CN112933967A - Separation and enrichment system of lithium isotope - Google Patents
Separation and enrichment system of lithium isotope Download PDFInfo
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- CN112933967A CN112933967A CN202110115402.6A CN202110115402A CN112933967A CN 112933967 A CN112933967 A CN 112933967A CN 202110115402 A CN202110115402 A CN 202110115402A CN 112933967 A CN112933967 A CN 112933967A
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- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims abstract description 84
- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 84
- 238000000926 separation method Methods 0.000 title claims abstract description 45
- 239000012071 phase Substances 0.000 claims abstract description 131
- 238000000605 extraction Methods 0.000 claims abstract description 122
- 239000007864 aqueous solution Substances 0.000 claims abstract description 74
- 229910003002 lithium salt Inorganic materials 0.000 claims abstract description 64
- 159000000002 lithium salts Chemical class 0.000 claims abstract description 64
- 239000000243 solution Substances 0.000 claims abstract description 62
- 239000012074 organic phase Substances 0.000 claims abstract description 57
- 239000012266 salt solution Substances 0.000 claims abstract description 54
- 230000002378 acidificating effect Effects 0.000 claims abstract description 42
- 238000006243 chemical reaction Methods 0.000 claims description 14
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 12
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 12
- UBOXGVDOUJQMTN-UHFFFAOYSA-N 1,1,2-trichloroethane Chemical compound ClCC(Cl)Cl UBOXGVDOUJQMTN-UHFFFAOYSA-N 0.000 claims description 10
- VZGDMQKNWNREIO-UHFFFAOYSA-N tetrachloromethane Chemical compound ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 claims description 8
- 239000003085 diluting agent Substances 0.000 claims description 7
- 239000000126 substance Substances 0.000 claims description 7
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 claims description 6
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims description 6
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 6
- 150000001875 compounds Chemical class 0.000 claims description 6
- AMXOYNBUYSYVKV-UHFFFAOYSA-M lithium bromide Chemical compound [Li+].[Br-] AMXOYNBUYSYVKV-UHFFFAOYSA-M 0.000 claims description 6
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical compound [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 claims description 6
- IIPYXGDZVMZOAP-UHFFFAOYSA-N lithium nitrate Chemical compound [Li+].[O-][N+]([O-])=O IIPYXGDZVMZOAP-UHFFFAOYSA-N 0.000 claims description 6
- 229910017604 nitric acid Inorganic materials 0.000 claims description 6
- LQNUZADURLCDLV-UHFFFAOYSA-N nitrobenzene Chemical compound [O-][N+](=O)C1=CC=CC=C1 LQNUZADURLCDLV-UHFFFAOYSA-N 0.000 claims description 6
- HSZCZNFXUDYRKD-UHFFFAOYSA-M lithium iodide Inorganic materials [Li+].[I-] HSZCZNFXUDYRKD-UHFFFAOYSA-M 0.000 claims description 5
- WSLDOOZREJYCGB-UHFFFAOYSA-N 1,2-Dichloroethane Chemical compound ClCCCl WSLDOOZREJYCGB-UHFFFAOYSA-N 0.000 claims description 4
- 238000005119 centrifugation Methods 0.000 claims description 4
- 125000003545 alkoxy group Chemical group 0.000 claims description 3
- 125000000217 alkyl group Chemical group 0.000 claims description 3
- YCOXTKKNXUZSKD-UHFFFAOYSA-N as-o-xylenol Natural products CC1=CC=C(O)C=C1C YCOXTKKNXUZSKD-UHFFFAOYSA-N 0.000 claims description 3
- 125000004432 carbon atom Chemical group C* 0.000 claims description 3
- SNHMUERNLJLMHN-UHFFFAOYSA-N iodobenzene Chemical compound IC1=CC=CC=C1 SNHMUERNLJLMHN-UHFFFAOYSA-N 0.000 claims description 3
- XIXADJRWDQXREU-UHFFFAOYSA-M lithium acetate Chemical compound [Li+].CC([O-])=O XIXADJRWDQXREU-UHFFFAOYSA-M 0.000 claims description 3
- MHCFAGZWMAWTNR-UHFFFAOYSA-M lithium perchlorate Chemical compound [Li+].[O-]Cl(=O)(=O)=O MHCFAGZWMAWTNR-UHFFFAOYSA-M 0.000 claims description 3
- 229910001486 lithium perchlorate Inorganic materials 0.000 claims description 3
- 125000000449 nitro group Chemical group [O-][N+](*)=O 0.000 claims description 3
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 claims description 3
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 claims description 3
- 239000011780 sodium chloride Substances 0.000 claims description 3
- 238000001556 precipitation Methods 0.000 claims 2
- ZXMGHDIOOHOAAE-UHFFFAOYSA-N 1,1,1-trifluoro-n-(trifluoromethylsulfonyl)methanesulfonamide Chemical compound FC(F)(F)S(=O)(=O)NS(=O)(=O)C(F)(F)F ZXMGHDIOOHOAAE-UHFFFAOYSA-N 0.000 claims 1
- 230000003534 oscillatory effect Effects 0.000 claims 1
- 230000000717 retained effect Effects 0.000 abstract description 4
- 239000011521 glass Substances 0.000 description 33
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 25
- 239000007788 liquid Substances 0.000 description 19
- 238000000034 method Methods 0.000 description 19
- 238000005086 pumping Methods 0.000 description 14
- 230000008569 process Effects 0.000 description 11
- 238000012360 testing method Methods 0.000 description 10
- 238000002156 mixing Methods 0.000 description 9
- 230000010355 oscillation Effects 0.000 description 9
- 230000002776 aggregation Effects 0.000 description 7
- 238000004220 aggregation Methods 0.000 description 7
- 229910000497 Amalgam Inorganic materials 0.000 description 4
- YZCKVEUIGOORGS-NJFSPNSNSA-N Tritium Chemical compound [3H] YZCKVEUIGOORGS-NJFSPNSNSA-N 0.000 description 4
- 229910052722 tritium Inorganic materials 0.000 description 4
- 238000009825 accumulation Methods 0.000 description 3
- 150000003983 crown ethers Chemical class 0.000 description 3
- 230000004927 fusion Effects 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000000053 physical method Methods 0.000 description 3
- VFTFKUDGYRBSAL-UHFFFAOYSA-N 15-crown-5 Chemical compound C1COCCOCCOCCOCCO1 VFTFKUDGYRBSAL-UHFFFAOYSA-N 0.000 description 2
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- FNEPSTUXZLEUCK-UHFFFAOYSA-N benzo-15-crown-5 Chemical compound O1CCOCCOCCOCCOC2=CC=CC=C21 FNEPSTUXZLEUCK-UHFFFAOYSA-N 0.000 description 2
- QSBFECWPKSRWNM-UHFFFAOYSA-N dibenzo-15-crown-5 Chemical compound O1CCOCCOC2=CC=CC=C2OCCOC2=CC=CC=C21 QSBFECWPKSRWNM-UHFFFAOYSA-N 0.000 description 2
- 229910052734 helium Inorganic materials 0.000 description 2
- 239000001307 helium Substances 0.000 description 2
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 2
- 238000005372 isotope separation Methods 0.000 description 2
- 229910001416 lithium ion Inorganic materials 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- XQQZRZQVBFHBHL-UHFFFAOYSA-N 12-crown-4 Chemical compound C1COCCOCCOCCO1 XQQZRZQVBFHBHL-UHFFFAOYSA-N 0.000 description 1
- XIWRBQVYCZCEPG-UHFFFAOYSA-N 17-nitro-2,5,8,11,14-pentaoxabicyclo[13.4.0]nonadeca-1(15),16,18-triene Chemical compound O1CCOCCOCCOCCOC2=CC([N+](=O)[O-])=CC=C21 XIWRBQVYCZCEPG-UHFFFAOYSA-N 0.000 description 1
- YZCKVEUIGOORGS-OUBTZVSYSA-N Deuterium Chemical compound [2H] YZCKVEUIGOORGS-OUBTZVSYSA-N 0.000 description 1
- 229910013553 LiNO Inorganic materials 0.000 description 1
- 239000003929 acidic solution Substances 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- -1 crown ether compounds Chemical class 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 229910052805 deuterium Inorganic materials 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000004992 fission Effects 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 238000009616 inductively coupled plasma Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000004255 ion exchange chromatography Methods 0.000 description 1
- 230000005445 isotope effect Effects 0.000 description 1
- 230000000155 isotopic effect Effects 0.000 description 1
- 238000000622 liquid--liquid extraction Methods 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000000199 molecular distillation Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000027756 respiratory electron transport chain Effects 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
Images
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D59/00—Separation of different isotopes of the same chemical element
- B01D59/22—Separation by extracting
- B01D59/24—Separation by extracting by solvent extraction
-
- 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
Abstract
The invention discloses a separation and enrichment system of lithium isotopes, which comprises an organic extraction phase, a lithium salt solution phase, a stripping solution and a tube body filled with a low-concentration acidic aqueous solution; wherein the organic extraction phase is used for reacting with the lithium salt solution phase to obtain a first enriched organic phase; the pipe filled with the low-concentration acidic aqueous solution is used for eluting the first enriched organic phase to form a second enriched organic phase; the back extraction solution is used for back extraction of the first solution to obtain enriched6A solution of Li. The separation and enrichment system of the lithium isotope provided by the invention elutes the first enriched organic phase by arranging the pipe body filled with the low-concentration acidic aqueous solution, and the organic phase contains7Li is more eluted into the aqueous solution,6the proportion of Li retained in the organic phase is greater, thus allowing the resulting second enriched organic phase6The abundance of Li is improved.
Description
Technical Field
The invention belongs to the technical field of lithium isotope separation, and particularly relates to a separation and enrichment system for lithium isotopes.
Background
Lithium (Li) exists in nature in two stable isotopes6Li and7li, their natural abundance (meaning)6Li and7the natural relative percentage of Li) is 7.42% and 92.58%, respectively, both isotopes having extremely important roles in the nuclear energy field. Wherein the thermal neutron absorption cross section reaches 940b6The Li is bombarded by neutrons (n) to fission to generate tritium and helium6Li+n→T+4He) so as to be of a certain abundance6Li can be used as a raw material for nuclear fusion and other uses; while the thermal neutron absorption cross section is only 0.037b7Li plays an important role in the regulation of the nuclear reaction process and the maintenance of equipment. The nuclear fusion energy supply is to polymerize deuterium (D) and tritium (T) into helium (4He) of 1kg, estimated6The total energy released during the fusion can generate at least 10000 kilowatts which are far larger than the same mass235Energy released when U fissures. However, the storage of tritium in nature is extremely limited and tritium production must rely on neutron bombardment6Li is generated and added.
At present, single-stage separation methods of lithium isotopes are various and can be divided into chemical methods and physical methods, wherein the chemical methods comprise a lithium amalgam exchange method, an ion exchange chromatography method, an extraction method and the like; physical methods include electromagnetic methods, electron transfer, molecular distillation, laser separation, and the like. The physical method is not suitable for industrial production due to the characteristics of expensive production equipment, harsh production conditions, high energy consumption, small yield and the like. The separation of lithium isotopes by the lithium amalgam method has the great disadvantages that a large amount of mercury metal is brought to ecological environment and safety problems in the separation process, and some factories for separating lithium isotopes by the lithium amalgam method are closed in European and American countries.
Since a series of crown ether compounds are synthesized by Pedersen and the like in 1967, researchers find that certain crown ethers have huge lithium isotope effect and separation factors which are comparable with lithium amalgam in the aspect of separating lithium isotopes, but in the separation and enrichment process of liquid-liquid extraction of lithium isotopes by a crown ether solvent,6it is very difficult to increase the abundance of Li by every 0.1%.
Disclosure of Invention
In view of the defects of the prior art, the invention provides a separation and enrichment system of lithium isotopes, which is used for improving6Separation-enriched abundance of Li.
A separation and enrichment system of lithium isotopes comprises an organic extraction phase, a lithium salt solution phase, a stripping solution and a tube body filled with a low-concentration acidic aqueous solution; wherein the content of the first and second substances,
the organic extraction phase is used for reacting with the lithium salt solution phase to obtain a first enriched organic phase;
the tube filled with the low-concentration acidic aqueous solution is used for eluting the first enriched organic phase, and comprises: (ii) injecting the first enriched organic phase dropwise into the tube filled with the low-concentration acidic aqueous solution, the first enriched organic phase accumulating at the bottom of the tube to form a second enriched organic phase;
the back extraction solution is used for back extraction of the first solution to obtain enriched6A solution of Li.
Preferably, the organic extract phase comprises an extractant and a diluent mixed with each other; wherein the content of the first and second substances,
the extractant is selected from any one of compounds shown in the following formulas 1 to 3,
in the compounds shown in the formulas 1 to 3, R is selected from alkyl, alkoxy, amino, nitro or phenyl with 0-20 carbon atoms, X is N or O, and N is 0, 1 or 2;
the diluent is selected from one or more than two of iodobenzene, dichloromethane, carbon tetrachloride, chloroform, 1, 2-dichloroethane, nitrobenzene or 1,1, 2-trichloroethane.
Preferably, the concentration of the extractant in the organic extraction phase is 0.4 mol/L-0.8 mol/L.
Preferably, the lithium salt in the lithium salt solution phase is selected from the group consisting of LiCl, LiBr, LiI, LiOH, LiNO3、LiClO4、LiSCN、CH3COOLi、CF3COOLi、CHF2COOLi、CH2FCOOLi and Li [ NTf ]2]And the concentration of the lithium salt in the lithium salt solution is 1-4 mol/L.
Preferably, the organic extraction phase and the lithium salt solution phase are mixed according to the volume ratio of 1 (1-10) to carry out a shaking extraction reaction, so as to obtain the first organic-rich phase.
Preferably, the strip liquor is selected from HCl, HBr, HI, NaCl, KCl, H2SO4、HNO3And HClO4The concentration of the stripping solution is 1 mol/L-5 mol/L.
Preferably, the low-concentration acidic aqueous solution is HCl, HBr, HI, H2SO4、HNO3And HClO4The concentration of the solute in the low-concentration acidic aqueous solution is 0.1 to 1 mol/L.
Preferably, the concentration of the solute in the low-concentration acidic aqueous solution is 0.2mol/L to 0.8 mol/L.
Preferably, the second organic rich phase is withdrawn from the tube and the aqueous solution therein is removed by centrifugation.
Preferably, the height of the pipe filled with the low-concentration acidic aqueous solution is 0.5-2 m.
According to the separation and enrichment system of the lithium isotope, provided by the embodiment of the invention, the first enriched organic phase is eluted by arranging the pipe body filled with the low-concentration acidic aqueous solution, and the organic phase is separated from the first enriched organic phase7Li is more eluted into the aqueous solution,6the proportion of Li retained in the organic phase is greater, and the content of Li in the organic phase is increased6Separation and enrichment abundance of Li; in addition, the organic extraction phase is made into organic small drops to be contacted with the low-concentration acidic aqueous solution, so that the contact area is increased, and the reaction time is saved.
Drawings
FIG. 1 is a schematic structural view of a pipe filled with a low-concentration acidic aqueous solution according to an embodiment of the present invention;
fig. 2 is a process flow chart of a method for separating and enriching lithium isotopes in the embodiment of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, embodiments of the present invention are described in detail below with reference to the accompanying drawings. Examples of these preferred embodiments are illustrated in the accompanying drawings. The embodiments of the invention shown in the drawings and described in accordance with the drawings are exemplary only, and the invention is not limited to these embodiments.
It should be noted that, in order to avoid obscuring the present invention with unnecessary details, only the structures and/or processing steps closely related to the scheme according to the present invention are shown in the drawings, and other details not so relevant to the present invention are omitted.
The abundance of lithium isotope refers to the content ratio of one isotope of lithium in the total lithium element, and the increased lithium isotope abundance refers to the increased percentage of one isotope of lithium after isotope separation and enrichment compared with that before enrichment, and the percentage is6Abundance of Li: (6Li%) and increased abundance (. DELTA.h) ((L) ()6Li%)) can be expressed as: Δ h: (6Li%)=h2(6Li%)-h1(6Li%); wherein, Δ h: (6Li%) means increased isotopic abundance of lithium, h1(6Li%) means separationAbundance of lithium isotope before enrichment, h2(6Li%) refers to the abundance of the lithium isotope after separation and enrichment.
It should be noted that the abundance before and after separation is calculated after one thousandth deviation of the lithium isotope is tested by using an inductively coupled plasma mass spectrometer, and the calculation formula is as follows:in the formula:7Li/6LiSVEC12.177, standard lithium used by test unit7Li and6abundance ratio of Li; delta7/6Li (‰) is the relative one thousandth deviation, given directly by the test instrument. Thus, two quantities are known from the three quantities in the above equation (7Li/6LiSVECAnd delta7/6Li (mill)) to calculate the value of the sample7Li/6LiSample (I)The numerical value of (c).
Because the total content of the two isotopes of lithium is 100 percent6The abundance of Li is x, then7The abundance of Li is 1-x, then:7Li/6Lisample (I)(1-x)/x, to give it6Specific values of the abundance x of Li.
The embodiment of the invention provides a separation and enrichment system of lithium isotopes, which comprises an organic extraction phase, a lithium salt solution phase, a stripping solution and a tube body filled with a low-concentration acidic aqueous solution; wherein the organic extraction phase is used for reacting with the lithium salt solution phase to obtain a first enriched organic phase; the tube filled with the low-concentration acidic aqueous solution is used for eluting the first enriched organic phase, and comprises: (ii) injecting the first enriched organic phase dropwise into the tube filled with the low-concentration acidic aqueous solution, the first enriched organic phase accumulating at the bottom of the tube to form a second enriched organic phase; the back extraction solution is used for back extraction of the first solution to obtain enriched6A solution of Li.
Wherein the organic extract phase comprises an extractant and a diluent mixed with each other.
Specifically, the extractant is selected from any one of the compounds shown in the following formulas 1 to 3,
in the compounds shown in the formulas 1 to 3, R is selected from alkyl, alkoxy, amino, nitro or phenyl with 0-20 carbon atoms, X is N or O, and N is 0, 1 or 2.
Specifically, the diluent is selected from one or more than two of iodobenzene, dichloromethane, carbon tetrachloride, chloroform, 1, 2-dichloroethane, nitrobenzene or 1,1, 2-trichloroethane.
In a preferable scheme, the concentration of the extractant in the organic extraction phase is 0.4 mol/L-0.8 mol/L.
Wherein the lithium salt in the lithium salt solution phase is selected from LiCl, LiBr, LiI, LiOH and LiNO3、LiClO4、LiSCN、CH3COOLi、CF3COOLi、CHF2COOLi、CH2FCOOLi and Li [ NTf ]2]One or more than two of them.
In a preferred embodiment, the concentration of the lithium salt in the lithium salt solution is 1mol/L to 4 mol/L.
Wherein, referring to fig. 1, the tube 1 filled with the low-concentration acidic aqueous solution is, for example, a glass tube, and comprises a liquid inlet 11 at the top and a water stop valve 12 and a liquid outlet 13 at the bottom, after the low-concentration acidic aqueous solution 2 is filled into the tube 1, the first organic phase rich is injected dropwise into the tube 1 filled with the low-concentration acidic aqueous solution 2 through the injector 3, and the organic phase droplets 4 sink in the low-concentration acidic aqueous solution 2 under the action of their own gravity and gather at the bottom of the tube, thereby gathering to obtain the second organic phase rich 5. After completion of the accumulation, the stop valve 12 can be opened to remove the second organic phase enriched 5.
The height of the tubular body 1 (i.e., the height at which the droplets of the first organic-phase-rich phase fall freely in the low-concentration acidic aqueous solution) is preferably 0.5m or more, more preferably 0.5m to 2m, and still more preferably 0.5m to 1 m.
Wherein the low-concentration acidic aqueous solution is HCl, HBr, HI and H2SO4、HNO3And HClO4An aqueous solution of one or more than two of the above substances. Further preferably, the concentration of the solute in the low-concentration acidic aqueous solution is 0.1mol/L to 1 mol/L. In a more preferred embodiment, the concentration of the solute in the low-concentration acidic aqueous solution is 0.2mol/L to 0.8 mol/L.
Wherein the stripping solution is selected from HCl, HBr, HI, NaCl, KCl and H2SO4、HNO3And HClO4One or more than two of them. In a preferable scheme, the concentration of the stripping solution is 1 mol/L-5 mol/L.
With the above concept of the separation and enrichment system for lithium isotopes, referring to fig. 2, the process applied to the separation and enrichment of lithium isotopes includes the following steps:
and step S1, dissolving the extracting agent in the diluent to prepare an organic extraction phase.
As mentioned above, the concentration of the extractant in the organic extraction phase is preferably 0.4mol/L to 0.8 mol/L.
And step S2, dissolving lithium salt in water to prepare a lithium salt solution phase.
As described above, the concentration of the lithium salt in the lithium salt solution is preferably 1 to 4 mol/L.
And step S3, mixing the organic extraction phase and the lithium salt solution phase, performing oscillation extraction, and after extraction is finished, performing centrifugal separation to remove the unreacted lithium salt solution phase to obtain a first enriched organic phase.
Specifically, the organic extraction phase and the lithium salt solution phase are mixed and then placed in a centrifuge tube, and then the centrifuge tube is placed in oscillation equipment for oscillation extraction, wherein the oscillation extraction time can be 1-30 min.
In a preferable scheme, the organic extraction phase and the lithium salt solution phase are mixed according to a volume ratio of 1 (1-5) to perform extraction reaction.
Step S4, dropwise injecting the first organic phase into a pipe filled with a low-concentration acidic aqueous solution, wherein the first organic phase is gathered at the bottom of the pipe to form a second organic phase.
In a preferred embodiment, in the step S4, the second organic-rich phase is taken out from the tube and the aqueous solution therein is removed by centrifugation.
In a more preferred embodiment, the operation of accumulating the organic phase enriched at the bottom of the tube in the step S4 is repeated according to the step 4 to obtain the second organic phase enriched. Specifically, the first enriched organic phase is gradually injected into the pipe filled with the low-concentration acidic aqueous solution, so that the first enriched organic phase is accumulated at the bottom of the pipe, the accumulated enriched organic phase is taken out and then injected into the pipe filled with the low-concentration acidic aqueous solution, and after repeating the operation for multiple times, the enriched organic phase obtained by the last accumulation is the second enriched organic phase.
In the step S4, the first enriched organic phase extracted in the step S3 contains6Li and7li, the lithium ions extracted in the organic phase during their fall in an acidic aqueous solution, due to the crown ether (extractant) pair6Li and7difference in Li selectivity6Li and7li is eluted out in unequal proportions by the aqueous acidic solution, in which7The ratio of Li diffusion into the acidic aqueous solution is higher7The proportion of Li in the organic phase is larger, and6the proportion of Li retained in the organic phase is greater, thus allowing the resulting second enriched organic phase6The abundance of Li is improved. In addition, due to extraction in the organic phase6Li and7li is eluted by the acidic aqueous solution, which inevitably causes the loss of lithium, but because the lithium isotope is much more expensive than the lithium salt, it is also of great significance to increase the abundance of the lithium isotope by sacrificing a small amount of lithium resources. Therefore, the acidic aqueous solution used in the present invention is a low-concentration acidic aqueous solution, preferably having a concentration of 0.1 to 1mol/L, more preferably having a concentration of 0.1 to 1mol/L0.2mol/L to 0.8mol/L of an acidic aqueous solution, and (c) a step of adding a target lithium isotope6Li) and simultaneously minimizing the loss amount of lithium resources.
Step S5, back extraction is carried out on the second enriched organic phase by using back extraction liquid to obtain enriched organic phase6A solution of Li.
As described above, the concentration of the stripping solution is preferably 1mol/L to 5 mol/L.
Example 1
The separation and enrichment system for lithium isotopes and the process thereof applied to separation and enrichment of lithium isotopes provided by the embodiment are as follows:
(1) and dissolving an extractant 12-crown-4 (structural formula 3) in chloroform to prepare an organic extraction phase with the extractant concentration of 0.8 mol/L.
(2) LiClO is added4Dissolving in water to obtain 3mol/L lithium salt solution6The abundance of Li was 7.57%.
(3) And mixing the organic extraction phase and the lithium salt solution phase according to the volume ratio of 1: and 5, placing the lithium salt solution into a centrifugal tube, performing oscillation extraction for 30min, and centrifuging to remove the reacted lithium salt solution.
(4) Filling a glass tube with the height of 0.5 meter with 0.2mol/L of HCl aqueous solution, pumping the organic extraction phase after reaction by using an injector, injecting the organic extraction phase into the HCl aqueous solution in the form of liquid drops from the top of the glass tube, opening a water stop valve to collect the organic extraction phase after the organic extraction phase completely and freely falls to an organic extraction phase aggregation area at the bottom of the glass tube, pumping the aggregated organic extraction phase by using the injector, injecting the organic extraction phase into fresh aqueous solution in the form of liquid drops from the top of the glass tube, and repeating the steps for 5 times.
(5) Centrifuging to remove water solution in organic extraction phase, and back-extracting with 4 times volume of 1mol/L HCl solution for 3 times to obtain concentrated solution6A solution of Li back-extract.
(6) And measuring the abundance of the lithium isotope in the stripping solution, and calculating the improved abundance of the lithium isotope. The test results are as follows:6the abundance of Li is 8.40%, which is improved by 0.83% compared with the initial abundance.
Example 2
The separation and enrichment system for lithium isotopes and the process thereof applied to separation and enrichment of lithium isotopes provided by the embodiment are as follows:
(1) and dissolving an extractant 15-crown-5 (structural formula 1) in 1,1, 2-trichloroethane to prepare an organic extraction phase with the concentration of the extractant of 0.6 mol/L.
(2) And reacting Li [ NTf ]2]Dissolving in water to obtain 4mol/L lithium salt solution6The abundance of Li was 7.50%.
(3) And mixing the organic extraction phase and the lithium salt solution phase according to the volume ratio of 1: 1, placing the lithium salt solution into a centrifugal tube, oscillating and extracting for 1min, and centrifuging to remove the reacted lithium salt solution.
(4) Filling a glass tube with the height of 0.5m with 1mol/L of HCl aqueous solution, pumping the organic extraction phase after reaction by using an injector, injecting the organic extraction phase into the HCl aqueous solution in the form of liquid drops from the top of the glass tube, opening a water stop valve to collect the organic extraction phase after the organic extraction phase completely and freely falls to an organic extraction phase aggregation area at the bottom of the glass tube, pumping the aggregated organic extraction phase by using the injector, injecting the organic extraction phase into fresh aqueous solution in the form of liquid drops from the top of the glass tube, and repeating the steps for 5 times.
(5) After removing the aqueous solution in the organic extract phase by centrifugation, 1mol/L H was added in a volume 2 times that of the extract2SO4Subjecting the solution to back extraction for 3 times to obtain enriched solution6A solution of Li back-extract.
(6) And measuring the abundance of the lithium isotope in the stripping solution, and calculating the improved abundance of the lithium isotope. The test results are as follows:6the abundance of Li is 8.34%, which is improved by 0.84% compared with the initial abundance.
Example 3
The separation and enrichment system for lithium isotopes and the process thereof applied to separation and enrichment of lithium isotopes provided by the embodiment are as follows:
(1) and dissolving an extractant dibenzo 15-crown-5 (structural formula 2) in chloroform to prepare an organic extraction phase with the extractant concentration of 0.5 mol/L.
(2) And reacting Li [ NTf ]2]Dissolving in water to obtain 1mol/L lithium salt solution6The abundance of Li was 7.50%.
(3) And mixing the organic extraction phase and the lithium salt solution phase according to the volume ratio of 1: 10 placing the lithium salt solution into a centrifuge tube, oscillating and extracting for 5min, and centrifuging to remove the lithium salt solution after reaction.
(4) Filling a glass tube with the height of 0.5 meter with 0.6mol/L of HCl aqueous solution, pumping the organic extraction phase after reaction by using an injector, injecting the organic extraction phase into the HCl aqueous solution in the form of liquid drops from the top of the glass tube, opening a water stop valve to collect the organic extraction phase after the organic extraction phase completely and freely falls to an organic extraction phase aggregation area at the bottom of the glass tube, pumping the aggregated organic extraction phase by using the injector, injecting the organic extraction phase into fresh aqueous solution in the form of liquid drops from the top of the glass tube, and repeating the steps for 8 times.
(5) Centrifuging to remove water solution in organic extraction phase, and back-extracting with 2 times volume of 5mol/L HBr solution for 3 times to obtain extract rich in HBr6A solution of Li back-extract.
(6) And measuring the abundance of the lithium isotope in the stripping solution, and calculating the improved abundance of the lithium isotope. The test results are as follows:6the abundance of Li is 8.78%, which is 1.28% higher than the initial abundance.
Example 4
The separation and enrichment system for lithium isotopes and the process thereof applied to separation and enrichment of lithium isotopes provided by the embodiment are as follows:
(1) and dissolving an extractant 4 nitrobenzo 15-crown-5 (structural formula 1) in carbon tetrachloride to prepare an organic extraction phase with the concentration of the extractant of 0.6 mol/L.
(2) Dissolving LiI in water to prepare a 4mol/L lithium salt solution, and dissolving LiI in the lithium salt solution6The abundance of Li was 7.61%.
(3) And mixing the organic extraction phase and the lithium salt solution phase according to the volume ratio of 1: 4, placing the lithium salt solution into a centrifugal tube, oscillating and extracting for 20min, and centrifuging to remove the lithium salt solution after reaction.
(4) Filling a glass tube with the height of 1 meter with 0.2mol/L of HCl aqueous solution, pumping the organic extraction phase after reaction by using an injector, injecting the organic extraction phase into the HCl aqueous solution in the form of liquid drops from the top of the glass tube, opening a water stop valve to collect the organic extraction phase after the organic extraction phase completely and freely falls to an organic extraction phase aggregation area at the bottom of the glass tube, pumping the aggregated organic extraction phase by using the injector, injecting the organic extraction phase into fresh aqueous solution in the form of liquid drops from the top of the glass tube, and repeating the steps for 5 times.
(5) Centrifuging to remove water solution in organic extraction phase, and back-extracting with 3 times volume of 2mol/L HCl solution for 3 times to obtain concentrated solution6A solution of Li back-extract.
(6) And measuring the abundance of the lithium isotope in the stripping solution, and calculating the improved abundance of the lithium isotope. The test results are as follows:6the abundance of Li is 8.73%, which is improved by 1.12% compared with the initial abundance.
Example 5
The separation and enrichment system for lithium isotopes and the process thereof applied to separation and enrichment of lithium isotopes provided by the embodiment are as follows:
(1) and dissolving an extractant benzo 15-crown-5 (structural formula 1) in 1, 2-dichloroethane to prepare an organic extraction phase with the concentration of the extractant of 0.8 mol/L.
(2) And reacting LiNO with a catalyst3Dissolving in water to obtain 3mol/L lithium salt solution6The abundance of Li was 7.57%.
(3) And mixing the organic extraction phase and the lithium salt solution phase according to the volume ratio of 1: and 5, placing the lithium salt solution into a centrifugal tube, performing oscillation extraction for 30min, and centrifuging to remove the reacted lithium salt solution.
(4) Filling a glass tube with the height of 1 meter with 0.1mol/L of HCl aqueous solution, pumping the organic extraction phase after reaction by using an injector, injecting the organic extraction phase into the HCl aqueous solution in the form of liquid drops from the top of the glass tube, opening a water stop valve to collect the organic extraction phase after the organic extraction phase completely and freely falls to an organic extraction phase aggregation area at the bottom of the glass tube, pumping the aggregated organic extraction phase by using the injector, injecting the organic extraction phase into fresh aqueous solution in the form of liquid drops from the top of the glass tube, and repeating the steps for 3 times.
(5) Centrifuging to remove water solution in organic extraction phase, and back-extracting with 1mol/L HCl solution 1 times the volume of the organic extraction phase for 3 times to obtain the product rich in HCl6A solution of Li back-extract.
(6) And measuring the abundance of the lithium isotope in the stripping solution, and calculating the improved abundance of the lithium isotope. The test results are as follows:6the abundance of Li is 8.38 percent, which is improved by 0.81 percent compared with the initial abundance.
Example 6
The separation and enrichment system for lithium isotopes and the process thereof applied to separation and enrichment of lithium isotopes provided by the embodiment are as follows:
(1) and dissolving an extractant dibenzo 15-crown-5 (structural formula 2) in dichloromethane to prepare an organic extraction phase with the extractant concentration of 0.6 mol/L.
(2) And reacting Li [ NTf ]2]Dissolving in water to obtain 2mol/L lithium salt solution6The abundance of Li was 7.50%.
(3) And mixing the organic extraction phase and the lithium salt solution phase according to the volume ratio of 1: and 5, placing the lithium salt solution into a centrifugal tube, performing oscillation extraction for 2min, and centrifuging to remove the reacted lithium salt solution.
(4) Filling a glass tube with the height of 0.8 meter with 0.8mol/L of HBr aqueous solution, pumping the organic extraction phase after reaction by using an injector into the HBr aqueous solution in the form of liquid drops from the top of the glass tube, opening a water stop valve to collect the organic extraction phase after the organic extraction phase completely and freely falls to an organic extraction phase aggregation area at the bottom of the glass tube, pumping the aggregated organic extraction phase by using the injector out from the top of the glass tube and injecting the organic extraction phase into a fresh aqueous solution in the form of liquid drops, and repeating the steps for 5 times.
(5) Centrifuging to remove water solution in organic extraction phase, and back-extracting with 4 times volume of 1mol/L HCl solution for 3 times to obtain concentrated solution6A solution of Li back-extract.
(6) And measuring the abundance of the lithium isotope in the stripping solution, and calculating the improved abundance of the lithium isotope. The test results are as follows:6the abundance of Li is 8.49%, which is improved by 0.99% compared with the initial abundance.
Example 7
The separation and enrichment system for lithium isotopes and the process thereof applied to separation and enrichment of lithium isotopes provided by the embodiment are as follows:
(1) and dissolving an extractant 4 aminobenzene 15-crown-5 (structural formula 1) in chloroform to prepare an organic extraction phase with the extractant concentration of 0.4 mol/L.
(2) And reacting Li [ NTf ]2]Dissolving in water to obtain 1mol/L lithium salt solution6The abundance of Li was 7.50%.
(3) And mixing the organic extraction phase and the lithium salt solution phase according to the volume ratio of 1: and 5, placing the lithium salt solution into a centrifugal tube, performing oscillation extraction for 10min, and centrifuging to remove the reacted lithium salt solution.
(4) Filling a glass tube with the height of 1 meter with 0.4mol/L of HCl aqueous solution, pumping the organic extraction phase after reaction by using an injector, injecting the organic extraction phase into the HCl aqueous solution in the form of liquid drops from the top of the glass tube, opening a water stop valve to collect the organic extraction phase after the organic extraction phase completely and freely falls to an organic extraction phase aggregation area at the bottom of the glass tube, pumping the aggregated organic extraction phase by using the injector, injecting the organic extraction phase into fresh aqueous solution in the form of liquid drops from the top of the glass tube, and repeating the steps for 4 times.
(5) Centrifuging to remove water solution in organic extraction phase, and back-extracting with 4 times volume of 1mol/L HCl solution for 3 times to obtain concentrated solution6A solution of Li back-extract.
(6) And measuring the abundance of the lithium isotope in the stripping solution, and calculating the improved abundance of the lithium isotope. The test results are as follows:6the abundance of Li is 8.47%, which is improved by 0.97% compared with the initial abundance.
Example 8
The separation and enrichment system for lithium isotopes and the process thereof applied to separation and enrichment of lithium isotopes provided by the embodiment are as follows:
(1) and dissolving an extractant benzo 15-crown-5 (structural formula 1) in 1,1, 2-trichloroethane to prepare an organic extraction phase with the concentration of the extractant of 0.8 mol/L.
(2) And reacting Li [ NTf ]2]Dissolving in water to obtain 3mol/L lithium salt solution6The abundance of Li was 7.50%.
(3) And mixing the organic extraction phase and the lithium salt solution phase according to the volume ratio of 1: and 8, putting the lithium salt solution into a centrifugal tube, performing oscillation extraction for 5min, and centrifuging to remove the reacted lithium salt solution.
(4) 0.1mol/L of H2SO4Filling a glass tube with the height of 1m with the aqueous solution, and extracting the organic extract phase after reaction from the top of the glass tube by using an injector as liquid dropsForm of (1) implanting said H2SO4In the aqueous solution, after the organic extraction phase completely and freely falls to the organic extraction phase accumulation zone at the bottom of the glass tube, the water stop valve is opened to collect the organic extraction phase, the accumulated organic extraction phase is pumped out by an injector and injected into fresh aqueous solution in the form of liquid drops from the top of the glass tube, and the steps are repeated for 7 times.
(5) Centrifuging to remove water solution in organic extraction phase, and back-extracting with 4 times volume of 1mol/L HCl solution for 3 times to obtain concentrated solution6A solution of Li back-extract.
(6) And measuring the abundance of the lithium isotope in the stripping solution, and calculating the improved abundance of the lithium isotope. The test results are as follows:6the abundance of Li is 8.87%, which is improved by 1.37% compared with the initial abundance.
In summary, in the separation and enrichment system for lithium isotopes provided in the embodiments of the present invention, the tube filled with the low-concentration acidic aqueous solution is disposed to elute the first enriched organic phase, and the tube in the organic phase is used to separate and enrich the lithium isotopes7Li is more eluted into the aqueous solution,6the proportion of Li retained in the organic phase is greater, and the content of Li in the organic phase is increased6Separation and enrichment abundance of Li; in addition, the organic extraction phase is made into organic small drops to be contacted with the low-concentration acidic aqueous solution, so that the contact area is increased, and the reaction time is saved.
The foregoing is directed to embodiments of the present application and it is noted that numerous modifications and adaptations may be made by those skilled in the art without departing from the principles of the present application and are intended to be within the scope of the present application.
Claims (10)
1. A separation and enrichment system of lithium isotopes is characterized by comprising an organic extraction phase, a lithium salt solution phase, a stripping solution and a pipe body filled with a low-concentration acidic aqueous solution; wherein the content of the first and second substances,
the organic extraction phase is used for reacting with the lithium salt solution phase to obtain a first enriched organic phase;
the tube filled with the low-concentration acidic aqueous solution is used for eluting the first enriched organic phase, and comprises: (ii) injecting the first enriched organic phase dropwise into the tube filled with the low-concentration acidic aqueous solution, the first enriched organic phase accumulating at the bottom of the tube to form a second enriched organic phase;
the back extraction solution is used for back extraction of the first solution to obtain enriched6A solution of Li.
2. The system for separating and enriching lithium isotopes as claimed in claim 1, wherein the organic extraction phase comprises an extractant and a diluent mixed with each other; wherein the content of the first and second substances,
the extractant is selected from any one of compounds shown in the following formulas 1 to 3,
in the compounds shown in the formulas 1 to 3, R is selected from alkyl, alkoxy, amino, nitro or phenyl with 0-20 carbon atoms, X is N or O, and N is 0, 1 or 2;
the diluent is selected from one or more than two of iodobenzene, dichloromethane, carbon tetrachloride, chloroform, 1, 2-dichloroethane, nitrobenzene or 1,1, 2-trichloroethane.
3. The system for separating and enriching lithium isotopes as claimed in claim 2, wherein the concentration of the extractant in the organic extraction phase is 0.4mol/L to 0.8 mol/L.
4. The system for separation and enrichment of lithium isotopes as claimed in claim 1, wherein the lithium salt in the solution phase of lithium salt is selected from the group consisting of LiCl, LiBr, LiI, LiOH, LiNO3、LiClO4、LiSCN、CH3COOLi、CF3COOLi、CHF2COOLi、CH2FCOOLi and Li [ 2 ]NTf2]And the concentration of the lithium salt in the lithium salt solution is 1-4 mol/L.
5. The separation and enrichment system for lithium isotopes as claimed in claim 1, wherein the organic extraction phase and the lithium salt solution phase are mixed according to a volume ratio of 1 (1-10) for oscillatory extraction reaction to obtain the first enriched organic phase.
6. The system for separating and enriching lithium isotopes as claimed in claim 1, wherein the stripping solution is selected from the group consisting of HCl, HBr, HI, NaCl, KCl, H2SO4、HNO3And HClO4The concentration of the stripping solution is 1 mol/L-5 mol/L.
7. The system for separating and enriching lithium isotopes as claimed in any one of claims 1 to 6, wherein the low-concentration acidic aqueous solution is HCl, HBr, HI, H2SO4、HNO3And HClO4The concentration of the solute in the low-concentration acidic aqueous solution is 0.1 to 1 mol/L.
8. The system for separating and enriching lithium isotopes as claimed in claim 7, wherein the concentration of the solute in the low-concentration acidic aqueous solution is 0.2mol/L to 0.8 mol/L.
9. The system for the precipitation separation of lithium isotopes as claimed in claim 7, wherein said second organic phase enriched is withdrawn from said tubular body and the aqueous solution therein is removed by centrifugation.
10. The system for the precipitation separation of lithium isotopes as claimed in claim 7, wherein the height of said tube filled with the low-concentration acidic aqueous solution is between 0.5 and 2 meters.
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