CN112452151A - Separation and enrichment method of lithium isotope - Google Patents
Separation and enrichment method of lithium isotope Download PDFInfo
- Publication number
- CN112452151A CN112452151A CN201910840738.1A CN201910840738A CN112452151A CN 112452151 A CN112452151 A CN 112452151A CN 201910840738 A CN201910840738 A CN 201910840738A CN 112452151 A CN112452151 A CN 112452151A
- Authority
- CN
- China
- Prior art keywords
- organic phase
- lithium
- separation
- enrichment
- enrichment method
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 238000000034 method Methods 0.000 title claims abstract description 41
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims abstract description 38
- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 37
- 238000000926 separation method Methods 0.000 title claims abstract description 24
- 239000012074 organic phase Substances 0.000 claims abstract description 104
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical group [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 claims abstract description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 21
- 229910003002 lithium salt Inorganic materials 0.000 claims abstract description 20
- 159000000002 lithium salts Chemical class 0.000 claims abstract description 19
- 238000002156 mixing Methods 0.000 claims abstract description 19
- 239000012266 salt solution Substances 0.000 claims abstract description 18
- 238000010828 elution Methods 0.000 claims abstract description 16
- 238000000605 extraction Methods 0.000 claims abstract description 15
- 239000003480 eluent Substances 0.000 claims abstract description 14
- WZJYKHNJTSNBHV-UHFFFAOYSA-N benzoquinoline Natural products C1=CN=C2C3=CC=CC=C3C=CC2=C1 WZJYKHNJTSNBHV-UHFFFAOYSA-N 0.000 claims abstract description 13
- -1 benzoquinoline compound Chemical class 0.000 claims abstract description 7
- 239000003085 diluting agent Substances 0.000 claims abstract description 5
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 3
- 238000005119 centrifugation Methods 0.000 claims abstract 2
- 230000010355 oscillation Effects 0.000 claims abstract 2
- 229910001416 lithium ion Inorganic materials 0.000 claims description 22
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 12
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical compound [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 claims description 10
- KESRRRLHHXXBRW-UHFFFAOYSA-N C1=CC=NC2=C3C(O)=CC=CC3=CC=C21 Chemical compound C1=CC=NC2=C3C(O)=CC=CC3=CC=C21 KESRRRLHHXXBRW-UHFFFAOYSA-N 0.000 claims description 9
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 9
- RDOXTESZEPMUJZ-UHFFFAOYSA-N anisole Chemical compound COC1=CC=CC=C1 RDOXTESZEPMUJZ-UHFFFAOYSA-N 0.000 claims description 8
- AIWXPYMIQOHCIW-UHFFFAOYSA-N CC1=CC=NC2=C3C(=CC=C12)C=CC=C3O Chemical compound CC1=CC=NC2=C3C(=CC=C12)C=CC=C3O AIWXPYMIQOHCIW-UHFFFAOYSA-N 0.000 claims description 6
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 6
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 claims description 6
- HSZCZNFXUDYRKD-UHFFFAOYSA-M lithium iodide Chemical compound [Li+].[I-] HSZCZNFXUDYRKD-UHFFFAOYSA-M 0.000 claims description 6
- BTKZSEVSMHPYGI-UHFFFAOYSA-N C1=CN=C2C3=CC=C(O)C=C3C=CC2=C1 Chemical compound C1=CN=C2C3=CC=C(O)C=C3C=CC2=C1 BTKZSEVSMHPYGI-UHFFFAOYSA-N 0.000 claims description 5
- 229910003473 lithium bis(trifluoromethanesulfonyl)imide Inorganic materials 0.000 claims description 5
- PQXKHYXIUOZZFA-UHFFFAOYSA-M lithium fluoride Chemical compound [Li+].[F-] PQXKHYXIUOZZFA-UHFFFAOYSA-M 0.000 claims description 5
- QSZMZKBZAYQGRS-UHFFFAOYSA-N lithium;bis(trifluoromethylsulfonyl)azanide Chemical compound [Li+].FC(F)(F)S(=O)(=O)[N-]S(=O)(=O)C(F)(F)F QSZMZKBZAYQGRS-UHFFFAOYSA-N 0.000 claims description 5
- SCYULBFZEHDVBN-UHFFFAOYSA-N 1,1-Dichloroethane Chemical compound CC(Cl)Cl SCYULBFZEHDVBN-UHFFFAOYSA-N 0.000 claims description 4
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 4
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 4
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 4
- MVPPADPHJFYWMZ-UHFFFAOYSA-N chlorobenzene Chemical compound ClC1=CC=CC=C1 MVPPADPHJFYWMZ-UHFFFAOYSA-N 0.000 claims description 4
- ZXEKIIBDNHEJCQ-UHFFFAOYSA-N isobutanol Chemical compound CC(C)CO ZXEKIIBDNHEJCQ-UHFFFAOYSA-N 0.000 claims description 4
- AMXOYNBUYSYVKV-UHFFFAOYSA-M lithium bromide Chemical compound [Li+].[Br-] AMXOYNBUYSYVKV-UHFFFAOYSA-M 0.000 claims description 4
- IIPYXGDZVMZOAP-UHFFFAOYSA-N lithium nitrate Chemical compound [Li+].[O-][N+]([O-])=O IIPYXGDZVMZOAP-UHFFFAOYSA-N 0.000 claims description 4
- UZKWTJUDCOPSNM-UHFFFAOYSA-N methoxybenzene Substances CCCCOC=C UZKWTJUDCOPSNM-UHFFFAOYSA-N 0.000 claims description 4
- VZGDMQKNWNREIO-UHFFFAOYSA-N tetrachloromethane Chemical compound ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 claims description 4
- 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
- OCJBOOLMMGQPQU-UHFFFAOYSA-N 1,4-dichlorobenzene Chemical compound ClC1=CC=C(Cl)C=C1 OCJBOOLMMGQPQU-UHFFFAOYSA-N 0.000 claims description 2
- LGKQWGIPMCZVEU-UHFFFAOYSA-N 3-methylbenzo[h]quinoline Chemical compound C1=CC=C2C3=NC=C(C)C=C3C=CC2=C1 LGKQWGIPMCZVEU-UHFFFAOYSA-N 0.000 claims description 2
- JZVUAOCDNFNSGQ-UHFFFAOYSA-N 7-methoxy-2-phenyl-1h-quinolin-4-one Chemical compound N=1C2=CC(OC)=CC=C2C(O)=CC=1C1=CC=CC=C1 JZVUAOCDNFNSGQ-UHFFFAOYSA-N 0.000 claims description 2
- DKPFZGUDAPQIHT-UHFFFAOYSA-N Butyl acetate Natural products CCCCOC(C)=O DKPFZGUDAPQIHT-UHFFFAOYSA-N 0.000 claims description 2
- ZAFNJMIOTHYJRJ-UHFFFAOYSA-N Diisopropyl ether Chemical compound CC(C)OC(C)C ZAFNJMIOTHYJRJ-UHFFFAOYSA-N 0.000 claims description 2
- 229940117389 dichlorobenzene Drugs 0.000 claims description 2
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 claims description 2
- XIXADJRWDQXREU-UHFFFAOYSA-M lithium acetate Chemical compound [Li+].CC([O-])=O XIXADJRWDQXREU-UHFFFAOYSA-M 0.000 claims description 2
- INHCSSUBVCNVSK-UHFFFAOYSA-L lithium sulfate Inorganic materials [Li+].[Li+].[O-]S([O-])(=O)=O INHCSSUBVCNVSK-UHFFFAOYSA-L 0.000 claims description 2
- 239000003208 petroleum Substances 0.000 claims description 2
- RBTVSNLYYIMMKS-UHFFFAOYSA-N tert-butyl 3-aminoazetidine-1-carboxylate;hydrochloride Chemical compound Cl.CC(C)(C)OC(=O)N1CC(N)C1 RBTVSNLYYIMMKS-UHFFFAOYSA-N 0.000 claims description 2
- 239000008096 xylene Substances 0.000 claims description 2
- 239000012071 phase Substances 0.000 abstract description 4
- 239000002253 acid Substances 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 238000011282 treatment Methods 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 16
- 238000006243 chemical reaction Methods 0.000 description 4
- 238000011161 development Methods 0.000 description 3
- 230000004927 fusion Effects 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 229910000497 Amalgam Inorganic materials 0.000 description 2
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 239000002826 coolant Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000007792 addition Methods 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 238000005372 isotope separation Methods 0.000 description 1
- WMFOQBRAJBCJND-UHFFFAOYSA-M lithium hydroxide Inorganic materials [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 description 1
- 239000003758 nuclear fuel Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 229920005597 polymer membrane Polymers 0.000 description 1
- 238000011112 process operation Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
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
Abstract
The invention discloses a separation and enrichment method of lithium isotopes, which comprises the following steps: s1, uniformly mixing a diluent and a benzoquinoline compound serving as an extracting agent to form an extracted organic phase; s2, uniformly mixing the extracted organic phase with a lithium salt solution, and performing oscillation centrifugation to collect an organic phase; s3, carrying out multistage elution treatment on the collected organic phase by using eluent to obtain enrichment7An organic phase of Li. The method provided by the invention realizes the enrichment of lithium isotopes in the multi-stage elution process. Different from the traditional extraction process, the process realizes the enrichment of lithium isotopes in the extraction and elution processes. During elution, eluent is added into the extracted organic phase, lithium ions form dynamic equilibrium in the two phases, and meanwhile, the extractant pair in the organic phase7The particular selectivity of Li, and therefore,7li is enriched in an organic phase, so that the high-efficiency separation of lithium isotopes is realized, and the method takes water as an eluent, thereby reducing the use of strong acid and the organic phase, and greatly reducing the production cost and the pollution to the environment.
Description
Technical Field
The invention belongs to the technical field of lithium isotope enrichment, and particularly relates to a separation and enrichment method of lithium isotopes.
Background
Naturally occurring lithium exists in two stable isotopes, namely6Li and7li in a relative abundance of6The content of Li is 7.53 percent,7li is 92.47%.7The thermal neutron absorption cross section of Li is very small and is only 0.036b, which shows that7Li is hard to collide with neutrons, and therefore7Li can regulate the reaction rate in nuclear reactions and also can maintain equipment in nuclear reactors, e.g. ultra-pure7LiF can be used as coolant and heat carrier of nuclear fusion reactor;7LiOH can be used as a pH regulator of a pressurized water reactor, reduces corrosion of reaction equipment and ensures safety of nuclear reaction.
The international thermonuclear fusion experimental reactor (ITER) plan participating in research and development in China is one of the currently recognized important ways of finally solving the energy problem and the environmental problem of the human society and promoting the sustainable development of the human society. And two isotopes of lithium6Li and7li is nuclear fuel and coolant necessary for the experiment and operation of thermonuclear fusion reactor. Therefore, separation of the two lithium isotopes is crucial. China has abundant lithium resources, the total reserve is the fourth place in the world, the lithium resource distribution is relatively concentrated, and the reserve of Qinghai, Tibet and Sichuan lithium resources accounts for 85.23 percent of the total amount. Therefore, the research on the separation of lithium isotopes has extremely important significance for the development of clean energy and the effective development and utilization of lithium resources in China.
In 1936, Lewis and Mac Donald reported a chemical exchange separation system for chemical lithium amalgam and LiCl solutions for the first time, and then reported a combination of lithium amalgam and lithiumMethod for separating Lithium Isotopes in organic-organic phase system (Lewis G N, Macdonald R T. the Separation of Lithium Isotopes [ J]Journal of the American Chemical Society,1936,58(12): 2519-; study on separation of lithium isotope with 6- (4-ethyl-1-methyloctyl) 8-hydroxybenzoquinoline as extractant and separation factor of 1.003 in Weeken [ D. study on novel system for extraction and separation of lithium isotope]South of the Yangtze university, 2014.); the patent CN106731838B provides an extraction chromatographic column prepared by filling a benzo crown ether functionalized SBA-15 type ordered mesoporous silica-based material in a chromatographic column; patent CN108619909A provides a method for separating lithium isotopes by using a porous polymer membrane with lithium isotope separation effect as a filler to fill a membrane chromatographic column, eluting with an eluent, and using a multi-stage membrane chromatographic cascade technology; patent CN108854536A provides a complete set of equipment for extracting enriched lithium isotopes; patent CN108854535A provides a split-flow extraction process for separating lithium isotopes; patent CN108854537A provides a method for simultaneously obtaining enrichment6Li and7two product-rich processes for Li. From the data, the enrichment of lithium isotopes in the traditional multistage process is completed in the extraction section, and the back extraction process only converts lithium ions in an organic phase into an aqueous solution, so that the lithium ions can conveniently enter the next-stage extraction process. Fresh organic extractant and organic solvent are required each time a new extraction run is entered. The use of strong acid and a large amount of organic matters easily causes serious pollution to the ecological environment, and in addition, the process cost is greatly increased.
Disclosure of Invention
The invention mainly aims to provide a method for separating and enriching lithium isotopes, so as to overcome the defects of the prior art.
In order to achieve the purpose, the technical scheme adopted by the invention comprises the following steps:
the embodiment of the invention provides a separation and enrichment method of lithium isotopes, which comprises the following steps:
s1, uniformly mixing a diluent and a benzoquinoline compound serving as an extracting agent to form an extracted organic phase;
s2, the extracted organic phase is mixed with a solvent containing6Li、7Lithium salt solution of LiMixing uniformly, oscillating, centrifuging and collecting an organic phase;
s3, eluting the collected organic phase with an eluent to obtain enrichment7An organic phase of Li.
Further, the diluent includes any one or a combination of two or more of anisole, dichloromethane, chlorobenzene, dichlorobenzene, toluene, xylene, carbon tetrachloride, dichloroethane, petroleum ether, ethyl acetate, n-butanol, toluene, n-heptane, butyl acetate, isopropyl ether, and isobutanol, without being limited thereto.
Further, the benzoquinoline compound includes any one or a combination of two or more of benzoquinoline, 10-hydroxybenzoquinoline, 4-methyl-10-hydroxybenzoquinoline, 3-methylbenzoquinoline, and 8-hydroxybenzoquinoline, but is not limited thereto.
Furthermore, the concentration of the benzoquinoline compound in the extracted organic phase is 0.01-10 mol/L.
Further, the lithium salt contained in the lithium salt solution includes any one or a combination of two or more of lithium fluoride, lithium chloride, lithium bromide, lithium iodide, lithium acetate, lithium sulfate, lithium nitrate, lithium perchlorate, lithium trifluoroacetate, and lithium bis (trifluoromethanesulfonyl) imide, and is not limited thereto.
Further, the concentration of lithium ions in the lithium salt solution is 0.1-20 mol/L, wherein the lithium salt solution contains lithium isotope6Li and7Li。
further, the volume ratio of the organic phase to the lithium salt solution in the step S2 is 1: 0.1-20.
Further, the eluent includes water, and is not limited thereto.
Further, the volume ratio of the eluent to the organic phase in the step S3 is 1: 1-100.
Further, the number of elution processes in step S3 is 1 to 1000.
In some preferred embodiments, the number of elution treatments in step S3 is 1 to 300.
Benzoquinolines as extractant pair7Li has special selectivity, and in the extraction stage, the extracted organic phase is mixed with lithium salt solution to make partial lithium ion enter into the organic phase and small amount of lithium ion is added7Li will be concentrated in the organic phase. In the elution section, eluent water is selected and uniformly mixed with the extracted organic phase, which is different from the traditional back extraction, and the purpose of the method is not to convert lithium ions in the organic phase into the eluent but to realize the purpose7Li is enriched in the organic phase. The enrichment of lithium isotopes during the elution process can be achieved mainly for the following reasons: firstly, in the elution process, partial lithium ions enter an elution phase, and the lithium ions reach dynamic equilibrium in the elution phase and an organic phase; second, benzoquinolines in the organic phase7Li has special selectivity, and lithium isotope can establish an abundance dynamic balance in an organic phase and an elution phase to achieve7Enrichment of Li in the organic phase.
Compared with the prior art, the invention has the advantages that: the invention provides a separation and enrichment method of lithium isotopes, which realizes the enrichment of the lithium isotopes at the extraction and elution stages simultaneously, changes the method that the lithium isotopes are enriched only at the extraction stage in the prior method, and adopts secondary water as the eluent, wherein the water is a green eluent and does not pollute the environment; meanwhile, the extraction-elution continuous multiple separation and enrichment method reduces the use of a large amount of strong acid and a fresh organic phase, and greatly reduces the production cost and the pollution to the environment.
Detailed Description
In view of the defects of the prior art, the inventors of the present invention have long studied and practiced in great numbers to provide the technical solution of the present invention, which mainly utilizes an extractant pair7The special selectivity of Li establishes a dynamic balance of the abundance of lithium isotopes in the extraction and elution processes to achieve7Enrichment of Li in the organic phase.
The technical solution of the present invention is further explained by the following embodiments. It is easily understood by those skilled in the art that the examples are only for the understanding of the present invention and should not be construed as the specific limitations of the present invention.
Example 1
(1) Uniformly mixing 10-hydroxybenzoquinoline and anisole to form an extracted organic phase, wherein the concentration of the 10-hydroxybenzoquinoline is 0.2mol/L, and a lithium chloride solution with the lithium ion concentration of 1mol/L is prepared;
(2) fully and uniformly mixing the extracted organic phase and the water-soluble lithium salt solution according to the volume ratio of 1:1, oscillating for 1h, centrifuging and collecting the organic phase, and analyzing the organic phase7The abundance of Li is 92.61%;
(3) eluting the extracted organic phase with water for 5 times to obtain enriched solution7An organic phase of Li, wherein the volume ratio of the organic phase to water is 1:1, was analyzed in the organic phase7The abundance of Li was 93.02%.
Example 2
(1) Uniformly mixing 8-hydroxybenzoquinoline and dichloroethane to form an extracted organic phase, wherein the concentration of the 10-hydroxybenzoquinoline is 0.4mol/L, and a lithium iodide solution with the lithium ion concentration of 3mol/L is prepared;
(2) fully and uniformly mixing the extracted organic phase and the water-soluble lithium salt solution according to the volume ratio of 1:1, oscillating for 1h, centrifuging and collecting the organic phase, and analyzing the organic phase7The abundance of Li is 92.64%;
(3) eluting the extracted organic phase with water for 10 times to obtain enriched solution7An organic phase of Li, wherein the volume ratio of the organic phase to water is 1:1, was analyzed in the organic phase7The abundance of Li was 93.89%.
Example 3
(1) Uniformly mixing 8-hydroxybenzoquinoline and anisole to form an extracted organic phase, wherein the concentration of the 8-hydroxybenzoquinoline is 0.6mol/L, and a lithium perchlorate solution with the lithium ion concentration of 3mol/L is prepared;
(2) fully and uniformly mixing the extracted organic phase and the water-soluble lithium salt solution according to the volume ratio of 1:1, oscillating for 1h, centrifuging and collecting the organic phase, and analyzing the organic phase7The abundance of Li is 92.51%;
(3) eluting the extracted organic phase with water, and repeating the eluting stepsCounting 10 times to obtain enrichment7An organic phase of Li, wherein the volume ratio of the organic phase to water is 1:1, was analyzed in the organic phase7The abundance of Li was 93.79%.
Example 4
(1) Uniformly mixing 4-methyl-10-hydroxybenzoquinoline and dichloroethane to form an extracted organic phase, wherein the concentration of the 4-methyl-10-hydroxybenzoquinoline is 2mol/L, and a lithium chloride solution with the lithium ion concentration of 10mol/L is prepared;
(2) fully and uniformly mixing the extracted organic phase and the water-soluble lithium salt solution according to the volume ratio of 20:1, oscillating for 1h, centrifuging and collecting the organic phase, and analyzing the organic phase7The abundance of Li is 92.81%;
(3) eluting the extracted organic phase with water for 50 times to obtain enriched solution7An organic phase of Li, wherein the volume ratio of the organic phase to water is 10:1, was analyzed in the organic phase7The abundance of Li was 94.56%.
Example 5
(1) Uniformly mixing 10-hydroxybenzoquinoline and dimethylbenzene to form an extracted organic phase, wherein the concentration of the 10-hydroxybenzoquinoline is 2mol/L, and preparing a lithium bis (trifluoromethanesulfonyl) imide solution with the lithium ion concentration of 10 mol/L;
(2) fully and uniformly mixing the extracted organic phase and the water-soluble lithium salt solution according to the volume ratio of 1:10, oscillating for 1h, centrifuging and collecting the organic phase, and analyzing the organic phase7The abundance of Li is 92.61%;
(3) eluting the extracted organic phase with water for 50 times to obtain enriched solution7And (3) an organic phase of Li, wherein the volume ratio of the organic phase to water is 20:1, the step (2) can be simultaneously carried out in multiple groups, and when the lithium ion concentration in each group of organic phases is low, all the organic phases rich in lithium ions can be mixed and concentrated to increase the concentration in the organic phases. Analyzed in the organic phase7The abundance of Li was 96.12%.
Example 6
(1) Uniformly mixing 4-methyl-10-hydroxybenzoquinoline and chloroform to form an extracted organic phase, wherein the concentration of the 4-methyl-10-hydroxybenzoquinoline is 2mol/L, and preparing a lithium bis (trifluoromethanesulfonyl) imide solution with the lithium ion concentration of 10 mol/L;
(2) fully and uniformly mixing the extracted organic phase and the water-soluble lithium salt solution according to the volume ratio of 1:20, oscillating for 1h, centrifuging and collecting the organic phase, and analyzing the organic phase7The abundance of Li is 92.43%;
(3) eluting the extracted organic phase with water for 100 times to obtain enriched solution7And (3) an organic phase of Li, wherein the volume ratio of the organic phase to water is 10:1, the step (2) can be simultaneously carried out in multiple groups, and when the lithium ion concentration in each group of organic phases is lower, all the organic phases rich in lithium ions can be mixed and concentrated to increase the concentration in the organic phases. Analyzed in the organic phase7The abundance of Li was 96.56%.
Example 7
(1) Uniformly mixing 10-hydroxybenzoquinoline and dichloromethane to form an extracted organic phase, wherein the concentration of the 10-hydroxybenzoquinoline is 3mol/L, and preparing a lithium bis (trifluoromethanesulfonyl) imide solution with the lithium ion concentration of 10 mol/L;
(2) fully and uniformly mixing the extracted organic phase and the water-soluble lithium salt solution according to the volume ratio of 10:1, oscillating for 1h, centrifuging and collecting the organic phase, and analyzing the organic phase7The abundance of Li is 92.55%;
(3) eluting the extracted organic phase with water for 300 times to obtain enriched solution7And (3) an organic phase of Li, wherein the volume ratio of the organic phase to water is 10:1, the step (2) can be simultaneously carried out in multiple groups, and when the lithium ion concentration in each group of organic phases is lower, all the organic phases rich in lithium ions can be mixed and concentrated to increase the concentration in the organic phases. Analyzed in the organic phase7The abundance of Li was 97.68%.
The aspects, embodiments, features and examples of the present invention should be considered as illustrative in all respects and not intended to be limiting of the invention, the scope of which is defined only by the claims. Other embodiments, modifications, and uses will be apparent to those skilled in the art without departing from the spirit and scope of the claimed invention.
The use of headings and chapters in this disclosure is not meant to limit the disclosure; each section may apply to any aspect, embodiment, or feature of the disclosure.
Throughout this specification, where a composition is described as having, containing, or comprising specific components or where a process is described as having, containing, or comprising specific process steps, it is contemplated that the composition of the present teachings also consist essentially of, or consist of, the recited components, and the process of the present teachings also consist essentially of, or consist of, the recited process steps.
It should be understood that the order of steps or the order in which particular actions are performed is not critical, so long as the teachings of the invention remain operable. Further, two or more steps or actions may be performed simultaneously.
In addition, the inventors of the present invention have also made experiments with other materials, process operations, and process conditions described in the present specification with reference to the above examples, and have obtained preferable results.
While the invention has been described with reference to illustrative embodiments, it will be understood by those skilled in the art that various other changes, omissions and/or additions may be made and substantial equivalents may be substituted for elements thereof without departing from the spirit and scope of the invention. In addition, many modifications may be made to adapt a particular situation or material to the teachings of the invention without departing from its scope. Therefore, it is intended that the invention not be limited to the particular embodiment disclosed for carrying out this invention, but that the invention will include all embodiments falling within the scope of the appended claims. Moreover, unless specifically stated any use of the terms first, second, etc. do not denote any order or importance, but rather the terms first, second, etc. are used to distinguish one element from another.
Claims (10)
1. A method for separating and enriching lithium isotopes is characterized by comprising the following steps:
s1, uniformly mixing a diluent and a benzoquinoline compound serving as an extracting agent to form an extracted organic phase;
s2, uniformly mixing the extracted organic phase with a lithium salt solution, and performing oscillation centrifugation to collect an organic phase;
s3, eluting the collected organic phase with an eluent to obtain enrichment7An organic phase of Li.
2. The separation and enrichment method according to claim 1, wherein the diluent comprises any one or a combination of two or more of anisole, dichloromethane, chlorobenzene, dichlorobenzene, toluene, xylene, carbon tetrachloride, dichloroethane, petroleum ether, ethyl acetate, n-butanol, toluene, n-heptane, butyl acetate, isopropyl ether and isobutanol.
3. The separation and enrichment method according to claim 1, wherein the benzoquinolines comprise any one or a combination of two or more of benzoquinoline, 10-hydroxybenzoquinoline, 4-methyl-10-hydroxybenzoquinoline, 3-methylbenzoquinoline and 8-hydroxybenzoquinoline.
4. The separation and enrichment method according to claim 1, wherein the concentration of the benzoquinolines in the extracted organic phase is 0.1mol/L to 10 mol/L.
5. The separation and enrichment method according to claim 1, wherein the lithium salt contained in the lithium salt solution comprises any one or a combination of two or more of lithium fluoride, lithium chloride, lithium bromide, lithium iodide, lithium acetate, lithium sulfate, lithium nitrate, lithium perchlorate, lithium trifluoroacetate, and lithium bis (trifluoromethanesulfonyl) imide.
6. The separation and enrichment method according to claim 1, wherein the concentration of lithium ions in the lithium salt solution is 0.1mol/L to 20 mol/L.
7. The separation and enrichment method according to claim 1, wherein the volume ratio of the extraction organic phase to the lithium salt solution in step S2 is 1: 0.1-20.
8. The separation and enrichment method according to claim 1, wherein the eluent comprises water.
9. The separation and enrichment method according to claim 1, wherein the volume ratio of the eluent to the organic phase in the step S3 is 1: 1-100.
10. The separation and enrichment method according to claim 1, wherein the number of elution processes in step S3 is 1-1000.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910840738.1A CN112452151A (en) | 2019-09-06 | 2019-09-06 | Separation and enrichment method of lithium isotope |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910840738.1A CN112452151A (en) | 2019-09-06 | 2019-09-06 | Separation and enrichment method of lithium isotope |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN112452151A true CN112452151A (en) | 2021-03-09 |
Family
ID=74807727
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910840738.1A Pending CN112452151A (en) | 2019-09-06 | 2019-09-06 | Separation and enrichment method of lithium isotope |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112452151A (en) |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103801194A (en) * | 2012-11-05 | 2014-05-21 | 中国科学院上海有机化学研究所 | Extraction agent for separation of lithium isotopes and application thereof |
| WO2014201890A1 (en) * | 2013-06-17 | 2014-12-24 | 中国科学院上海有机化学研究所 | Backflow cascade novel process for producing lithium-7 isotope |
| CN105536537A (en) * | 2015-12-17 | 2016-05-04 | 中国科学院青海盐湖研究所 | Method for extracting lithium isotope |
| CN108854534A (en) * | 2017-05-15 | 2018-11-23 | 中国科学院上海有机化学研究所 | The technique of crown ether extraction separation lithium isotope |
| CN109260950A (en) * | 2018-11-16 | 2019-01-25 | 中国科学院青海盐湖研究所 | A kind of method for separating and concentrating of lithium isotope |
-
2019
- 2019-09-06 CN CN201910840738.1A patent/CN112452151A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103801194A (en) * | 2012-11-05 | 2014-05-21 | 中国科学院上海有机化学研究所 | Extraction agent for separation of lithium isotopes and application thereof |
| WO2014201890A1 (en) * | 2013-06-17 | 2014-12-24 | 中国科学院上海有机化学研究所 | Backflow cascade novel process for producing lithium-7 isotope |
| CN105536537A (en) * | 2015-12-17 | 2016-05-04 | 中国科学院青海盐湖研究所 | Method for extracting lithium isotope |
| CN108854534A (en) * | 2017-05-15 | 2018-11-23 | 中国科学院上海有机化学研究所 | The technique of crown ether extraction separation lithium isotope |
| CN109260950A (en) * | 2018-11-16 | 2019-01-25 | 中国科学院青海盐湖研究所 | A kind of method for separating and concentrating of lithium isotope |
Non-Patent Citations (1)
| Title |
|---|
| 肖江;贾永忠;石成龙;王兴权;姚颖;景燕;: "化学交换法分离锂同位素研究进展", 《化工进展》, no. 01, 5 January 2017 (2017-01-05) * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104607046B (en) | A kind of method and apparatus utilizing membrane extraction to carry out lithium isotope separation and concentration | |
| CN105536537B (en) | A kind of method of extract and separate lithium isotope | |
| CN102430338B (en) | Method for extracting and separating lithium isotope aqueous solution | |
| CN109260950B (en) | Separation and enrichment method of lithium isotope | |
| CN105536536B (en) | A kind of extraction system for extracting lithium isotope | |
| CN112473370B (en) | Method for separating lithium isotope by electrodialysis | |
| CN105498542B (en) | The method for extracting lithium isotope | |
| CN103768945A (en) | Method for extraction separating of lithium isotope by virtue of sol-gel material | |
| CN105536707B (en) | A kind of material for separating lithium isotope and its preparation method and application | |
| CN106086471A (en) | A kind of method that lepidolite defluorinate and valuable metal leach | |
| CN112981139B (en) | Hydrophobic eutectic solvent for separating nickel and cobalt ions, preparation method thereof and method for separating nickel and cobalt ions | |
| CN103589866B (en) | Separation and recovery method for thorium and uranium by using silicon-based anion exchange resin | |
| CN112452150A (en) | Separation and enrichment method of lithium isotope | |
| CN101252027A (en) | Dissolution of UO in Ionic liquids2、PuO2Or spent fuel process | |
| CN108193058A (en) | A kind of method for the ion liquid abstraction that lithium is extracted from salt lake | |
| CN113262636B (en) | Extraction-electromigration coupling separation and enrichment 7 Method for producing Li isotopes | |
| CN108538417A (en) | A method of being directly separated uranium dioxide or spentnuclear fuel rare earth elements | |
| CN112452151A (en) | Separation and enrichment method of lithium isotope | |
| CN107181014A (en) | A kind of recovery method of waste lithium manganese oxide battery | |
| CN106731838A (en) | A kind of lithium isotope efficiently separates method | |
| CN109535474A (en) | A kind of application of cladded type impregnating resin and preparation method thereof and its rhenium in selective absorption waste acid | |
| CN112680609B (en) | Plutonium recovery ionic liquid extractant and method for extracting and separating plutonium from plutonium-containing waste liquid | |
| CN104789803A (en) | Method for separating uranium from uranium-containing alkaline sodium carbonate solution | |
| CN108977659A (en) | Plutonium, palladium, silver, cadmium, tin and antimony group separation method | |
| CN107686898B (en) | A method of hafnium oxide is prepared from recycling in waste material containing hafnium |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |