CN106636673B - A method of lithium is extracted from salt lake bittern using extraction - Google Patents
A method of lithium is extracted from salt lake bittern using extraction Download PDFInfo
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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
- C22B26/00—Obtaining alkali, alkaline earth metals or magnesium
- C22B26/10—Obtaining alkali metals
- C22B26/12—Obtaining lithium
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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
- C22B3/40—Mixtures
- C22B3/409—Mixtures at least one compound being an organo-metallic compound
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- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/007—Contaminated open waterways, rivers, lakes or ponds
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Abstract
The present invention relates to a kind of method for extracting lithium from salt lake bittern using extraction, this method produces the production process of lithium carbonate and lithium chloride suitable for being concentrated from salt lake brine with high magnesium-lithium ratio and salt pan containing lithium old halogen.This method uses co-extraction agent FeCl3, extractant and diluent carry out the extraction of lithium, the extractant is the mixture of neutral phosphorus oxygen class compound A and phase modifier B, the wherein described phase modifier B is to extract the organic compound that protonation reaction can occur in reaction process with neutral phosphorus oxygen class compound A, and the extracted species group after the extractant extraction lithium becomes xLiFeCl4YHClaAbB, the extracted species are soluble in diluent, and extraction system has good split-phase performance and back extraction, regenerability, advanced optimized the technique that extraction carries lithium.The method of the present invention is low for equipment requirements, organic compound used is cheap and easy to get, is suitable for commercial Application.
Description
Technical field
The present invention relates to chemical technology field more particularly to a kind of sides extracting lithium from salt lake bittern using extraction
Method.
Background technology
Lithium has various excellent properties, is referred to as " energy metal of 21st century ", " industrial monosodium glutamate ", " space of tomorrow
Navigate alloy ", strategic position is notable.Salt lake bittern is the valuable source of lithium, and China has abundant salt lake bittern lithium resource, storage
It measures at the forefront in the world.The brine that foreign countries have produced now carries lithium and is all only limitted to the lower brine containing magnesium density, and Mg/Li ratio value is less than
6:1, and detached in so-called " high Mg/Li ratio " brine for containing high concentration magnesium, low concentration lithium for such as China Caidamu Basin salt lake
Lithium is extracted, is generally acknowledged worldwide technological puzzle.
Solvent extraction technology is the effective technology of the various metals of separation and Extraction from solution, in carrying for low concentration intentional metal
Take aspect to be widely used, there is simple separative efficiency high, technique and equipment, operation serialization, be easily achieved automatically control etc. it is excellent
Point, researcher extract separating Li from salt lake brine with high magnesium-lithium ratio to solvent extraction technology and have carried out a large amount of research, it is proposed that
Several extraction systems and technique, wherein with FeCl3Make co-extraction agent, the closest industry of system that tributyl phosphate makees extractant is answered
With.The Chinese invention patent 87103431 of the application of Qinghai Yanhu Inst., Chinese Academy of Sciences in 1987, which proposes, uses FeCl3It is total to
Extract agent, the system and technique of the kerosin extraction lithium of single extractant tributyl phosphate, which has carried out big bavin denier salt lake
The pilot-plant test of lithium is extracted in brine.But the system middle and high concentration tributyl phosphate exist it is strong to extraction equipment corrosivity,
The water-soluble loss of organic phase is big, the deficiencies of easily degrading in acid medium, it is difficult to large-scale industrial application.Chinese section in 2012
Institute's Qinghai Salt Lake is studied apllied Chinese invention patent 201210055323.1 and is proposed with alkali metal chloride, alkaline earth gold
Belong to the full alkali phase inversion of full acid in or mixtures thereof chloride substitution 87103431 extraction process of Chinese invention patent, to reduce soda acid
The corrosion of expense and reduction to equipment, the Chinese invention patent of the application of Qinghai Yanhu Inst., Chinese Academy of Sciences in 2012
201210164150.7 propose with the extraction system that the mixture of amides and neutral phosphorus oxygen class compound is extractant, the extraction
Take system that can reduce the corrosion to equipment, document " N523-TBP- sulfonated kerosene extractor bodies compared to single extractant tributyl phosphate
Be the technical study that lithium is extracted from Saturated with Magnesium chloride bittern " (when east etc., salt lake research, 2013,21 (2)：52-57) report in detail
The mixture of the novel amide kind of extractants N523 in road and neutral phosphorus oxygen kind of extractants TBP is the extraction system of extractant, is used
The new extraction system of " 20%N523-30%TBP-50% sulfonated kerosenes ", has studied adverse current cascade extraction, washing, back extraction, phase inversion
The technological parameter of equal workshop sections, it is determined that extraction process flow completes the experiment of whole process extraction process, for lithium concentration about 2g/
L, Mg/Li ratio about 55:1 Qinghai salt lake carries old halogen after potassium, and for the extraction system after 8 grades of whole processes extract, lithium extraction yield is reachable
To 96% or more, extraction split-phase is fast, no three-phase and emulsion.The phase inversion regenerative process of the extraction system organic phase is that hydrochloric acid is anti-
Empty load organic phases after extraction neutralize the acid in organic phase after being shaken up with quantitative sodium hydroxide, then contact and will enter with raffinate
The iron of water phase extracts into organic phase, makes HFeCl4It is converted into NaFeCl4、Mg(FeCl4)2, keep the ability that extractant restores extraction lithium complete
At phase inversion process, the amount that alkali is added must be accurately controlled during phase inversion, caustic dosage is too low, can seriously affect regeneration organic phase lithium
Extracting power, caustic dosage is too high, and excessive alkali cannot can be seriously affected by the sour complete neutralization in brine in load organic phases
Split-phase effect proposes industrial controlled level very high requirement.On the whole, existing salt lake bittern extraction carries lithium side
Method still remains that technological process is complicated, extraction agent price is high, extraction equipment requirement for anticorrosion is high and invests big, whole production cost
It is high.
Invention content
In view of the deficiencies of the prior art, it is an object of the present invention to provide a kind of corrosivity and technique stream that can be reduced to equipment
Journey is simply controllable, the method for being easy to extract lithium in the slave salt lake bittern of Project Realization.
The present invention provides a kind of method for extracting lithium from salt lake bittern using extraction, uses co-extraction agent FeCl3, extraction
Agent and diluent is taken to carry out the extraction of lithium, the extractant is the mixture of neutral phosphorus oxygen class compound A and phase modifier B, institute
It is to extract the organic compound that protonation reaction can occur in reaction process with neutral phosphorus oxygen class compound A to state phase modifier B, institute
Stating the extracted species group after extractant extraction lithium becomes xLiFeCl4YHClaAbB, extractant regenerated after extracting lithium through back extraction-
Journey can return to extraction and carry lithium.
The method for extracting lithium from salt lake bittern using extraction specifically includes following step：
1) blank organic phase is prepared：Dilution dilution agent is used after neutral phosphorus oxygen class compound A and phase modifier B are mixed,
The neutral phosphorus oxygen class compound of control ratio in blank organic phase is 10%~40%；
2) prepared by load organic phases：Organic phase load titanium tetrachloride complex compound and hydrochloric acid：By above-mentioned blank organic phase and packet
Solution containing 0.1~1mol/l ferric trichlorides and 0.1~1mol/l hydrochloric acid is according to volume ratio 1:1 is mixed, and is stood after oscillation
Split-phase obtains the load organic phases of load iron and acid；
3) load organic phases make the transition：Load organic phases are mixed with the chloride solution of alkali metal, split-phase is stood after oscillation,
Complete load organic phases transition；
4) extraction section：Load organic phases after transition are mixed with brine containing lithium, split-phase is stood after oscillation, are measured respectively point
Organic phase and water phase Li after phase+、Mg2+、Na+And K+Concentration calculates the separation of Li/Mg, Li/Na and Li/K, it is known that Li+It is transferred to
Into organic phase, and Mg2+、Na+And K+It is transferred in water phase.Wherein Li in brine+With LiFeCl4Complex form exists；
5) washing section：It is mixed with organic using water phase, split-phase is stood after oscillation, repeatedly, by the Mg in organic phase2 +、Na+And K+It is transferred in water phase；
The method for extracting lithium from salt lake bittern using extraction can also include that stripping section and organic phase regenerate,
Wherein stripping section includes the following steps：The organic phase of extraction lithium is taken, 1-6mol/l hydrochloric acid is added thereto, oscillation is quiet after ten minutes
Set split-phase, H+With HFeCl4Complex form extracts the Li into organic phase, and in organic phase+It is counter enter water phase, wherein emerald green area's lithium is organic
It is preferably mutually 20 with the volume ratio of hydrochloric acid：1.
The organic phase regeneration includes the following steps：The chlorination of 3~6mol/l is added in organic phase after taking hydrochloric acid to be stripped
Magnesium solution, oscillation stand split-phase to get regeneration organic phase after ten minutes, and regeneration organic phase, which can return to extract, carries lithium.
It is above-mentioned using extraction from the method for extracting lithium in salt lake bittern, the described neutral phosphorus oxygen class compound A
For the one or two of tributyl phosphate TBP, trioctyl phosphate TOP.The phase modifier B is itself or can be carried after extracting hydrochloric acid
Protogenic organic compound, it is preferable that the phase modifier B be high-carbon alcohol compound, one kind in aminated compounds or
A combination thereof.It is highly preferred that the high-carbon alcohol compound is C6-C12 alcohol, more preferably the high-carbon alcohol compound is secondary
Octanol, isooctanol, n-octyl alcohol, n-heptanol are one or more.The aminated compounds is primary amine RNH2, secondary amine R2NH, tertiary amine R3N
In it is one or more.
It is above-mentioned using extraction from salt lake bittern extract lithium method in, the neutrality phosphorus oxygen class compound A with mutually adjust
Contents (percentage by volume V%) of the agent B in extractant and diluent mixture is saved between 30% to 80%, wherein described
Contents of the neutral phosphorus oxygen class compound A in extractant and diluent mixture is 10%~40%.
Wherein, the relative volume of the neutrality phosphorus oxygen class compound A and two kinds of extractants of phase modifier B than ranging from 1:
30 to 30:1.
Wherein, the diluent is aliphatic hydrocarbon or aromatic hydrocarbon.Preferably, the diluent is sulfonated kerosene.
The above-mentioned method for extracting lithium from salt lake bittern using extraction, further includes the stripping process, wherein being stripped
The hydrochloric acid of 1~6mol/l is used to be stripped in the process.
The regenerative process is organic after being stripped with alkali or alkaline earth metal chloride brine hydrochloric acid, makes HFeCl4Turn
Turn to NaFeCl4、Mg(FeCl4)2Deng the ability for making extractant restore extraction lithium.Compared to the prior art, acquirement of the invention
Following unexpected technique effect：
1) the phase modifier B of protonation reaction can occur with neutral phosphorus oxygen class compound A by being introduced into extraction system,
Split-phase effect of the neutral phosphorus oxygen class compound extraction titanium tetrachloride complex compound in sulfonated kerosene diluent, split-phase can be significantly improved
Speed is fast, and extraction system has a certain range of acidity self-adjusting ability after extracting a certain amount of hydrochloric acid, is conducive to control extraction
The hydrolysis of iron in whole process, cyclic process are smooth.
2) extraction system proposed by the present invention has advanced optimized the regenerated extraction of extraction-back extraction-and has proposed lithium technological process,
Reduce the dosage of neutral phosphorus oxygen class compound, in organic phase regenerative process using alkali or alkaline earth metal chloride salting liquid without
It needs to use alkali, so that solubility and chemistry drop in the corrosivity of neutral phosphorus oxygen class compound, water in existing extraction process
Solution effect is significantly alleviated, while whole process does not use alkali, reduces extraction process expense and reduces the corrosion to equipment.This
Inventive method is low for equipment requirements, organic compound used is cheap and easy to get, is suitable for commercial Application.
Description of the drawings
Fig. 1 is the flow diagram that the embodiment of the present invention extracts lithium using extraction from salt lake bittern.
Specific implementation mode
The present invention is described in detail below by way of specific and infinite embodiment, so that advantages and features of the invention energy
It is easier to be readily appreciated by one skilled in the art.
Fig. 1 is the flow diagram that the embodiment of the present invention extracts lithium using extraction from salt lake bittern.It can be seen by Fig. 1
Go out, the flow of the extraction lithium includes：Preparing blank organic phase -- organic phase load titanium tetrachloride complex compound and hydrochloric acid -- has
Machine mutually makes the transition --- extraction section-extraction section washing is extracted to obtain, it is described
Following embodiment is all made of technique as shown in Figure 1.
The composition of 1 certain salt lake brine with high magnesium-lithium ratio of table
| Ingredient | Li+ | Mg2+ | Na+ | K+ | Cl- | B2O3 |
| Content (g/l) | 0.5~5 | 80~130 | 0~3 | 0~3 | ≥200 | 0~3 |
Embodiment 1
Neutral phosphorus oxygen class compound A selects tributyl phosphate TBP, phase modifier B to select aminated compounds tri-iso-octylamine
N235 and high-carbon alcohol compound sec-octyl alcohol, diluent select sulfonated kerosene to form extractant, and tributyl phosphate TBP is in extractant
In account for volume ratio 10%~40%.
0.1~6mol/l hydrochloric acid solutions of 1 part of extractant and 1 part of 0.1~3mol/l of ferric trichloride concentration are vibrated 10 points
Split-phase is stood after clock, obtains the load organic phases of load iron and acid；By 1 part of above-mentioned load organic phases and 4 parts of 3~6mol/l chlorinations
Calcium solution oscillation stands split-phase after ten minutes, completes load organic phases transition；By the load organic phases and 1 after 1 part of above-mentioned transition
Certain salt lake (Mg/Li=100 of brine containing lithium of ingredient shown in part table 1:1 mass ratio) oscillation extracted for 10 minutes, and oscillation terminates
After stand split-phase, measure organic phase and water phase Li after split-phase respectively+、Mg2+、Na+And K+Thus concentration calculates the extraction yield of lithium
For 78.56%, Li+、Mg2+、Na+And K+Distribution ratio is respectively 3.265,0.0085,0.0837,0.0425, Li/Mg, Li/Na and
The separation of Li/K is 384.1,39.0,76.8 respectively.
Embodiment 2
Neutral phosphorus oxygen class compound A select trioctyl phosphate TOP, phase modifier B select aminated compounds primary amine N1923 and
High-carbon alcohol compound n-heptanol, diluent select sulfonated kerosene to form extractant, and trioctyl phosphate TOP accounts for body in extractant
Product ratio 10%~40%.
By the saturation chlorination of 1 part of extractant and 1 part of 0.1~1mol/l of ferric trichloride concentration, 0.1~1mol/l of concentration of hydrochloric acid
Magnesium solution oscillation stands split-phase after ten minutes, obtains the load organic phases of load iron and acid；By 1 part of above-mentioned load organic phases and 6
Part 3~6mol/l magnesium chloride solutions oscillation stands split-phase after ten minutes, completes load organic phases transition；After 2 parts of above-mentioned transition
Load organic phases and ingredient shown in 1 part of table 1 certain salt lake (Mg/Li=50 of brine containing lithium:1 mass ratio) oscillation progress in 10 minutes
Extraction, stands split-phase, measures organic phase and water phase Li after split-phase respectively after oscillation+、Mg2+、Na+And K+Thus concentration calculates
The extraction yield for going out lithium is 90.45%, Li+、Mg2+、Na+And K+Distribution ratio is respectively 4.536,0.0096,0.0987,0.0479,
The separation of Li/Mg, Li/Na and Li/K are 472.5,45.96,94.7 respectively.
Embodiment 3
Neutral phosphorus oxygen class compound A select tributyl phosphate TBP, phase modifier B select aminated compounds primary amine N1923 and
High-carbon alcohol compound sec-octyl alcohol, diluent select sulfonated kerosene to form extractant, and tributyl phosphate TBP accounts for body in extractant
Product ratio 10%~40%.
By the saturation chlorination of 1 part of extractant and 1 part of 0.1~1mol/l of ferric trichloride concentration, 0.1~1mol/l of concentration of hydrochloric acid
Magnesium solution oscillation stands split-phase after ten minutes, obtains the load organic phases of load iron and acid；By 1 part of above-mentioned load organic phases and 6
Part 3~6mol/l magnesium chloride solutions oscillation stands split-phase after ten minutes, completes load organic phases transition；After 2 parts of above-mentioned transition
Load organic phases and ingredient shown in 1 part of table 1 certain salt lake (Mg/Li=50 of brine containing lithium:1 mass ratio) carry out three stage countercurrent extractions
It takes, balance back loading organic phase Li+、Mg2+、Na+And K+Concentration (g/l) is 1.287,0.203,0.075,0.008 respectively；By 30
The aqueous solution of the above-mentioned extraction lithium organic phase of part and 1 part of 0.1~3mol/l of chlorination lithium concentration, 0.1~3mol/l of concentration of hydrochloric acid are washed
It washs, back loading organic phase Li is balanced after washing+、Mg2+、Na+And K+Concentration (g/l) is 1.178 respectively, 0.002,0.018,
0.002。
Embodiment 4
Neutral phosphorus oxygen class compound A select tributyl phosphate TBP, phase modifier B select aminated compounds primary amine N1923 and
High-carbon alcohol compound sec-octyl alcohol, diluent select sulfonated kerosene to form extractant, and tributyl phosphate TBP accounts for body in extractant
Product ratio 10%~40%.
It is suitble to the extraction system of commercial Application, do not require nothing more than has good extraction ability and selectivity to object ion,
And to there is good back extraction performance, organic phase to be easy to regeneration and permanent stable circulation, " 10%~40%TBP- is enumerated thus
" extraction-back extraction-is again for -30%~80% sulfonated kerosene of -0%~30% sec-octyl alcohol of 0%~30% primary amine N1923 " extraction system
Life " carries the example of lithium from salt lake bittern.
Organic extractant phase carries lithium and operates with embodiment 3, after extraction carries lithium, a concentration of 1.287g/l of organic phase Li, and raffinate
Water phase Fe concentration≤1mg/l；1 part of 6mol/l hydrochloric acid (comparing O/A=20), oscillation 10 is added in the organic phase for taking 20 parts of extraction lithiums
Minute is stripped, and split-phase is stood after oscillation, measures organic phase Li after split-phase respectively+A concentration of 0.034g/l, water phase Li+
The back extraction ratio of a concentration of 25.12g/l, lithium are 97.6%, strip aqueous Fe concentration≤30mg/l；Take having after 1 part of hydrochloric acid back extraction
The magnesium chloride solution of 6 parts of 3~6mol/l is added in machine phase, vibrates 10 minutes and carries out organic phase regeneration, stands and divides after oscillation
Phase measures water phase Fe concentration≤1mg/l, and the organic phase after regeneration returns to extraction and carries lithium, after extraction carries lithium, organic phase Li concentration
For 1.284g/l.
By back extraction and organic phase regeneration cycle data as it can be seen that " sec-octyl alcohols of 10%~40%TBP-10%~30% -30%~
80% sulfonated kerosene " extraction system back extraction ratio is high, and organic phase regeneration is easy, and organic extractant phase capacity is substantially unattenuated after regeneration,
Using big compared to the rich lithium strip liquor lithium concentration height obtained after back extraction, be conducive to obtain lithium chloride or lithium carbonate using conventional method
Product.
Claims (10)
1. a kind of method for extracting lithium from salt lake bittern using extraction uses co-extraction agent FeCl3, extractant and diluent
Carrying out the extraction of lithium, which is characterized in that the extractant is the mixture of neutral phosphorus oxygen class compound A and phase modifier B, wherein
The phase modifier B is to extract the organic compound that protonation reaction can occur in reaction process with neutral phosphorus oxygen class compound A,
Extracted species group after the extractant extraction lithium becomes xLiFeCl4YHClaAbB, extractant extract lithium after through back extraction-regeneration
Process can return to extraction and carry lithium；The method for extracting lithium from salt lake bittern using extraction specifically includes following step：
1) blank organic phase is prepared：Dilution dilution agent, control are used after neutral phosphorus oxygen class compound A and phase modifier B are mixed
Neutral phosphorus oxygen class compound ratio in blank organic phase is 10%~40%；
2) prepared by load organic phases：Organic phase load titanium tetrachloride complex compound and hydrochloric acid：By above-mentioned blank organic phase and include 0.1
The solution of~1mol/L ferric trichlorides and 0.1~1mol/L hydrochloric acid is according to volume ratio 1:1 is mixed, and split-phase is stood after oscillation and is obtained
Obtain the load organic phases of load iron and acid；
3) load organic phases make the transition：Load organic phases are mixed with the chloride solution of alkali metal, split-phase is stood after oscillation, are completed
Load organic phases make the transition；
4) extraction section：Load organic phases after transition are mixed with brine containing lithium, split-phase are stood after oscillation, after measuring split-phase respectively
Organic phase and water phase Li+、Mg2+、Na+And K+Concentration calculates the separation of Li/Mg, Li/Na and Li/K, it is known that Li+It has been transferred to
In machine phase, and Mg2+、Na+And K+It is transferred in water phase, wherein Li in brine+With LiFeCl4Complex form exists；
5) washing section：It is mixed with organic using water phase, split-phase is stood after oscillation, repeatedly, by the Mg in organic phase2+、Na+
And K+It is transferred in water phase.
2. the method according to claim 1 for extracting lithium from salt lake bittern using extraction, which is characterized in that in described
Property phosphorus oxygen class compound A be tbp or the pungent fat of tricresyl phosphate one or two.
3. the method according to claim 1 for extracting lithium from salt lake bittern using extraction, which is characterized in that the phase
Conditioning agent B is itself or can carry protogenic organic compound after extracting hydrochloric acid, and the phase modifier B is high-carbon alcohols chemical combination
One kind or combinations thereof in object, aminated compounds, wherein the high-carbon alcohol compound is C6-C12 alcohol, the amine chemical combination
Object is one kind or combinations thereof in primary amine RNH2, secondary amine R2NH, tertiary amine R3N.
4. the method according to claim 3 for extracting lithium from salt lake bittern using extraction, which is characterized in that described
High-carbon alcohol compound is one kind or combinations thereof in sec-octyl alcohol, isooctanol, n-octyl alcohol, n-heptanol.
5. the method according to claim 1 for extracting lithium from salt lake bittern using extraction, which is characterized in that in described
The total content of property phosphorus oxygen class compound A and phase modifier B in organic phase is between 30% to 80%, wherein the neutral phosphor oxygen
The relative volume of class compound A and two kinds of extractants of phase modifier B than ranging from 1:30 to 30:1, the neutral phosphorus oxygen class
Contents of the compound A in extractant and diluent mixture is 10%~40%.
6. the method according to claim 1 for extracting lithium from salt lake bittern using extraction, which is characterized in that described dilute
It is aliphatic hydrocarbon or aromatic hydrocarbon to release agent.
7. the method according to claim 1 for extracting lithium from salt lake bittern using extraction, which is characterized in that described dilute
It is sulfonated kerosene to release agent.
8. the method according to claim 1 for extracting lithium from salt lake bittern using extraction, which is characterized in that described total
Extract agent FeCl3Load capacity in organic phase is 0.05mol/L to 1mol/L.
9. the method according to claim 1 for extracting lithium from salt lake bittern using extraction, which is characterized in that it is also wrapped
Stripping section and organic phase regeneration are included, wherein stripping section includes the following steps：The organic phase for taking extraction lithium, is added 1- thereto
6mol/L hydrochloric acid, oscillation stand split-phase, H after ten minutes+With HFeCl4Complex form extracts the Li into organic phase, and in organic phase+
It is counter enter water phase, wherein extraction lithium organic phase and hydrochloric acid volume ratio be 20：1；The organic phase regeneration includes the following steps：
Organic phase after taking hydrochloric acid to be stripped, is added the magnesium chloride solution of 3~6mol/L, and oscillation stands split-phase to get regeneration after ten minutes
Organic phase, regeneration organic phase, which can return to extract, carries lithium.
10. the method according to claim 1 for extracting lithium from salt lake bittern using extraction, which is characterized in that described
Back extraction system include 10%~40% tributyl phosphate, 0%~30% primary amine N1923,0%~30% sec-octyl alcohol, 30%~
80% sulfonated kerosene.
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| WO2019114817A1 (en) * | 2017-12-16 | 2019-06-20 | 虔东稀土集团股份有限公司 | Extraction solvent and method thereof for extracting and separating lithium element |
| CN108359813B (en) * | 2018-02-09 | 2019-10-01 | 陕西省膜分离技术研究院有限公司 | A kind of energy-saving and environment-friendly salt lake bittern proposes lithium technique |
| CN109825722B (en) * | 2019-02-26 | 2021-06-18 | 江西科丰锂业有限公司 | Method for extracting lithium from chloride leaching solution with high aluminum-lithium ratio |
| CN109762987B (en) * | 2019-03-06 | 2020-08-11 | 清华大学 | Dialkyl sulfone extractant and method for extracting lithium from salt lake brine |
| CN111793755A (en) * | 2020-08-03 | 2020-10-20 | 苏州增华新能源科技有限公司 | Organic phase online purification method and device in lithium extraction process of salt lake and application |
| CN112063857A (en) * | 2020-09-01 | 2020-12-11 | 长沙矿冶研究院有限责任公司 | Method for extracting lithium from brine |
| CN112853119B (en) * | 2020-12-30 | 2021-09-21 | 宿迁哈托科技有限公司 | Extraction system for extracting lithium from brine, preparation method of extraction system and method for extracting lithium from brine |
| CN113061722B (en) * | 2021-03-22 | 2022-08-09 | 湘潭大学 | Extraction method for separating calcium from low-temperature calcium-containing brine to extract lithium and application of extraction method |
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| DE112011103839B4 (en) * | 2010-11-19 | 2016-08-18 | Central South University | Process and apparatus for separating lithium from magnesium and accumulating lithium in brine |
| CN103055538B (en) * | 2012-05-24 | 2015-11-25 | 中国科学院上海有机化学研究所 | Adopt extraction from containing the method extracting lithium salts lithium bittern |
| CN104388677A (en) * | 2014-12-02 | 2015-03-04 | 中国科学院青海盐湖研究所 | Regeneration method of lithium extraction system |
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