CN114380431A - Method for recovering lithium from seawater - Google Patents
Method for recovering lithium from seawater Download PDFInfo
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- CN114380431A CN114380431A CN202210050730.7A CN202210050730A CN114380431A CN 114380431 A CN114380431 A CN 114380431A CN 202210050730 A CN202210050730 A CN 202210050730A CN 114380431 A CN114380431 A CN 114380431A
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- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 86
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims abstract description 83
- 238000000034 method Methods 0.000 title claims abstract description 28
- 239000013535 sea water Substances 0.000 title claims abstract description 26
- 238000000909 electrodialysis Methods 0.000 claims abstract description 55
- 239000012528 membrane Substances 0.000 claims abstract description 21
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000000926 separation method Methods 0.000 claims abstract description 12
- 238000002474 experimental method Methods 0.000 claims abstract description 10
- 239000007788 liquid Substances 0.000 claims abstract description 9
- 239000002608 ionic liquid Substances 0.000 claims abstract description 8
- 150000002500 ions Chemical class 0.000 claims abstract description 8
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 claims abstract description 6
- 229910052808 lithium carbonate Inorganic materials 0.000 claims abstract description 6
- 239000007787 solid Substances 0.000 claims abstract description 6
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims abstract description 5
- 238000001914 filtration Methods 0.000 claims abstract description 3
- 238000000502 dialysis Methods 0.000 claims description 11
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical group [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 10
- 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 description 5
- 238000011084 recovery Methods 0.000 claims description 5
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 5
- 238000004062 sedimentation Methods 0.000 claims description 4
- 238000007667 floating Methods 0.000 claims description 2
- 239000002562 thickening agent Substances 0.000 claims description 2
- 238000000605 extraction Methods 0.000 abstract description 6
- 239000000243 solution Substances 0.000 description 16
- 239000011734 sodium Substances 0.000 description 9
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 description 7
- 239000012267 brine Substances 0.000 description 6
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 229910052791 calcium Inorganic materials 0.000 description 3
- 150000001768 cations Chemical class 0.000 description 3
- 229910052749 magnesium Inorganic materials 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 229910052700 potassium Inorganic materials 0.000 description 3
- 239000002244 precipitate Substances 0.000 description 3
- 238000005086 pumping Methods 0.000 description 3
- 229910052708 sodium Inorganic materials 0.000 description 3
- 239000004927 clay Substances 0.000 description 2
- 239000010438 granite Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 241000871495 Heeria argentea Species 0.000 description 1
- CNLWCVNCHLKFHK-UHFFFAOYSA-N aluminum;lithium;dioxido(oxo)silane Chemical compound [Li+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O CNLWCVNCHLKFHK-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 229910052629 lepidolite Inorganic materials 0.000 description 1
- GCICAPWZNUIIDV-UHFFFAOYSA-N lithium magnesium Chemical compound [Li].[Mg] GCICAPWZNUIIDV-UHFFFAOYSA-N 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 229910052642 spodumene Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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Classifications
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/469—Treatment of water, waste water, or sewage by electrochemical methods by electrochemical separation, e.g. by electro-osmosis, electrodialysis, electrophoresis
- C02F1/4693—Treatment of water, waste water, or sewage by electrochemical methods by electrochemical separation, e.g. by electro-osmosis, electrodialysis, electrophoresis electrodialysis
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D15/00—Lithium compounds
- C01D15/08—Carbonates; Bicarbonates
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/001—Processes for the treatment of water whereby the filtration technique is of importance
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F9/00—Multistage treatment of water, waste water or sewage
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B26/00—Obtaining alkali, alkaline earth metals or magnesium
- C22B26/10—Obtaining alkali metals
- C22B26/12—Obtaining lithium
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/44—Treatment or purification of solutions, e.g. obtained by leaching by chemical processes
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/38—Treatment of water, waste water, or sewage by centrifugal separation
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/58—Treatment of water, waste water, or sewage by removing specified dissolved compounds
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F2001/007—Processes including a sedimentation step
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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Abstract
The invention discloses a method for recovering lithium from seawater, which comprises the following steps: a) filtering the lithium-containing seawater to remove suspended matters to obtain filtered liquid; b) adding the filtered solution into a first electrodialysis experimental device, performing electrodialysis to remove divalent ions, and concentrating to obtain a lithium-containing concentrated solution; c) injecting ionic liquid into an electrodialysis membrane of the electrodialysis experiment device II; d) hydrochloric acid is introduced into the cathode of the electrodialysis experiment device II, the concentrated solution is introduced into the anode of the electrodialysis experiment device II, and electrodialysis is performed to obtain a lithium-containing solution; e) adding carbonate into the lithium-containing solution to precipitate lithium, and performing solid-liquid separation to obtain a lithium carbonate solid. The method for recovering lithium from seawater with the structure can extract lithium from seawater, solves the problems of shortage of lithium resources and high product price at present, reduces the lithium extraction cost, and promotes the development of automobile electromotion and lithium industry.
Description
Technical Field
The invention relates to the technical field of lithium extraction, in particular to a method for recovering lithium from seawater.
Background
The rare metal lithium is widely used in the emerging fields of batteries, medicines, nuclear industry, aerospace, new energy automobiles and the like, and is an indispensable raw material for the modern high-tech industry. So called "21 st century new energy metal" and "metal promoting world progress", have extremely high economic and strategic values. As an important energy metal, lithium energy is internationally recognized as a development direction of new energy in the future, and the strength of competing and developing lithium resources in various countries is continuously strengthened. According to the general classification, lithium deposits are classified mainly into three major types, namely, pegmatite type, brine type and clay type. According to the latest statistics of 2016, the world-wide has found that the amount of Li resource is larger than 4099X 104t, reserve of about 14X 106t, wherein the pegmatite type accounts for about 29%, the brine type accounts for about 64%, and the clay type accounts for 7%. Before the 90 s of the 20 th century, pegmatite-type lithium resources were exploited and utilized worldwide most, with the ore minerals mainly being spodumene and lepidolite from granite/granite pegmatite. The pegmatite type lithium deposit is lower than the salt lake type lithium deposit in scale and potential reserve, and the energy consumption for extracting lithium is large and the production cost is high. After the 80 s of the 20 th century, the salt lake brine type lithium resource gradually replaced the pegmatite type lithium resource and became the main raw material for the lithium industrial production. Lithium in the brine form of salt lakes in the region of "lithium triangle" (bolivia, argentina, chile) provides a global supply of 60% lithium resources. The Chinese lithium resource amount is 54 multiplied by 105t accounts for about 13.8% of the total world resources, 5 th rank, mainly brine type, about 70% and pegmatite type accounts for 30%. Although the lithium ore resources in China are rich, most of the lithium ores are distributed in Qinghai-Tibet plateau, and the development conditions are poor. And most of brine type lithium ores have high magnesium-lithium ratio, the lithium extraction technology is not completely mature, and the resource development and utilization are limited by the environment and the technology. Therefore, the guarantee of lithium resources in China is seriously insufficient, and the external dependence is highUp to 76%. Currently, the main global lithium production capacity is concentrated in SQM, FMC and Rockwood, which account for about 73% of the global production capacity, and thus, the global oligopolistic pattern of the lithium industry is created. The supply pattern of the lithium resource, namely the resource concentration and the energy concentration, brings huge risks to the supply of the lithium resource in various countries. Therefore, the search for new lithium resources, particularly new types of lithium resources, has become a priority in major industrial countries.
Disclosure of Invention
The invention aims to provide a method for recovering lithium from seawater, which can extract lithium from seawater, solve the problems of the lack of lithium resources and high product price at present, reduce the lithium extraction cost and promote the development of automobile electromotion and lithium industry.
In order to achieve the above objects, the present invention provides a method for recovering lithium from seawater,
a) filtering the lithium-containing seawater to remove suspended matters to obtain filtered liquid;
b) adding the filtered solution into a first electrodialysis experimental device, performing electrodialysis to remove divalent ions, and concentrating to obtain a lithium-containing concentrated solution;
c) injecting ionic liquid into an electrodialysis membrane in an electrodialysis experimental device II;
d) hydrochloric acid is introduced into the cathode of the electrodialysis experiment device II, the concentrated solution is introduced into the anode of the electrodialysis experiment device II, and electrodialysis is performed to obtain a lithium-containing solution;
e) adding carbonate into the lithium-containing solution to precipitate lithium, and performing solid-liquid separation to obtain a lithium carbonate solid.
Preferably, the solid-liquid separation equipment is one or more of a filter press, a sedimentation centrifuge, a sedimentation thickener, a floating ball clarifier, a bag filter or a separation column.
Preferably, in step b), the electrodialysis experimental device is a separation membrane using SELEMION CSO as a divalent ion.
Preferably, in step b), the electrodialysis has a dialysis voltage of 3V and a dialysis time of about 5 hours.
Preferably, in step c), the ionic liquid is N-methyl-N-propylpiperidine bis (trifluoromethanesulfonyl) imide (PP 13-TFSI).
Preferably, in step c), the electrodialysis membrane of the second electrodialysis experimental device is a SELEMION CMV membrane.
Preferably, in step d), the concentration of the hydrochloric acid is 0.1mol/L, the dialysis voltage of the electrodialysis is 2V, and the dialysis time is about 120 minutes.
Preferably, in step d), the recovery rate of lithium from the lithium-containing solution is 24.5 to 40.6%.
Preferably, in step e), the carbonate is sodium carbonate.
The invention has the beneficial effects that:
(1) the method can extract lithium from seawater, and solves the problems of the prior art that lithium resources are scarce and the product price is high;
(2) compared with the extraction of lithium from ore and brine, the method can greatly reduce the cost of lithium extraction;
(3) promote the development of automobile electromotion and the development of lithium industry.
The technical solution of the present invention is further described in detail by the accompanying drawings and embodiments.
Drawings
FIG. 1 is a process flow diagram of an embodiment of a method of the present invention for recovering lithium from seawater.
Detailed Description
The present invention will be further described with reference to the accompanying drawings and examples, in which various chemicals and reagents are commercially available unless otherwise specified.
Example 1
Pumping a large amount of lithium-containing seawater into a bag filter to filter and remove suspended particles for later use. 15L of the filtered solution is added into a first electrodialysis experimental device, wherein the first electrodialysis experimental device adopts SELEMION CSO as a divalent ion separation membrane, and Na in seawater is 10500ppm, Mg is 1350ppm, Ca is 400ppm, K is 380ppm and Li is 170 ppb. The voltage was adjusted to 3V and after 5h of electrodialysis, 3.8L of lithium-containing concentrated solution was collected at the cathode, which contained 26140ppm of Na, 68ppm of Mg, 44ppm of Ca, 1013ppm of K and 340ppb of Li. And adding 3.8L of lithium-containing concentrated solution into the anode of a second electrodialysis experimental device, wherein the second electrodialysis experimental device takes a SELEMION CMV membrane as an electrodialysis membrane, an ionic liquid N-methyl-N-propylpiperidine bis (trifluoromethanesulfonyl) imide (PP13-TFSI) is injected into the SELEMION CMV membrane, 0.1mol/L hydrochloric acid is added into the cathode of the second electrodialysis experimental device, the voltage is adjusted to 2V, electrodialysis is carried out for 120min, lithium and other cations can be dialyzed towards the cathode, but lithium dialysis is faster. Finally, the recovery rates of Li, K, Ca, Mg and Na are respectively 24.5%, 4.1%, 3.2%, 1.0% and 0.5%. Then adding excessive sodium carbonate to obtain solid lithium carbonate precipitate.
Example 2
Pumping a large amount of lithium-containing seawater into a bag filter to filter and remove suspended particles for later use. 15L of seawater filtered liquid is added into a first electrodialysis experimental device, wherein the first electrodialysis experimental device adopts SELEMION CSO as a divalent ion separation membrane, and Na in the seawater accounts for 10500ppm, Mg in the seawater accounts for 1350ppm, Ca in the seawater accounts for 400ppm, K in the seawater accounts for 380ppm, and Li in the seawater accounts for 170 ppb. The voltage was adjusted to 3V and after 5h of electrodialysis, 3.8L of lithium-containing concentrated solution was collected at the cathode, which contained 26140ppm of Na, 68ppm of Mg, 44ppm of Ca, 1013ppm of K and 340ppb of Li. And adding 3.8L of lithium-containing concentrated solution into the anode of an electrodialysis experiment device II, wherein a SELEMION CMV membrane is used as an electrodialysis membrane of the electrodialysis experiment device II, an ionic liquid N-methyl-N-propylpiperidine bis (trifluoromethanesulfonyl) imide (PP13-TFSI) is injected into the SELEMION CMV membrane, 0.1mol/L hydrochloric acid is added into the cathode of the electrodialysis experiment device, the voltage is adjusted to 2V, electrodialysis is carried out for 180min, lithium and other cations can be dialyzed towards the cathode, but lithium dialysis is faster. Finally, the recovery rates of Li, K, Ca, Mg and Na are 31.7%, 5.3%, 4.1%, 1.3% and 0.8%, respectively. Then adding excessive sodium carbonate to obtain solid lithium carbonate precipitate.
Example 3
Pumping a large amount of lithium-containing seawater into a bag filter to filter and remove suspended particles for later use. 15L of the filtered solution is added into a first electrodialysis experimental device, wherein the first electrodialysis experimental device adopts SELEMION CSO as a divalent ion separation membrane, and Na in seawater is 10500ppm, Mg is 1350ppm, Ca is 400ppm, K is 380ppm and Li is 170 ppb. The voltage was adjusted to 3V, and after 5h of electrodialysis, 3.8L of lithium-containing concentrated solution was collected at the cathode, which contained 26140ppm of Na, 68ppm of Mg, 44ppm of Ca, 1013ppm of K, and 340ppb of Li. And adding 3.8L of lithium-containing concentrated solution into the anode of a second electrodialysis experimental device, wherein the second electrodialysis experimental device takes a SELEMION CMV membrane as an electrodialysis membrane, an ionic liquid N-methyl-N-propylpiperidine bis (trifluoromethanesulfonyl) imide (PP13-TFSI) is injected into the SELEMION CMV membrane, 0.1mol/L hydrochloric acid is added into the cathode of the second electrodialysis experimental device, the voltage is adjusted to 2V, and electrodialysis is carried out for 240min, so that lithium and other cations can be dialyzed towards the cathode, but lithium dialysis is faster. Finally, the recovery rates of Li, K, Ca, Mg and Na are respectively 40.6%, 6.7%, 5.8%, 1.8% and 1.1%. Then adding excessive sodium carbonate to obtain solid lithium carbonate precipitate.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solutions of the present invention and not for limiting the same, and although the present invention is described in detail with reference to the preferred embodiments, those of ordinary skill in the art should understand that: modifications and equivalents may be made to the invention without departing from the spirit and scope of the invention.
Claims (9)
1. A method for recovering lithium from seawater, comprising the steps of:
a) filtering the lithium-containing seawater to remove suspended matters to obtain filtered liquid;
b) adding the filtered solution into a first electrodialysis experimental device, performing electrodialysis to remove divalent ions, and concentrating to obtain a lithium-containing concentrated solution;
c) injecting ionic liquid into an electrodialysis membrane in an electrodialysis experimental device II;
d) hydrochloric acid is introduced into the cathode of the electrodialysis experiment device II, the concentrated solution is introduced into the anode of the electrodialysis experiment device II, and electrodialysis is performed to obtain a lithium-containing solution;
e) adding carbonate into the lithium-containing solution to precipitate lithium, and performing solid-liquid separation to obtain a lithium carbonate solid.
2. The method of claim 1, wherein the method further comprises the steps of: the solid-liquid separation equipment is one or more of a filter press, a sedimentation centrifuge, a sedimentation thickener, a floating ball clarifier, a bag filter or a separation column.
3. The method of claim 1, wherein the method further comprises the steps of: in the step b), the first electrodialysis experimental device adopts SELEMION CSO as a separation membrane of divalent ions.
4. The method of claim 1, wherein the method further comprises the steps of: in step b), the electrodialysis has a dialysis voltage of 3V and a dialysis time of about 5 hours.
5. The method of claim 1, wherein the method further comprises the steps of: in step c), the ionic liquid is N-methyl-N-propylpiperidine bis (trifluoromethanesulfonyl) imide (PP 13-TFSI).
6. The method of claim 1, wherein the method further comprises the steps of: in the step c), the electrodialysis membrane of the electrodialysis experimental device II is a SELEMION CMV membrane.
7. The method of claim 1, wherein the method further comprises the steps of: in the step d), the concentration of the hydrochloric acid is 0.1mol/L, the dialysis voltage of the electrodialysis is 2V, and the dialysis time is about 120 minutes.
8. The method of claim 1, wherein the method further comprises the steps of: in step d), the recovery rate of lithium from the lithium-containing solution is 24.5-40.6%.
9. The method of claim 1, wherein the method further comprises the steps of: in step e), the carbonate is sodium carbonate.
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- 2022-01-17 CN CN202210050730.7A patent/CN114380431A/en active Pending
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| JP2010029797A (en) * | 2008-07-29 | 2010-02-12 | Japan Atomic Energy Agency | Lithium isotope separation and condensation method, apparatus, measure, lithium ion selective permeation membrane, and lithium isotope concentrate |
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