CN106222412A - A kind of from containing the method for extracting vanadium vanadium solution - Google Patents
A kind of from containing the method for extracting vanadium vanadium solution Download PDFInfo
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- CN106222412A CN106222412A CN201610780592.2A CN201610780592A CN106222412A CN 106222412 A CN106222412 A CN 106222412A CN 201610780592 A CN201610780592 A CN 201610780592A CN 106222412 A CN106222412 A CN 106222412A
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- 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
- C22B3/26—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds
- C22B3/41—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds using a solution of normally solid organic compounds, e.g. dissolved polymers, sugars, or the like
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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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- General Life Sciences & Earth Sciences (AREA)
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Abstract
The present invention relates to a kind of from containing the method for extracting vanadium vanadium solution.Its technical scheme is: by surfactant, carrier, liquid paraffin, membrane solvent mixing, obtain mixing organic facies；Again back washing agent is added in described mixing organic facies, stirring, prepare emulsion；Vanadium solution will be contained mix with described emulsion, stirring, stand, split-phase, and obtain loading vanadium emulsion and one section of raffinate；By described load vanadium emulsion breaking, split-phase, obtain lean organic phase and rich vanadium liquid；Being mixed with described one section of raffinate by described lean organic phase, stirring, stand, split-phase, obtain loading vanadium organic facies and two-stage nitration raffinate, described load vanadium organic facies directly returns breast the most processed.The present invention has the advantages that Solvent quantity is few, technological process is short, vanadium recovery is high, production efficiency is high and continuous production is strong.
Description
Technical field
The invention belongs to extracting vanadium from stone coal technical field.It is specifically related to a kind of from containing the method for extracting vanadium vanadium solution.
Background technology
V is extracted from bone coal2O5Have become as China and obtain a kind of important channel of vanadium resource.Owing to vanadium occurrence status is multiple
Miscellaneous, grade is relatively low, needs to use concentrated acid or strong acid to leach, and causes the pH of leaching solution Al concentration below 0, in foreign ion to be
10 ~ 20g/L and Fe concentration are 4 ~ 8g/L, make subsequent purification enrichment operation be difficult to be normally carried out.
When processing this peracid many impurity leachate, it is low to there is separation efficiency in ion-exchange process, resin easily poisoning etc.
Problem (Li W.Comparison of ion exchange and solvent extraction in recovering
vanadium from sulfuric acid leach solutions of stone coal[J].
Hydrometallurgy, 2013,131-132:1-7).And solvent extraction with its strong adaptability, selectivity is high, balancing speed is fast
The most extensively applied etc. advantage." a kind of method controlling the extracting vanadium that ferrum is extracted from bone coal navajoite leachate "
(CN102560115A) patented technology, uses 2.5mol/LP204 organic facies, is just extracting 4 ~ 6 times, back extraction 3 ~ 4 times.Before extraction,
First extraction stock solution is carried out reduction treatment, ferric ion is reduced to ferrous ion, thus reduces extractant to impurity iron
The extraction yield of ion, reduces the difficulty of organic facies regeneration, but it is big to there is extractant consumption, just extracts, the lacking of back extraction progression length
Point.
Liquid film extraction just extracts, back extraction one step is carried out, and concentration ratio is high, can realize the one-level to purpose ion in theory complete
Extraction, can make up solvent extraction progression length, shortcoming that extractant consumption is big, is used widely in field of waste water treatment, but
It is to there is extraction time length, swelling big problem when processing high concentration leachate." a kind of pressurized acid leaching-emulsion liquid membrane carries
The method taking nickel in lateritic nickel ore " (CN104232891A), use emulsion liquid membrane to process lateritic nickel ore pickle liquor, by will
Extraction mixing time is foreshortened to 20min by the method that pickle liquor dilute is 3 times, has reached good effect of extracting.But leaching
After going out liquid dilution, the disposal ability of unit emulsion declines, and also reduces production efficiency simultaneously.
In sum, when extraction is containing vanadium solution, existing technique exists that Solvent quantity is big, extraction progression length, produce effect
The shortcoming that rate is low.
Summary of the invention
It is contemplated that overcome the deficiencies in the prior art, it is therefore intended that Solvent quantity is few, technological process is short to provide one
High with production efficiency from containing the method for extracting vanadium vanadium solution.
For achieving the above object, the comprising the concrete steps that of the technical solution used in the present invention:
Step one, preparation mixing organic facies
By volume percentage composition, carrier, the liquid paraffin of 8 ~ 12%, the surfactant of 2 ~ 8% and surplus by 5 ~ 15% are that film is molten
Agent mixes, and obtains mixing organic facies.
Step 2, preparation emulsion
Again by described mixing organic facies: the volume ratio of back washing agent is 1: (1 ~ 1.3), described back washing agent is added described mixing organic
Xiang Zhong, stirs 5 ~ 20min under the conditions of rotating speed is 2000 ~ 3000r/min, obtains emulsion.
The concentration of described back washing agent is 0.2 ~ 2mol/L.
Step 3, liquid film extraction
By described emulsion: the volume ratio containing vanadium solution is 1: (2 ~ 8), by described emulsion and described containing vanadium solution mix, stirring 10 ~
60min, stands, split-phase, obtains loading vanadium emulsion and one section of raffinate.
The described pH value containing vanadium solution is 1 ~ 10, is 0.5 ~ 6g/L containing the vanadium concentration in vanadium solution.
Step 4, breakdown of emulsion
Described load vanadium emulsion is carried out breakdown of emulsion, stands, split-phase, obtain lean organic phase and rich vanadium liquid.
Step 5, solvent extraction
By described lean organic phase: the volume ratio of described one section of raffinate is 1: (4 ~ 18.4), by described lean organic phase and described
Section raffinate mixing, stirs 1 ~ 15min, stands, split-phase, obtains loading vanadium organic facies and two-stage nitration raffinate；Described load vanadium has
Machine the most directly returns step 2 breast the most processed.
Described carrier be acidic extractant or for basic extractant for Neutral-neutral Extractants or for acidic extractant and in
The mixture of property extractant or be the mixture of basic extractant and Neutral-neutral Extractants.
Described surfactant is more than one in sorbitan fatty acid esters, poly-amine surfactants.
Described membrane solvent is more than one in kerosene, alcohols, organic solvent of ketone.
Described back washing agent is sulfuric acid solution or for sodium hydroxide solution or for sodium carbonate liquor.
The present invention uses liquid film extraction to combine with solvent extraction the method for extracting vanadium, compared with prior art, have as
Lower good effect:
(1) instant invention overcomes solvent extraction just extracting and back extraction progression length, shortcoming that Solvent quantity is big, just extracting and back extraction one step
Carry out, have the advantages that Solvent quantity is few and technological process is short.
(2) vanadium in raffinate is carried out back by the stronger extracting power of the lean organic phase obtained after the present invention utilizes breakdown of emulsion
Receiving, total extraction yield reaches more than 99.9%, has the advantages that vanadium recovery is high.
(3) present invention uses liquid film extraction to combine with solvent extraction the method for extracting vanadium, reduces the place of liquid film extraction
Reason pressure, it is ensured that the low swelling ratio of emulsion and rupture rate, and the load vanadium organic facies obtained by solvent extraction is without back extraction
Directly return preparation emulsion and carry out liquid film extraction, have the advantages that production efficiency is high, continuous production is strong.
Therefore, the present invention has that Solvent quantity is few, technological process is short, vanadium recovery is high, production efficiency is high and gives birth to continuously
The feature that producing property is strong.
Detailed description of the invention
Below in conjunction with detailed description of the invention, the present invention will be further described, not the restriction to its protection domain:
Embodiment 1
A kind of from containing the method for extracting vanadium vanadium solution.Comprising the concrete steps that of described method:
Step one, preparation mixing organic facies
By volume percentage composition, carrier, the liquid paraffin of 8 ~ 9%, the surfactant of 2 ~ 5% and surplus by 5 ~ 9% are membrane solvent
Mixing, obtains mixing organic facies.
Step 2, preparation emulsion
Again by described mixing organic facies: the volume ratio of back washing agent is 1: (1 ~ 1.1), described back washing agent is added described mixing organic
Xiang Zhong, stirs 5 ~ 20min under the conditions of rotating speed is 2000 ~ 3000r/min, obtains emulsion.
The concentration of described back washing agent is 0.2 ~ 1mol/L.
Step 3, liquid film extraction
By described emulsion: the volume ratio containing vanadium solution is 1: (2 ~ 5), by described emulsion and described containing vanadium solution mix, stirring 10 ~
30min, stands, split-phase, obtains loading vanadium emulsion and one section of raffinate.
The described pH value containing vanadium solution is 1 ~ 10, is 0.5 ~ 3g/L containing the vanadium concentration in vanadium solution.
Step 4, breakdown of emulsion
Described load vanadium emulsion is carried out breakdown of emulsion, stands, split-phase, obtain lean organic phase and rich vanadium liquid.
Step 5, solvent extraction
By described lean organic phase: the volume ratio of described one section of raffinate is 1: (4 ~ 10.5), by described lean organic phase and described
Section raffinate mixing, stirs 1 ~ 9min, stands, split-phase, obtains loading vanadium organic facies and two-stage nitration raffinate；Described load vanadium is organic
The most directly return step 2 breast the most processed.
In the present embodiment: described carrier is acidic extractant；Described surfactant is sorbitan fatty acid esters；
Described membrane solvent is kerosene；Described back washing agent is sulfuric acid solution.
Embodiment 2
A kind of from containing the method for extracting vanadium vanadium solution.In addition to following component, remaining is with embodiment 1:
Described carrier is the mixture of basic extractant and Neutral-neutral Extractants；Described surfactant is polyamine class surface activity
Agent；Described membrane solvent is the mixture of alcohols and organic solvent of ketone；Described back washing agent is sodium carbonate liquor.
Embodiment 3
A kind of from containing the method for extracting vanadium vanadium solution.Comprising the concrete steps that of described method:
Step one, preparation mixing organic facies
By volume percentage composition, carrier, the liquid paraffin of 9 ~ 10%, the surfactant of 3 ~ 6% and surplus by 7 ~ 11% are that film is molten
Agent mixes, and obtains mixing organic facies.
Step 2, preparation emulsion
Again by described mixing organic facies: the volume ratio of back washing agent is 1: (1.1 ~ 1.2), the described mixing of addition of described back washing agent is had
Machine mutually in, under the conditions of rotating speed is 2000 ~ 3000r/min stir 5 ~ 20min, obtain emulsion.
The concentration of described back washing agent is 0.6 ~ 1.4mol/L.
Step 3, liquid film extraction
By described emulsion: the volume ratio containing vanadium solution is 1: (3 ~ 6), by described emulsion and described containing vanadium solution mix, stirring 20 ~
40min, stands, split-phase, obtains loading vanadium emulsion and one section of raffinate.
The described pH value containing vanadium solution is 1 ~ 10, is 1.5 ~ 4g/L containing the vanadium concentration in vanadium solution.
Step 4, breakdown of emulsion
Described load vanadium emulsion is carried out breakdown of emulsion, stands, split-phase, obtain lean organic phase and rich vanadium liquid.
Step 5, solvent extraction
By described lean organic phase: the volume ratio of described one section of raffinate is 1: (6.3 ~ 13.2), by described lean organic phase and described
One section of raffinate mixing, stirs 3 ~ 11min, stands, split-phase, obtains loading vanadium organic facies and two-stage nitration raffinate；Described load vanadium
Organic facies directly returns step 2 breast the most processed.
In the present embodiment: described carrier is basic extractant；Described surfactant is poly-amine surfactants；Described
Membrane solvent is alcohols；Described back washing agent is sodium hydroxide solution.
Embodiment 4
A kind of from containing the method for extracting vanadium vanadium solution.In addition to following component, remaining is with embodiment 3:
Described carrier is acidic extractant；Described surfactant is sorbitan fatty acid esters and polyamine class surface activity
The mixture of agent；Described membrane solvent is the mixture of kerosene and organic solvent of ketone；Described back washing agent is sulfuric acid solution.
Embodiment 5
A kind of from containing the method for extracting vanadium vanadium solution.Comprising the concrete steps that of described method:
Step one, preparation mixing organic facies
By volume percentage composition, carrier, the liquid paraffin of 10 ~ 11%, the surfactant of 4 ~ 7% and surplus by 9 ~ 13% are film
Solvent mixes, and obtains mixing organic facies.
Step 2, preparation emulsion
Again by described mixing organic facies: the volume ratio of back washing agent is 1: (1.2 ~ 1.3), the described mixing of addition of described back washing agent is had
Machine mutually in, under the conditions of rotating speed is 2000 ~ 3000r/min stir 5 ~ 20min, obtain emulsion.
The concentration of described back washing agent is 1 ~ 1.6mol/L.
Step 3, liquid film extraction
By described emulsion: the volume ratio containing vanadium solution is 1: (4 ~ 7), by described emulsion and described containing vanadium solution mix, stirring 30 ~
50min, stands, split-phase, obtains loading vanadium emulsion and one section of raffinate.
The described pH value containing vanadium solution is 1 ~ 10, is 2.5 ~ 5g/L containing the vanadium concentration in vanadium solution.
Step 4, breakdown of emulsion
Described load vanadium emulsion is carried out breakdown of emulsion, stands, split-phase, obtain lean organic phase and rich vanadium liquid.
Step 5, solvent extraction
By described lean organic phase: the volume ratio of described one section of raffinate is 1: (8.8 ~ 16.1), by described lean organic phase and described
One section of raffinate mixing, stirs 5 ~ 13min, stands, split-phase, obtains loading vanadium organic facies and two-stage nitration raffinate；Described load vanadium
Organic facies directly returns step 2 breast the most processed.
In the present embodiment: described carrier is Neutral-neutral Extractants；Described surfactant is sorbitan fatty acid esters
Mixture with poly-amine surfactants；Described membrane solvent is organic solvent of ketone；Described back washing agent is sodium carbonate liquor.
Embodiment 6
A kind of from containing the method for extracting vanadium vanadium solution.In addition to following component, remaining is with embodiment 5:
Described carrier is basic extractant；Described surfactant is sorbitan fatty acid esters；Described membrane solvent is coal
Oil, alcohols and the mixture of organic solvent of ketone；Described back washing agent is sodium hydroxide solution.
Embodiment 7
A kind of from containing the method for extracting vanadium vanadium solution.Comprising the concrete steps that of described method:
Step one, preparation mixing organic facies
By volume percentage composition, carrier, the liquid paraffin of 11 ~ 12%, the surfactant of 5 ~ 8% and surplus by 11 ~ 15% are film
Solvent mixes, and obtains mixing organic facies.
Step 2, preparation emulsion
Again by described mixing organic facies: the volume ratio of back washing agent is 1: (1.2 ~ 1.3), the described mixing of addition of described back washing agent is had
Machine mutually in, under the conditions of rotating speed is 2000 ~ 3000r/min stir 5 ~ 20min, obtain emulsion.
The concentration of described back washing agent is 1.4 ~ 2mol/L.
Step 3, liquid film extraction
By described emulsion: the volume ratio containing vanadium solution is 1: (5 ~ 8), by described emulsion and described containing vanadium solution mix, stirring 40 ~
60min, stands, split-phase, obtains loading vanadium emulsion and one section of raffinate.
The described pH value containing vanadium solution is 1 ~ 10, is 3.5 ~ 6g/L containing the vanadium concentration in vanadium solution.
Step 4, breakdown of emulsion
Described load vanadium emulsion is carried out breakdown of emulsion, stands, split-phase, obtain lean organic phase and rich vanadium liquid.
Step 5, solvent extraction
By described lean organic phase: the volume ratio of described one section of raffinate is 1: (11 ~ 18.4), by described lean organic phase and described
Section raffinate mixing, stirs 7 ~ 15min, stands, split-phase, obtains loading vanadium organic facies and two-stage nitration raffinate；Described load vanadium has
Machine the most directly returns step 2 breast the most processed.
In the present embodiment: described carrier is the mixture of acidic extractant and Neutral-neutral Extractants；Described surfactant is
Sorbitan fatty acid esters；Described membrane solvent is the mixture of kerosene and alcohols；Described back washing agent is sulfuric acid solution.
Embodiment 8
A kind of from containing the method for extracting vanadium vanadium solution.In addition to following component, remaining is with embodiment 1:
Described carrier is Neutral-neutral Extractants；Described surfactant is poly-amine surfactants；Described membrane solvent is kerosene；Institute
Stating back washing agent is sodium carbonate liquor.
This detailed description of the invention uses liquid film extraction to combine with solvent extraction the method for extracting vanadium, compared with prior art, has
There is a following good effect:
(1) this detailed description of the invention overcomes solvent extraction and is just extracting and back extraction progression length, shortcoming that Solvent quantity is big, just extracting with
Back extraction one step is carried out, and has the advantages that Solvent quantity is few and technological process is short.
(2) the stronger extracting power of the lean organic phase obtained after this detailed description of the invention utilizes breakdown of emulsion is to the vanadium in raffinate
Reclaiming, total extraction yield reaches more than 99.9%, has the advantages that vanadium recovery is high.
(3) this detailed description of the invention uses liquid film extraction to combine with solvent extraction the method for extracting vanadium, reduces liquid film
The processing pressure of extraction, it is ensured that the low swelling ratio of emulsion and rupture rate, and the load vanadium organic facies that solvent extraction is obtained
Directly return preparation emulsion without back extraction and carry out liquid film extraction, have the advantages that production efficiency is high, continuous production is strong.
Therefore, this detailed description of the invention has that Solvent quantity is few, technological process is short, vanadium recovery is high, production efficiency is high
The feature strong with continuous production.
Claims (5)
1. one kind from containing the method for extracting vanadium vanadium solution, it is characterised in that comprising the concrete steps that of described method:
Step one, preparation mixing organic facies
By volume percentage composition, carrier, the liquid paraffin of 8 ~ 12%, the surfactant of 2 ~ 8% and surplus by 5 ~ 15% are that film is molten
Agent mixes, and obtains mixing organic facies；
Step 2, preparation emulsion
Again by described mixing organic facies: the volume ratio of back washing agent is 1: (1 ~ 1.3), described back washing agent is added described mixing organic
Xiang Zhong, stirs 5 ~ 20min under the conditions of rotating speed is 2000 ~ 3000r/min, obtains emulsion；
The concentration of described back washing agent is 0.2 ~ 2mol/L；
Step 3, liquid film extraction
By described emulsion: the volume ratio containing vanadium solution is 1: (2 ~ 8), by described emulsion and described containing vanadium solution mix, stirring 10 ~
60min, stands, split-phase, obtains loading vanadium emulsion and one section of raffinate；
The described pH value containing vanadium solution is 1 ~ 10, is 0.5 ~ 6g/L containing the vanadium concentration in vanadium solution；
Step 4, breakdown of emulsion
Described load vanadium emulsion is carried out breakdown of emulsion, stands, split-phase, obtain lean organic phase and rich vanadium liquid；
Step 5, solvent extraction
By described lean organic phase: the volume ratio of described one section of raffinate is 1: (4 ~ 18.4), by described lean organic phase and described
Section raffinate mixing, stirs 1 ~ 15min, stands, split-phase, obtains loading vanadium organic facies and two-stage nitration raffinate；Described load vanadium has
Machine the most directly returns step 2 breast the most processed.
The most according to claim 1 from containing the method for extracting vanadium vanadium solution, it is characterised in that described carrier is acid extract
Take agent or for basic extractant or for Neutral-neutral Extractants or for acidic extractant and the mixture of Neutral-neutral Extractants or for alkali
Property extractant and the mixture of Neutral-neutral Extractants.
The most according to claim 1 from containing the method for extracting vanadium vanadium solution, it is characterised in that described surfactant is
More than one in sorbitan fatty acid esters, poly-amine surfactants.
The most according to claim 1 from containing the method for extracting vanadium vanadium solution, it is characterised in that described membrane solvent be kerosene,
More than one in alcohols, organic solvent of ketone.
The most according to claim 1 from containing the method for extracting vanadium vanadium solution, it is characterised in that described back washing agent is sulphuric acid
Solution or be sodium hydroxide solution or for sodium carbonate liquor.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201610780592.2A CN106222412A (en) | 2016-08-31 | 2016-08-31 | A kind of from containing the method for extracting vanadium vanadium solution |
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| CN201610780592.2A CN106222412A (en) | 2016-08-31 | 2016-08-31 | A kind of from containing the method for extracting vanadium vanadium solution |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107058765A (en) * | 2017-04-26 | 2017-08-18 | 武汉理工大学 | A kind of V-extracting solvent impregnating resin and its preparation method and application |
| CN107502747A (en) * | 2017-10-13 | 2017-12-22 | 重庆大学 | It is a kind of with microemulsion from vanadium wastewater extracting vanadium method |
| CN112080765A (en) * | 2020-08-07 | 2020-12-15 | 江苏理工学院 | Method for recovering palladium chloride in waste colloidal palladium activation solution |
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| CN102757107A (en) * | 2012-08-10 | 2012-10-31 | 长沙矿冶研究院有限责任公司 | Microemulsion liquid membrane chemical and treating method thereof applicable to treating heavy metal, ammonia nitrogen and radioactive wastewater |
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| CN102757107A (en) * | 2012-08-10 | 2012-10-31 | 长沙矿冶研究院有限责任公司 | Microemulsion liquid membrane chemical and treating method thereof applicable to treating heavy metal, ammonia nitrogen and radioactive wastewater |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107058765A (en) * | 2017-04-26 | 2017-08-18 | 武汉理工大学 | A kind of V-extracting solvent impregnating resin and its preparation method and application |
| CN107058765B (en) * | 2017-04-26 | 2019-03-19 | 武汉理工大学 | A kind of V-extracting solvent impregnating resin and its preparation method and application |
| CN107502747A (en) * | 2017-10-13 | 2017-12-22 | 重庆大学 | It is a kind of with microemulsion from vanadium wastewater extracting vanadium method |
| CN112080765A (en) * | 2020-08-07 | 2020-12-15 | 江苏理工学院 | Method for recovering palladium chloride in waste colloidal palladium activation solution |
| CN112080765B (en) * | 2020-08-07 | 2021-10-19 | 江苏理工学院 | Method for recovering palladium chloride in waste colloidal palladium activation solution |
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Application publication date: 20161214 |