CN109276997A - The extraction system and its extracting process of lithium isotope - Google Patents
The extraction system and its extracting process of lithium isotope Download PDFInfo
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- CN109276997A CN109276997A CN201811366945.XA CN201811366945A CN109276997A CN 109276997 A CN109276997 A CN 109276997A CN 201811366945 A CN201811366945 A CN 201811366945A CN 109276997 A CN109276997 A CN 109276997A
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Abstract
The invention discloses a kind of extraction systems of lithium isotope comprising uniformly mixed extractant, hydrophobic ionic liquid and diluent;Wherein, extractant is crown ether derivative shown in formula A or formula B.The present invention has the crown ether derivative of electron-donating group as extractant by selected side base band, cloud density therein can be improved, to enhance the effect of the ion-dipole between extractant and lithium ion, when the extractant of the class formation being thus applied to the extraction and separation of lithium isotope, especially there is better separative efficiency.The kind of extractants in use, completing back extraction after only need to carry out simple carrying out washing treatment regeneration can be realized and reuse, circulation technology also cost saved the separation costs of lithium isotope.Extraction system of the invention has many advantages, such as that green, exchange rate is fast, separative efficiency is good, is suitable for different scales and produces.The invention also discloses the lithium isotope extracting process based on above-mentioned extraction system.
Description
Technical field
The invention belongs to lithium isotope separation and concentration technology fields, it relates in particular to a kind of extractor body of lithium isotope
System and its extracting process.
Background technique
Nuclear Power Development is placed on highly important status by China, meanwhile, China is also international controlled thermonuclear fusion plan
(ITER) project is primarily involved in unit, and country successively starts correlation engineering project thus.Such as, 2002, Ministry of Nuclear Industry west
Nan Wuliyanjiuyuan builds up " No. two A of state's circulator ", pre- by carrying out the key projects technologies such as novel divertor, superconducting magnet
It grinds, ETR Engineering Test Reactor design, investigation of materials and its critical component beforehand research, provides skill for design-build deuterium tritium corrosion chamber
Art and physical basis.2006, Hefei Inst. of Plasma Physics, Chinese Academy of Sciences, which has built up in the world, while to be had complete by first
The nuclear fusion experimental device of superconducting magnet and active cooling structure.According to " controlled nuclear fusion " engineering progress, scientist is optimistically
Nuclear fusion power generation will can be achieved in estimation within 30~50 years futures.2011, China formally started " the following advanced nuclear fission-again
The relevant item of thorium base molten salt reactor nuclear power system ".Fusion reactor, the key reaction being related to be D+T →4He+n, i.e. deuterium
(D) huge energy can be released when and tritium (T) aggregates into helium (He) core.The resource of deuteron (D) on earth is extremely abundant, and
Existing amount is few in nature for another raw material tritium (T).
There are two kinds of stable isotopes in nature for lithium (Li)6Li and7Li, their natural abundance (refer to6Li and7Li's
Natural percentage contents) it is 7.42% and 92.58% respectively.Both isotopes all have of crucial importance in nuclear energy source domain
Effect.Wherein, thermal neutron absorption cross section is up to 940b's6Li can be generated after neutron (n) bombardment fission tritium and helium (6Li+n→T
+4He), so certain abundance6Li can be used as the raw material and other purposes of nuclear fusion;And thermal neutron absorption cross section is only 0.037b
's7Li has important role to the regulation of nuclear process and the maintenance of equipment.
Currently, there are many kinds of the single-stage separation methods of lithium isotope chemical method and physical method can be divided into, wherein chemical method packet
Include lithium amalgam exchange process, ion exchange chromatography, extraction etc.;Physical method includes electromagnetic method, electron transfer, molecular distillation and swashs
Light separation etc..Physical method is not suitable for being applied to because of the features such as production equipment valuableness and working condition are harsh, energy consumption is high but yield is small
Industrialized production.Lithium amalgam method separation lithium isotope haves the shortcomings that very big, and a large amount of mercury metal tapes have been used in separation process
Carry out ecological environmental and safety problems, the states such as America and Europe have been turned off some factories with lithium amalgam method separation lithium isotope.Since
Pedersen discovery crown ether compound can have complexing work with alkali metal ion according to its cavity size selectivity within 1976
It is used to, the related isotopic separation research based on crown ether mainly has solvent liquid-liquid extraction method and ion exchange chromatography.But
It is that the used extraction system based on crown ether is generally both needed to grafting phenyl or alkyl, alkoxy (the especially alkane of long-chain at present
Base, alkoxy) etc. side groups, and this grafting generally requires its corresponding crown ether and passes through with the cation on glyoxaline ion liquid
Chemical reaction is to realize.However, due to the special macrocyclic structure of crown ether, due to the steric effect of crown ether in process of grafting,
The low group of this reactivity of alkyl, alkoxy, phenyl and crown ether are difficult to carry out graft reaction, are synthetically prepared difficulty;And
Since extractant extraction efficiency is lower, the extractant of compounding high concentration is needed to can be only achieved preferable extraction effect when preparing extraction phase
Rate, it is high that whens carried out extraction and separation, will will cause cost.
During the separation and concentration of lithium isotope, lithium isotope6The every raising 0.1% of the abundance of Li is all extremely difficult
's.Such as stone Cheng Long (C.Shi et al.Journal of Molecular Liquids.2016,224:662-667) utilizes
It is extractant that dibenzo 14, which is preced with four (DB14C4), when lithium chloride (LiCl) is water phase, only can by extracting-back extraction method
It will6The relative abundance of Li is increased to 7.634% from 7.563%, only improves only 0.071%.
Summary of the invention
To solve the above-mentioned problems of the prior art, the present invention provides a kind of extraction system of lithium isotope and its extractions
Method is taken, which, as extractant, has better lithium isotope separating effect using completely new crown ether substance.
In order to achieve the above object of the invention, present invention employs the following technical solutions:
A kind of extraction system of lithium isotope, including uniformly mixed extractant, hydrophobic ionic liquid and diluent;Its
In, the extractant is crown ether derivative shown in following formula A or formula B;
Wherein, the value of n is 0,1,2;R is any in amino, hydroxyl, amide groups, ester group, bromide ion, iodide ion
It is a kind of.
Further, in the extraction system, the concentration of the extractant is 0.1mol/L~1mol/L.
Further, cation shown in hydrophobic ionic liquid anion as shown in following formula C and following formula D
Composition:
Wherein, the integer that the value of k is 1~17.
Further, in the extraction system, the ratio between volume of the hydrophobic ionic liquid and the diluent is 1
~20:2~10.
Further, the diluent be selected from methyl phenyl ethers anisole, chloroform, kerosene, methylene chloride, 1,2- dichloroethanes, n-hexane,
Normal heptane, carbon tetrachloride, tetrachloro-ethylene, toluene, dimethylbenzene, diethylbenzene, bromobenzene, any one in nitrobenzene.
The present invention also provides a kind of extracting process of lithium isotope, comprising steps of
S1, it prepares aqueous phase extracted: water-soluble lithium salts being configured to lithium salt solution, as aqueous phase extracted;
S2, extraction organic phase is prepared: using above-mentioned extraction system as extraction organic phase;
S3, extraction: the extraction organic phase and the aqueous phase extracted are sufficiently mixed according to the volume ratio of 1~5:1~10
It is extracted, obtains the extraction system that organic phase and water phase are uniformly mixed;
S4, isotope exchange: the extraction system is stood into 5min~80min, makes the lithium isotope in the organic phase7Lithium isotope in Li and the water phase6Li is sufficiently exchanged, and carries out split-phase, obtains load organic phases;
S5, back extraction: using hydrochloric acid solution as stripping agent, by the load organic phases and the stripping agent according to 1~5:1~
10 volume ratio, which is sufficiently mixed, to be stripped, and carries out split-phase, is obtained6Li pregnant solution.
Further, in the step S5, empty organic phase is also obtained after split-phase;The empty organic phase is pressed with ultrapure water
It is sufficiently mixed simultaneously regenerated from washing 1~10 time according to the volume ratio of 1~3:1~5, the regeneration organic phase of acquisition returns in the step S3
It is recycled as extraction organic phase.
Further, in the step S5, empty organic phase is also obtained after split-phase;The empty organic phase is pressed with ultrapure water
It is sufficiently mixed simultaneously regenerated from washing 1~10 time according to the volume ratio of 1~3:1~5, the regeneration organic phase of acquisition returns in the step S3
It is recycled as extraction organic phase.
Further, Li in the lithium salt solution+Concentration be 0.1mol/L~4mol/L;And/or the water-soluble lithium
Salt is selected from least one of lithium chloride, lithium bromide, lithium iodide, trifluoroacetic acid lithium, bis- (fluoroform sulphonyl) imine lithiums.
Further, the stripping agent is the hydrochloric acid solution that concentration is 0.01mol/L~4mol/L.
The present invention has the crown ether derivative of electron-donating group as extractant by selected side base band, and electricity therein can be improved
Thus sub- cloud density answers the extractant of the class formation to enhance the ion-dipole effect between extractant and lithium ion
When extraction and separation for lithium isotope, especially there is better separative efficiency;Also, the kind of extractants is in use, complete
Only needing to carry out simple carrying out washing treatment after back extraction can be realized regeneration and reuses, and it is same that circulation technology also cost saved lithium
The separation costs of position element.Extraction system of the invention is with green, exchange rate is fast, separative efficiency is good, is suitable for different scales
The advantages that production.Meanwhile the side group structure in the extractant in extraction system of the invention is also relatively simple, in being synthetically prepared
Synthesis is simple, high income, at low cost.
Specific embodiment
Hereinafter, detailed description of the present invention embodiment in future.However, it is possible to implement this hair in many different forms
It is bright, and the present invention should not be construed as limited to the specific embodiment illustrated here.On the contrary, provide these embodiments be for
Explanation the principle of the present invention and its practical application, to make others skilled in the art it will be appreciated that of the invention is various
Embodiment and the various modifications for being suitable for specific intended application.
Existing extractant preparation synthesis is difficult when based on crown ether analog derivative in the prior art as extractant, extracts
The problems such as low separation efficiency, high separation costs, present applicant proposes a kind of extraction system of completely new lithium isotope, which employs
Completely new extractant.
Specifically, which includes uniformly mixed extractant, hydrophobic ionic liquid and diluent;Wherein extract
Taking agent is crown ether derivative shown in following formula A or formula B;Wherein, extractant is crown ether derivative shown in following formula A or formula B;
Cation composition shown in hydrophobic ionic liquid anion as shown in following formula C and following formula D.
In above-mentioned formula A, the value of n is 0,1,2;R is that amino, hydroxyl, amide groups, ester group, bromide ion, iodide ion etc. supply
Electron group, especially preferably amino.
In above-mentioned formula D, integer that the value of k is 1~17.
In completely new extraction system provided by the invention, the concentration for controlling extractant is 0.1mol/L~1mol/L.
The specific structure of extractant represented by above-mentioned formula A is as shown in table 1 below.
The specific structure of the extractant shown in formula A of table 1
It is worth noting that above-mentioned hydrophobic ionic liquid is a kind of both as association's extraction in extraction system of the invention
Agent is the ionic liquid at room temperature of green solvent again.
The ratio between the volume of both the hydrophobic ionic liquid and diluent general control is 1~20:2~10, the two
Mix the dissolution solvent collectively as above-mentioned extractant.
Further, diluent is preferably methyl phenyl ethers anisole, chloroform, kerosene, methylene chloride, 1,2- dichloroethanes, n-hexane, just
Heptane, carbon tetrachloride, tetrachloro-ethylene, toluene, dimethylbenzene, diethylbenzene, bromobenzene, any one in nitrobenzene.
Based on above-mentioned completely new extraction system, the present invention also provides a kind of extracting process of lithium isotope, i.e., above-mentioned extraction
Take application of the system in extraction lithium isotope.The extracting process its include the following steps:
In step sl, aqueous phase extracted is prepared.
Specifically, water-soluble lithium salts is configured to lithium salt solution, as aqueous phase extracted.
It is worth noting that because being only capable of quantitative determination Li for the test of lithium content at present+Total amount, i.e., can not be right6Li
With7Li is quantitative determined, and the relative amount (i.e. abundance) of the two can be only measured, therefore, in prepared lithium salt solution, Li+
Concentration for lithium isotope6The Initial abundance of Li has no too much influence, i.e., in the lithium salt solution of any concentration, generally abides by
It follows6Li and7The natural abundance of Li is distributed, i.e., and respectively 7.42% and 92.58%.But due in extraction field, extraction water
In phase by the concentration of extraction substance for extraction yield be with significant impact, and then influence separation factor, therefore, in the lithium salt solution
Li+Concentration i.e. to lithium isotope6The separating effect of Li generates large effect, predominantly lithium isotope6Li is from aqueous phase extracted
The relative quantity being transferred in extraction organic phase.Therefore, general to prepare wherein Li in extracting process of the invention+Concentration be
0.1mol/L~4mol/L, the preferably lithium salt solution of 1mol/L can meet condition;Also, water-soluble lithium salts is selected from chlorination
At least one of lithium, lithium bromide, lithium iodide, trifluoroacetic acid lithium, bis- (fluoroform sulphonyl) imine lithiums.
In step s 2, using above-mentioned extraction system as extraction organic phase.
In step s3, extraction organic phase and aqueous phase extracted are sufficiently mixed and are extracted, obtained organic phase and water phase is mixed
Close uniform extraction system.
Specifically, controlling extraction phase ratio (extraction the ratio between organic phase and the volume of aqueous phase extracted) is that 1~5:1~10 are
It can.
In step s 4, isotope exchanges: extraction system being stood 5min~80min and carries out isotope exchange, and is carried out
Split-phase obtains load organic phases.
It should be noted that during step S3 is extracted, lithium isotope6Li and lithium isotope7Li will together by
Extractant extraction in extraction system enters in organic phase, therefore, in order to further make lithium isotope6Li has more been transferred to
In machine phase, by standing the lithium isotope made in organic phase7Lithium isotope in Li and water phase6Li is sufficiently exchanged, then is divided
Phase.
In general, in order to which split-phase is rapidly completed, the system can be subjected to centrifugally operated in supercentrifuge.
In step s 5, using hydrochloric acid solution as stripping agent, load organic phases and strip liquor is sufficiently mixed and are stripped,
And split-phase is carried out, it obtains6Li pregnant solution.
Specifically, control back extraction is 1~5:1~10 compared to (the ratio between load organic phases and the volume of stripping agent).
Further, it is preferable to using the hydrochloric acid solution of 0.01mol/L~4mol/L as stripping agent.
Above-mentioned extraction-isotope exchange-back extraction operation is completed to think to complete single-stage extraction process, in order to further mention
High lithium isotope6The separation and concentration effect of Li can carry out multitple extraction operation;Obtained with upper level6Li pregnant solution is as extraction
Water intaking mutually carries out extracting-isotope exchange-back extraction operation again.
Meanwhile above-mentioned individual back extraction operation can also carry out improving back extraction ratio by being repeated as many times.
By back extraction, obtaining6Empty organic phase can be also obtained while Li pregnant solution, which is pressed with ultrapure water
It is sufficiently mixed and washs 1~10 time according to the volume ratio of 1~3:1~5, regeneration can be realized, obtain regeneration organic phase;The regeneration has
Machine can mutually be recycled using in return step S3 as extraction organic phase.
Meanwhile above-mentioned individual regenerated from washing operation can also carry out improving regeneration rate by being repeated as many times.
As a result, in extracting process of the invention, using crown ether derivative shown in formula A as extractant, extraction and separation
Lithium isotope6Li, by following three steps: i.e. extraction, isotope exchange and back extraction.And in this process, mainly same position
Element exchange link can realize isotope6The separation and concentration of Li, lithium isotope exchange reaction formula may be expressed as:
In above-mentioned formula, S and G respectively indicate lithium isotope6Li and lithium isotope7Ligand of the Li in water phase and organic phase.
Extraction yield (E%) and separation factor (α) can be calculated separately by following formula as a result:
Wherein, when separation factor α is equal to 1, then it represents that two substances cannot be separated;And α pairs of separation factor of 1 departure degree
When bigger, then it represents that two substances are readily achieved separation.
It will illustrate the method for separating and concentrating of above-mentioned lithium isotope of the invention, but ability by specific embodiment below
It is the specific example of above-mentioned method for separating and concentrating that field technique personnel, which will be appreciated that following embodiments only, and being not used in restriction, it is complete
Portion.
Embodiment 1
Extraction system provided in this embodiment is preced with pentaether (4-NH by 4- amino-benzo 152- B15C5) extractant, 1-
Double trifluoromethanesulfonimide salt ([the EMIm] [NTf of ethyl-3-methylimidazole2]) hydrophobic ionic liquid and methyl phenyl ethers anisole it is dilute
Agent is released to mix;In the extraction system, the concentration of extractant is 0.3mol/L, the body of hydrophobic ionic liquid and diluent
Product is than being 3:1.
Below using 0.7mol/L lithium chloride solution as aqueous phase extracted, the extraction system based on the present embodiment has as extraction
Machine mutually carries out specific extraction application:
In the separatory funnel of 100mL, the extraction organic phase of 20mL and the aqueous phase extracted mixing of 20mL are added with liquid-transfering gun,
30min is acutely shaken on constant temperature oscillator, obtains the extraction system that organic phase and water phase are uniformly mixed.
Extraction system 10min is stood to carry out isotope exchange, being then transferred to centrifugation 2min on supercentrifuge makes two
Mutually complete split-phase obtains load organic phases;It is 37.57% that extraction yield, which is calculated,.
Load organic phases are transferred in new container, 0.5mol/L hydrochloric acid solution 20mL is added and is once stripped, bears
It is placed on constant temperature oscillator after load organic phase and stripping agent mixing and acutely shakes 40min, high speed centrifugation is transferred to after the completion of concussion
5min is centrifuged on machine makes the complete split-phase of two-phase, collects the first strip liquor;It is added again into the first empty organic phase generated simultaneously
20mL hydrochloric acid solution carries out secondary back extraction, until costrip five times.Primary back extraction and five back extraction ratios being stripped are respectively
43.25% and 99.64%.
It is same that lithium is carried out respectively to five strip liquors of water phase generated after the water phase raffinate generated after extraction and five back extraction
The plain abundance test in position, it is 1.041 that single-stage separating factor α, which is calculated,.
Embodiment 2
Extraction system provided in this embodiment is preced with extractant, the 1- butyl -3- methyl miaow of pentaether by 4- amino-benzo 15
Double trifluoromethanesulfonimide salt ([the BMIm] [NTf of azoles2]) hydrophobic ionic liquid and the diluent of methyl phenyl ethers anisole mix;
In the extraction system, the concentration of extractant is 0.3mol/L, and the volume ratio of hydrophobic ionic liquid and diluent is 3:2.
Below using 0.7mol/L lithium chloride solution as aqueous phase extracted, the extraction system based on the present embodiment has as extraction
Machine mutually carries out specific extraction application:
In the separatory funnel of 100mL, the extraction organic phase of 20mL and the aqueous phase extracted mixing of 20mL are added with liquid-transfering gun,
30min is acutely shaken on constant temperature oscillator, obtains the extraction system that organic phase and water phase are uniformly mixed.
Extraction system 10min is stood to carry out isotope exchange, being then transferred to centrifugation 2min on supercentrifuge makes two
Mutually complete split-phase obtains load organic phases;It is 31.05% that extraction yield, which is calculated,.
Load organic phases are transferred in new container, 0.5mol/L hydrochloric acid solution 40mL is added and is once stripped, bears
It is placed on constant temperature oscillator after load organic phase and stripping agent mixing and acutely shakes 50min, high speed centrifugation is transferred to after the completion of concussion
4min is centrifuged on machine makes the complete split-phase of two-phase, collects the first strip liquor;It is added again into the first empty organic phase generated simultaneously
40mL hydrochloric acid solution carries out secondary back extraction, until costrip five times.Primary back extraction and five back extraction ratios being stripped are respectively
48.61% and 99.79%.
It is same that lithium is carried out respectively to five strip liquors of water phase generated after the water phase raffinate generated after extraction and five back extraction
The plain abundance test in position, it is 1.040 that single-stage separating factor α, which is calculated,.
Embodiment 3
Extraction system provided in this embodiment is preced with the extractant of pentaether (4-Br-B15C5), 1- second by the bromo- benzo 15 of 4-
The hydrophobic ionic liquid of the double trifluoromethanesulfonimide salt of base -3- methylimidazole and the diluent of methyl phenyl ethers anisole mix;?
In the extraction system, the concentration of extractant is 0.5mol/L, and the volume ratio of hydrophobic ionic liquid and diluent is 5:2.
Below using 2mol/L trifluoroacetic acid lithium solution as aqueous phase extracted, the extraction system based on the present embodiment is as extraction
Organic phase carries out specific extraction application:
In the separatory funnel of 100mL, the extraction organic phase of 20mL and the aqueous phase extracted mixing of 20mL are added with liquid-transfering gun,
40min is acutely shaken on constant temperature oscillator, obtains the extraction system that organic phase and water phase are uniformly mixed.
Extraction system 30min is stood to carry out isotope exchange, being then transferred to centrifugation 3min on supercentrifuge makes two
Mutually complete split-phase obtains load organic phases;It is 23.85% that extraction yield, which is calculated,.
Load organic phases are transferred in new container, 0.3mol/L hydrochloric acid solution 20mL is added and is once stripped, bears
It is placed on constant temperature oscillator after load organic phase and stripping agent mixing and acutely shakes 35min, high speed centrifugation is transferred to after the completion of concussion
2min is centrifuged on machine makes the complete split-phase of two-phase, collects the first strip liquor;It is added again into the first empty organic phase generated simultaneously
20mL hydrochloric acid solution carries out secondary back extraction, until costrip five times.Primary back extraction and five back extraction ratios being stripped are respectively
34.66% and 99.18%.
It is same that lithium is carried out respectively to five strip liquors of water phase generated after the water phase raffinate generated after extraction and five back extraction
The plain abundance test in position, it is 1.043 that single-stage separating factor α, which is calculated,.
Embodiment 4
Extraction system provided in this embodiment is preced with extractant, the 1- butyl -3- methyl miaow of pentaether by 4- amino-benzo 15
The hydrophobic ionic liquid of the double trifluoromethanesulfonimide salt of azoles and the diluent of methyl phenyl ethers anisole mix;In the extraction system
In, the concentration of extractant is 0.7mol/L, and the volume ratio of hydrophobic ionic liquid and diluent is 2:1.
Below using 1.5mol/L lithium iodide solution as aqueous phase extracted, the extraction system based on the present embodiment has as extraction
Machine mutually carries out specific extraction application:
In the separatory funnel of 100mL, the extraction organic phase of 40mL and the aqueous phase extracted mixing of 20mL are added with liquid-transfering gun,
60min is acutely shaken on constant temperature oscillator, obtains the extraction system that organic phase and water phase are uniformly mixed.
Extraction system 30min is stood to carry out isotope exchange, being then transferred to centrifugation 5min on supercentrifuge makes two
Mutually complete split-phase obtains load organic phases;It is 39.68% that extraction yield, which is calculated,.
Load organic phases are transferred in new container, 1mol/L hydrochloric acid solution 40mL is added and is once stripped, loads
It is placed on constant temperature oscillator after organic phase and stripping agent mixing and acutely shakes 60min, supercentrifuge is transferred to after the completion of concussion
Upper centrifugation 5min makes the complete split-phase of two-phase, collects the first strip liquor;40mL is added into the first empty organic phase generated simultaneously again
Hydrochloric acid solution carries out secondary back extraction, until costrip five times.The back extraction ratio of primary back extraction and five back extraction is respectively 57.47% He
99.94%.
It is same that lithium is carried out respectively to five strip liquors of water phase generated after the water phase raffinate generated after extraction and five back extraction
The plain abundance test in position, it is 1.041 that single-stage separating factor α, which is calculated,.
Embodiment 5
Extraction system provided in this embodiment is preced with extractant, the 1- octyl -3- methylimidazole of pentaether by the bromo- benzo 15 of 4-
Double trifluoromethanesulfonimide salt ([OMIm] [NTf2]) hydrophobic ionic liquid and the diluent of methyl phenyl ethers anisole mix;?
In the extraction system, the concentration of extractant is 0.5mol/L, and the volume ratio of hydrophobic ionic liquid and diluent is 3:5.
Below using 1mol/L lithium-bromide solution as aqueous phase extracted, the extraction system based on the present embodiment is organic as extracting
Mutually carry out specific extraction application:
In the separatory funnel of 100mL, the extraction organic phase of 20mL and the aqueous phase extracted mixing of 20mL are added with liquid-transfering gun,
60min is acutely shaken on constant temperature oscillator, obtains the extraction system that organic phase and water phase are uniformly mixed.
Extraction system 30min is stood to carry out isotope exchange, being then transferred to centrifugation 5min on supercentrifuge makes two
Mutually complete split-phase obtains load organic phases;It is 33.62% that extraction yield, which is calculated,.
Load organic phases are transferred in new container, 1.5mol/L hydrochloric acid solution 20mL is added and is once stripped, bears
It is placed on constant temperature oscillator after load organic phase and stripping agent mixing and acutely shakes 60min, high speed centrifugation is transferred to after the completion of concussion
5min is centrifuged on machine makes the complete split-phase of two-phase, collects the first strip liquor;It is added again into the first empty organic phase generated simultaneously
20mL hydrochloric acid solution carries out secondary back extraction, until costrip five times.Primary back extraction and five back extraction ratios being stripped are respectively
55.47% and 99.91%.
It is same that lithium is carried out respectively to five strip liquors of water phase generated after the water phase raffinate generated after extraction and five back extraction
The plain abundance test in position, it is 1.042 that single-stage separating factor α, which is calculated,.
Embodiment 6
Extraction system provided in this embodiment is preced with extractant, the 1- butyl -3- methyl miaow of pentaether by 4- amino-benzo 15
The hydrophobic ionic liquid of the double trifluoromethanesulfonimide salt of azoles and the diluent of methyl phenyl ethers anisole mix;In the extraction system
In, the concentration of extractant is 0.6mol/L, and the volume ratio of hydrophobic ionic liquid and diluent is 4:3.
Below using 2.5mol/L trifluoroacetic acid lithium solution as aqueous phase extracted, the extraction system based on the present embodiment is as extraction
Organic phase is taken to carry out specific extraction application:
In the separatory funnel of 100mL, the extraction organic phase of 20mL and the aqueous phase extracted mixing of 20mL are added with liquid-transfering gun,
60min is acutely shaken on constant temperature oscillator, obtains the extraction system that organic phase and water phase are uniformly mixed.
Extraction system 40min is stood to carry out isotope exchange, being then transferred to centrifugation 5min on supercentrifuge makes two
Mutually complete split-phase obtains load organic phases;It is 27.79% that extraction yield, which is calculated,.
Load organic phases are transferred in new container, 0.4mol/L hydrochloric acid solution 20mL is added and is once stripped, bears
It is placed on constant temperature oscillator after load organic phase and stripping agent mixing and acutely shakes 60min, high speed centrifugation is transferred to after the completion of concussion
5min is centrifuged on machine makes the complete split-phase of two-phase, collects the first strip liquor;It is added again into the first empty organic phase generated simultaneously
20mL hydrochloric acid solution carries out secondary back extraction, until costrip five times.Primary back extraction and five back extraction ratios being stripped are respectively
30.89% and 99.37%.
It is same that lithium is carried out respectively to five strip liquors of water phase generated after the water phase raffinate generated after extraction and five back extraction
The plain abundance test in position, it is 1.042 that single-stage separating factor α, which is calculated,.
Embodiment 7
Extraction system provided in this embodiment is preced with extractant, the 1- hexyl -3- methyl miaow of pentaether by 4- amino-benzo 15
Double trifluoromethanesulfonimide salt ([the HMIm] [NTf of azoles2]) hydrophobic ionic liquid and the diluent of methyl phenyl ethers anisole mix;
In the extraction system, the concentration of extractant is 1mol/L, and the volume ratio of hydrophobic ionic liquid and diluent is 3:7.
Below using 1mol/L lithium chloride solution as aqueous phase extracted, the extraction system based on the present embodiment is organic as extracting
Mutually carry out specific extraction application:
In the separatory funnel of 100mL, the extraction organic phase of 20mL and the aqueous phase extracted mixing of 20mL are added with liquid-transfering gun,
60min is acutely shaken on constant temperature oscillator, obtains the first extraction system that organic phase and water phase are uniformly mixed.
The first extraction system 30min is stood to carry out isotope exchange, is then transferred on supercentrifuge and is centrifuged 5min
Make the complete split-phase of two-phase, obtains the first load organic phases;It is 40.53% that extraction yield, which is calculated,.
First load organic phases are transferred in new container, it is primary anti-that 0.8mol/L hydrochloric acid solution 20mL progress is added
It is placed on constant temperature oscillator after extraction, the first load organic phases and stripping agent mixing and acutely shakes 60min, be transferred to after the completion of concussion
5min is centrifuged on supercentrifuge makes the complete split-phase of two-phase, collects the first strip liquor;Again toward the first empty organic phase generated simultaneously
Middle addition 20mL hydrochloric acid solution carries out secondary back extraction, until costrip five times.The back extraction ratio difference of primary back extraction and five back extraction
For 47.59% and 99.68%.
To the five strip liquor difference of water phase generated after the first raffinate of water phase generated after single extraction and five back extraction
The test of lithium isotope abundance is carried out, it is 1.041 that single-stage separating factor α, which is calculated,.
It has the 20mL after back extraction first in vain machine to be mutually transferred in new separatory funnel, 40mL ultrapure water is added, in constant temperature
10min is acutely shaken on oscillator, centrifugation 1min on supercentrifuge is transferred to after the completion of concussion makes the complete split-phase of two-phase;It is past again
40mL ultrapure water is added in the second empty organic phase after split-phase and carries out regenerated from washing, washes repeatedly four times, obtains regeneration organic phase.
Regeneration organic phase is transferred in 100mL separatory funnel, the aqueous phase extracted of 20mL is added, it is acute on constant temperature oscillator
Violent shock swings 60min, obtains the second extraction system that organic phase and water phase are uniformly mixed.
The second extraction system 30min is stood to carry out isotope exchange, is then transferred on supercentrifuge and is centrifuged 5min
Make the complete split-phase of two-phase, obtains the second load organic phases;It is 42.27% that extraction yield, which is calculated,.
Second load organic phases are transferred in new container, it is primary anti-that 0.8mol/L hydrochloric acid solution 20mL progress is added
It is placed on constant temperature oscillator after extraction, the second load organic phases and stripping agent mixing and acutely shakes 60min, be transferred to after the completion of concussion
5min is centrifuged on supercentrifuge makes the complete split-phase of two-phase, collects the first strip liquor;Again toward the first empty organic phase generated simultaneously
Middle addition 20mL hydrochloric acid solution carries out secondary back extraction, until costrip five times.The back extraction ratio difference of primary back extraction and five back extraction
For 46.60% and 99.67%.
Five strip liquors of water phase generated to the second raffinate of water phase after reextraction and after being stripped for five times carry out respectively
The test of lithium isotope abundance, it is 1.041 that single-stage separating factor α, which is calculated,.
As a result, by after single extraction empty organic phase carry out regenerated from washing operation, it is seen then that its in reextraction again
Extraction ability is restored, in reextraction, extraction efficiency does not decline completely.
Embodiment 8
Extraction system provided in this embodiment is preced with extractant, the 1- octyl -3- methyl miaow of pentaether by 4- amino-benzo 15
The hydrophobic ionic liquid of the double trifluoromethanesulfonimide salt of azoles and the diluent of methyl phenyl ethers anisole mix;In the extraction system
In, the concentration of extractant is 0.4mol/L, and the volume ratio of hydrophobic ionic liquid and diluent is 2:8.
Below using 1mol/L lithium chloride solution as aqueous phase extracted, the extraction system based on the present embodiment is organic as extracting
Mutually carry out specific extraction application:
In the separatory funnel of 100mL, the extraction organic phase of 20mL and the aqueous phase extracted mixing of 20mL are added with liquid-transfering gun,
60min is acutely shaken on constant temperature oscillator, obtains the first extraction system that organic phase and water phase are uniformly mixed.
The first extraction system 10min is stood to carry out isotope exchange, is then transferred on supercentrifuge and is centrifuged 5min
Make the complete split-phase of two-phase, obtains the first load organic phases;It is 26.71% that extraction yield, which is calculated,.
First load organic phases are transferred in new container, 2mol/L hydrochloric acid solution 20mL are added and is once stripped,
It is placed on constant temperature oscillator after first load organic phases and stripping agent mixing and acutely shakes 60min, height is transferred to after the completion of concussion
5min is centrifuged on fast centrifuge makes the complete split-phase of two-phase, collects the first strip liquor;Again into the first empty organic phase generated simultaneously
20mL hydrochloric acid solution is added and carries out secondary back extraction, until costrip five times.Primary back extraction and five back extraction ratios being stripped are respectively
58.44% and 99.94%.
To the five strip liquor difference of water phase generated after the first raffinate of water phase generated after single extraction and five back extraction
The test of lithium isotope abundance is carried out, it is 1.040 that single-stage separating factor α, which is calculated,.
It has the 20mL after back extraction first in vain machine to be mutually transferred in new separatory funnel, 20mL ultrapure water is added, in constant temperature
7min is acutely shaken on oscillator, centrifugation 1min on supercentrifuge is transferred to after the completion of concussion makes the complete split-phase of two-phase;It is past again
20mL ultrapure water is added in the second empty organic phase after split-phase and carries out regenerated from washing, repeated washing three times, obtains regeneration organic phase.
Regeneration organic phase is transferred in 100mL separatory funnel, the aqueous phase extracted of 20mL is added, it is acute on constant temperature oscillator
Violent shock swings 60min, obtains the second extraction system that organic phase and water phase are uniformly mixed.
The second extraction system 10min is stood to carry out isotope exchange, is then transferred on supercentrifuge and is centrifuged 5min
Make the complete split-phase of two-phase, obtains the second load organic phases;It is 26.47% that extraction yield, which is calculated,.
Second load organic phases are transferred in new container, 2mol/L hydrochloric acid solution 20mL are added and is once stripped,
It is placed on constant temperature oscillator after second load organic phases and stripping agent mixing and acutely shakes 60min, height is transferred to after the completion of concussion
5min is centrifuged on fast centrifuge makes the complete split-phase of two-phase, collects the first strip liquor;Again into the first empty organic phase generated simultaneously
20mL hydrochloric acid solution is added and carries out secondary back extraction, until costrip five times.Primary back extraction and five back extraction ratios being stripped are respectively
58.17% and 99.89%.
Five strip liquors of water phase generated to the second raffinate of water phase after reextraction and after being stripped for five times carry out respectively
The test of lithium isotope abundance, it is 1.040 that single-stage separating factor α, which is calculated,.
As a result, by after single extraction empty organic phase carry out regenerated from washing operation, it is seen then that its in reextraction again
Extraction ability is restored, in reextraction, extraction efficiency does not decline completely.
Embodiment 9
Extraction system provided in this embodiment is preced with extractant, the 1- hexyl -3- methyl miaow of pentaether by 4- amino-benzo 15
The hydrophobic ionic liquid of the double trifluoromethanesulfonimide salt of azoles and the diluent of methyl phenyl ethers anisole mix;In the extraction system
In, the concentration of extractant is 0.1mol/L, and the volume ratio of hydrophobic ionic liquid and diluent is 3:7.
Below using 1mol/L lithium chloride solution as aqueous phase extracted, the extraction system based on the present embodiment is organic as extracting
Mutually carry out specific extraction application:
In the separatory funnel of 100mL, the extraction organic phase of 20mL and the aqueous phase extracted mixing of 20mL are added with liquid-transfering gun,
60min is acutely shaken on constant temperature oscillator, obtains the first extraction system that organic phase and water phase are uniformly mixed.
The first extraction system 30min is stood to carry out isotope exchange, is then transferred on supercentrifuge and is centrifuged 5min
Make the complete split-phase of two-phase, obtains the first load organic phases;It is 7.87% that extraction yield, which is calculated,.
First load organic phases are transferred in new container, it is primary anti-that 0.8mol/L hydrochloric acid solution 20mL progress is added
It is placed on constant temperature oscillator after extraction, the first load organic phases and stripping agent mixing and acutely shakes 60min, be transferred to after the completion of concussion
5min is centrifuged on supercentrifuge makes the complete split-phase of two-phase, collects the first strip liquor;Again toward the first empty organic phase generated simultaneously
Middle addition 20mL hydrochloric acid solution carries out secondary back extraction, until costrip five times.The back extraction ratio difference of primary back extraction and five back extraction
For 63.13% and 99.97%.
To the five strip liquor difference of water phase generated after the first raffinate of water phase generated after single extraction and five back extraction
The test of lithium isotope abundance is carried out, it is 1.043 that single-stage separating factor α, which is calculated,.
It has the 20mL after back extraction first in vain machine to be mutually transferred in new separatory funnel, 40mL ultrapure water is added, in constant temperature
10min is acutely shaken on oscillator, centrifugation 1min on supercentrifuge is transferred to after the completion of concussion makes the complete split-phase of two-phase;It is past again
40mL ultrapure water is added in the second empty organic phase after split-phase and carries out regenerated from washing, washes repeatedly four times, obtains regeneration organic phase.
Regeneration organic phase is transferred in 100mL separatory funnel, the aqueous phase extracted of 20mL is added, it is acute on constant temperature oscillator
Violent shock swings 60min, obtains the second extraction system that organic phase and water phase are uniformly mixed.
The second extraction system 30min is stood to carry out isotope exchange, is then transferred on supercentrifuge and is centrifuged 5min
Make the complete split-phase of two-phase, obtains the second load organic phases;It is 7.87% that extraction yield, which is calculated,.
Second load organic phases are transferred in new container, it is primary anti-that 0.8mol/L hydrochloric acid solution 20mL progress is added
It is placed on constant temperature oscillator after extraction, the second load organic phases and stripping agent mixing and acutely shakes 60min, be transferred to after the completion of concussion
5min is centrifuged on supercentrifuge makes the complete split-phase of two-phase, collects the first strip liquor;Again toward the first empty organic phase generated simultaneously
Middle addition 20mL hydrochloric acid solution carries out secondary back extraction, until costrip five times.The back extraction ratio difference of primary back extraction and five back extraction
For 63.13% and 99.97%.
Five strip liquors of water phase generated to the second raffinate of water phase after reextraction and after being stripped for five times carry out respectively
The test of lithium isotope abundance, it is 1.043 that single-stage separating factor α, which is calculated,.
As a result, by after single extraction empty organic phase carry out regenerated from washing operation, it is seen then that its in reextraction again
Extraction ability is restored, in reextraction, extraction efficiency does not decline completely.
It is worth noting that isotope exchange is very crucial step, specifically in above-mentioned extracting process of the invention
Comparative example 7 and embodiment 9, it can be seen that the two is using identical extraction system composition, identical aqueous phase extracted, identical
Compare and identical extraction conditions and isotope give-and-take conditions (i.e. time of repose is identical), the difference is that only extraction
The difference in size of agent concentration;Although can be seen that under high concentration extractant, extraction yield is higher, separates under low concentration extractant
Factor is higher, this is because caused by the isotope that high concentration extractant carries out under the short period exchanges not enough thoroughly;
As a result, comparatively, the time of repose that the extraction organic phase of high concentration extractant takes more time carries out sufficient same position
Plain exchange process.
Although the present invention has shown and described referring to specific embodiment, it should be appreciated by those skilled in the art that:
In the case where not departing from the spirit and scope of the present invention being defined by the claims and their equivalents, can carry out herein form and
Various change in details.
Claims (9)
1. a kind of extraction system of lithium isotope, which is characterized in that including uniformly mixed extractant, hydrophobic ionic liquid and
Diluent;Wherein, the extractant is crown ether derivative shown in following formula A or formula B;
Wherein, the value of n is 0,1,2;Any one of R in amino, hydroxyl, amide groups, ester group, bromide ion, iodide ion.
2. extraction system according to claim 1, which is characterized in that in the extraction system, the extractant it is dense
Degree is 0.1mol/L~1mol/L.
3. extraction system according to claim 1 or 2, which is characterized in that the hydrophobic ionic liquid is by following formula C institute
Cation composition shown in the anion and following formula D shown:
Wherein, the integer that the value of k is 1~17.
4. extraction system according to claim 3, which is characterized in that in the extraction system, the Hydrophobic Ionic
The ratio between volume of liquid and the diluent is 1~20:2~10.
5. extraction system according to claim 1 or 2, which is characterized in that the diluent is selected from methyl phenyl ethers anisole, chloroform, coal
Oil, methylene chloride, 1,2- dichloroethanes, n-hexane, normal heptane, carbon tetrachloride, tetrachloro-ethylene, toluene, dimethylbenzene, diethylbenzene,
Any one in bromobenzene, nitrobenzene.
6. a kind of extracting process of lithium isotope, which is characterized in that comprising steps of
S1, it prepares aqueous phase extracted: water-soluble lithium salts being configured to lithium salt solution, as aqueous phase extracted;
S2, extraction organic phase is prepared: using any extraction system of claim 1-5 as extraction organic phase;
S3, extraction: the extraction organic phase and the aqueous phase extracted are sufficiently mixed progress according to the volume ratio of 1~5:1~10
Extraction obtains the extraction system that organic phase and water phase are uniformly mixed;
S4, isotope exchange: the extraction system is stood into 5min~80min, makes the lithium isotope in the organic phase7Li and
Lithium isotope in the water phase6Li is sufficiently exchanged, and carries out split-phase, obtains load organic phases;
S5, back extraction: using hydrochloric acid solution as stripping agent, by the load organic phases and the stripping agent according to 1~5:1~10
Volume ratio, which is sufficiently mixed, to be stripped, and carries out split-phase, is obtained6Li pregnant solution.
7. extracting process according to claim 6, which is characterized in that in the step S5, also had in vain after split-phase
Machine phase;The empty organic phase and ultrapure water are sufficiently mixed simultaneously regenerated from washing 1~10 time according to the volume ratio of 1~3:1~5, obtained
The regeneration organic phase obtained is returned in the step S3 and is recycled as extraction organic phase.
8. extracting process according to claim 6 or 7, which is characterized in that Li in the lithium salt solution+Concentration be
0.1mol/L~4mol/L;And/or the water-soluble lithium salts is selected from lithium chloride, lithium bromide, lithium iodide, trifluoroacetic acid lithium, double
At least one of (fluoroform sulphonyl) imine lithium.
9. extracting process according to claim 8, which is characterized in that the stripping agent be concentration be 0.01mol/L~
The hydrochloric acid solution of 4mol/L.
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