aobvious；Excessive ammonium sulfate is added, production cost is high, therefore liquid-solid ratio needs to control in certain scope.
In step a, added to containing vanadium leachate after ammonium sulfate, it is necessary to make ammonium sulfate fully dissolve, sodium efficiency removed to improve,
Generally require 0.5~3h of stirring.
The inventive method uses crystallisation by cooling mode, at a lower temperature, because the solubility of ammonium sulfate is significantly larger than sulphur
Sour sodium, reducing temperature can make to separate out in the form of ammonia sulfate crystal containing sodium in vanadium leachate, can effectively reduce containing in vanadium leachate
The content of sodium, while in follow-up calcination process, ammonium root can decompose, will not remaining in the product, avoid ammonium root to follow-up
Process influences；Qualified product is can obtain through a precipitation again containing vanadium solution after gained purification, is advantageous to subsequent technique
Carry out.
Solution A is subjected to crystallisation by cooling in the inventive method, the temperature of crystallization is -10 DEG C~0 DEG C, crystallization time 0.5h
~5h, so that sodium can be separated out fully；Cooling crystallization can use stirring cooling crystallization or stand cooling crystallization；Actual industrial production
In, crystallisation by cooling can be placed in high/low temperature alternation stove and carry out.
Preferably, a kind of method of the reduction containing sodium content in vanadium leachate, this method comprise the following steps：
A, ammonium sulfate is added in containing vanadium leachate, is stirred, ammonium sulfate is fully dissolved, obtain solution A；It is described to be leached containing vanadium
The vanadium concentration of liquid is 20~60g/L, and na concn is 10~60g/L；The liquid-solid ratio containing vanadium leachate and ammonium sulfate is 10：3
~10：8；Wherein, containing vanadium leachate by volume, ammonium sulfate is in mass；
B, under the conditions of solution a is -10 DEG C~0 DEG C in temperature after cooling crystallization 0.5h~5h, filter, containing after must purifying
Vanadium leachate.
The present invention is described in further detail below by test example and embodiment, but therefore not protected the present invention
Scope is limited among described scope of embodiments.
Embodiment 1
Take 500mL to climb steel (vanadium concentration is 30g/L, na concn 20g/L) containing vanadium leachate, add 150g ammonium sulfate, stir
0.5h is mixed, ammonium sulfate is fully dissolved, obtains solution A；Solution A is placed in high/low temperature alternation stove and stirred, is 0 by temperature setting
DEG C, 3h is stirred, there are a large amount of light yellow crystals to separate out, filters, contains vanadium leachate after must purifying；Liquor capacity is determined, detection is molten
Vanadium and impurity content, are computed in liquid, and the clearance of sodium is 32.52%, vanadium recovery 100%.
Embodiment 2
Take 1000mL to climb steel (vanadium concentration is 40g/L, na concn 40g/L) containing vanadium leachate, add 800g ammonium sulfate, stir
3h is mixed, ammonium sulfate is fully dissolved, obtains solution A；Solution A is placed in high/low temperature alternation stove, is -5 DEG C by temperature setting, stands
5h, there are a large amount of light yellow crystals to separate out, filter, contain vanadium leachate after must purifying；Determine liquor capacity, detect solution in vanadium and
Impurity content, it is computed, the clearance of sodium is 41.93%, vanadium recovery 100%.
Embodiment 3
Take 800mL to climb steel (vanadium concentration is 20g/L, na concn 10g/L) containing vanadium leachate, add 400g ammonium sulfate, stir
2h is mixed, ammonium sulfate is fully dissolved, obtains solution A；Leachate is placed in high/low temperature alternation stove, is -10 DEG C by temperature setting, it is quiet
3h is put, there are a large amount of light yellow crystals to separate out, filters, contains vanadium leachate after must purifying；Liquor capacity is determined, detects vanadium in solution
And impurity content, it is computed, the clearance of sodium is 49.56%, vanadium recovery 100%.
From embodiment 1~3, the inventive method, which substantially reduces, contains sodium content in vanadium leachate, crystallisation step without vanadium from
Son separates out, vanadium recovery 100%, and the process letter that cleans；Be advantageous to subsequent technique containing vanadium leachate using after purification
Progress, shorten the process cycle of vanadic anhydride, sodium content substantially reduces in the vanadic anhydride finally prepared.
Claims (6)
1. the method containing sodium content in vanadium leachate of reduction, it is characterised in that：Comprise the following steps：
A, ammonium sulfate is added in containing vanadium leachate, is stirred, ammonium sulfate is fully dissolved, obtain solution A；
B, solution A filters after cooling crystallization, contains vanadium leachate after must purifying.
2. method of the reduction containing sodium content in vanadium leachate according to claim 1, it is characterised in that：It is described in step a
Vanadium concentration containing vanadium leachate is 20~60g/L, and na concn is 10~60g/L.
3. method of the reduction containing sodium content in vanadium leachate according to claim 1 or 2, it is characterised in that：In step a,
The liquid-solid ratio containing vanadium leachate and ammonium sulfate is 10：3~8；Wherein, containing vanadium leachate by volume, ammonium sulfate is with quality
Meter.
4. method of the reduction containing sodium content in vanadium leachate according to claim 1, it is characterised in that：It is described in step b
Cooling crystallization is stirring cooling crystallization or stands cooling crystallization.
5. the method for reduction according to claims 1 to 4 containing sodium content in vanadium leachate, it is characterised in that：In step b,
The temperature of the cooling crystallization is -10 DEG C~0 DEG C.
6. method of the reduction containing sodium content in vanadium leachate according to claim 4 or 5, it is characterised in that：In step b,
The time of the cooling crystallization is 0.5h~5h.
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| CN201711049523.5A CN107739826A (en) | 2017-10-31 | 2017-10-31 | A kind of method of the reduction containing sodium content in vanadium leachate |
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| CN201711049523.5A CN107739826A (en) | 2017-10-31 | 2017-10-31 | A kind of method of the reduction containing sodium content in vanadium leachate |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20040026330A1 (en) * | 2002-04-18 | 2004-02-12 | Bayer Aktiengesellschaft | Process for the utilization of vanadium from chromium ore as vanadium (V) oxide |
| CN101343695A (en) * | 2008-08-20 | 2009-01-14 | 攀钢集团研究院有限公司 | Method for reducing content of kalium and sodium in vanadium solvent extraction circulation liquid |
| WO2011018799A2 (en) * | 2009-08-10 | 2011-02-17 | Aditya Birla Science & Technology Co. Ltd | A process for preparing vanadium oxide from vanadate sludge |
| CN103145187A (en) * | 2013-03-22 | 2013-06-12 | 中南大学 | Production technology of harmless high-purity vanadium pentoxide |
-
2017
- 2017-10-31 CN CN201711049523.5A patent/CN107739826A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20040026330A1 (en) * | 2002-04-18 | 2004-02-12 | Bayer Aktiengesellschaft | Process for the utilization of vanadium from chromium ore as vanadium (V) oxide |
| CN101343695A (en) * | 2008-08-20 | 2009-01-14 | 攀钢集团研究院有限公司 | Method for reducing content of kalium and sodium in vanadium solvent extraction circulation liquid |
| WO2011018799A2 (en) * | 2009-08-10 | 2011-02-17 | Aditya Birla Science & Technology Co. Ltd | A process for preparing vanadium oxide from vanadate sludge |
| CN103145187A (en) * | 2013-03-22 | 2013-06-12 | 中南大学 | Production technology of harmless high-purity vanadium pentoxide |
Non-Patent Citations (1)
| Title |
|---|
| 曹洪文 等: ""钠盐处理含钒铁水及钠化钒渣水浸提钒"", 《钢铁钒钛》 * |
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Application publication date: 20180227 |