CN115717200A - Selective lithium extraction method from levextrel resin - Google Patents
Selective lithium extraction method from levextrel resin Download PDFInfo
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- CN115717200A CN115717200A CN202211474772.XA CN202211474772A CN115717200A CN 115717200 A CN115717200 A CN 115717200A CN 202211474772 A CN202211474772 A CN 202211474772A CN 115717200 A CN115717200 A CN 115717200A
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- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims abstract description 125
- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 125
- 239000011347 resin Substances 0.000 title claims abstract description 75
- 229920005989 resin Polymers 0.000 title claims abstract description 75
- 238000000605 extraction Methods 0.000 title claims abstract description 64
- 238000000034 method Methods 0.000 claims abstract description 53
- 239000011148 porous material Substances 0.000 claims abstract description 15
- 238000001914 filtration Methods 0.000 claims abstract description 14
- 238000002156 mixing Methods 0.000 claims abstract description 14
- 238000003756 stirring Methods 0.000 claims abstract description 10
- 239000000243 solution Substances 0.000 claims description 44
- 238000001179 sorption measurement Methods 0.000 claims description 28
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 12
- 238000003795 desorption Methods 0.000 claims description 12
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 claims description 11
- 239000004793 Polystyrene Substances 0.000 claims description 11
- 239000012267 brine Substances 0.000 claims description 11
- 229910001416 lithium ion Inorganic materials 0.000 claims description 11
- 229920002223 polystyrene Polymers 0.000 claims description 11
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 claims description 11
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 10
- 238000002386 leaching Methods 0.000 claims description 9
- 239000007788 liquid Substances 0.000 claims description 9
- 239000003960 organic solvent Substances 0.000 claims description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 8
- 239000000463 material Substances 0.000 claims description 7
- 238000005406 washing Methods 0.000 claims description 7
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- 239000003245 coal Substances 0.000 claims description 6
- 238000001556 precipitation Methods 0.000 claims description 6
- 239000013535 sea water Substances 0.000 claims description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 5
- 239000002253 acid Substances 0.000 claims description 5
- 239000012452 mother liquor Substances 0.000 claims description 5
- 239000001913 cellulose Substances 0.000 claims description 4
- 229920002678 cellulose Polymers 0.000 claims description 4
- 150000002148 esters Chemical class 0.000 claims description 4
- 239000006260 foam Substances 0.000 claims description 4
- 239000003672 gas field water Substances 0.000 claims description 4
- 239000004033 plastic Substances 0.000 claims description 4
- 229920003053 polystyrene-divinylbenzene Polymers 0.000 claims description 4
- SCYULBFZEHDVBN-UHFFFAOYSA-N 1,1-Dichloroethane Chemical compound CC(Cl)Cl SCYULBFZEHDVBN-UHFFFAOYSA-N 0.000 claims description 3
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 claims description 3
- -1 polytetrafluoroethylene Polymers 0.000 claims description 3
- 238000009270 solid waste treatment Methods 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- UOCLXMDMGBRAIB-UHFFFAOYSA-N 1,1,1-trichloroethane Chemical compound CC(Cl)(Cl)Cl UOCLXMDMGBRAIB-UHFFFAOYSA-N 0.000 claims description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 2
- 229910021389 graphene Inorganic materials 0.000 claims description 2
- 229910002804 graphite Inorganic materials 0.000 claims description 2
- 239000010439 graphite Substances 0.000 claims description 2
- 229910017604 nitric acid Inorganic materials 0.000 claims description 2
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 2
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 2
- 238000004064 recycling Methods 0.000 claims description 2
- 239000000741 silica gel Substances 0.000 claims description 2
- 229910002027 silica gel Inorganic materials 0.000 claims description 2
- FVBUAEGBCNSCDD-UHFFFAOYSA-N silicide(4-) Chemical class [Si-4] FVBUAEGBCNSCDD-UHFFFAOYSA-N 0.000 claims description 2
- 238000000926 separation method Methods 0.000 abstract description 4
- 238000001035 drying Methods 0.000 abstract description 3
- 230000000694 effects Effects 0.000 abstract description 2
- 229910000510 noble metal Inorganic materials 0.000 abstract 1
- 239000002904 solvent Substances 0.000 abstract 1
- 238000010025 steaming Methods 0.000 abstract 1
- 239000003463 adsorbent Substances 0.000 description 9
- 238000002360 preparation method Methods 0.000 description 6
- 230000010355 oscillation Effects 0.000 description 5
- 238000005303 weighing Methods 0.000 description 5
- 239000011521 glass Substances 0.000 description 4
- 238000002390 rotary evaporation Methods 0.000 description 4
- 239000002910 solid waste Substances 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 239000000919 ceramic Substances 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- 238000005265 energy consumption Methods 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- 241001131796 Botaurus stellaris Species 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- WAEMQWOKJMHJLA-UHFFFAOYSA-N Manganese(2+) Chemical compound [Mn+2] WAEMQWOKJMHJLA-UHFFFAOYSA-N 0.000 description 1
- LCKIEQZJEYYRIY-UHFFFAOYSA-N Titanium ion Chemical compound [Ti+4] LCKIEQZJEYYRIY-UHFFFAOYSA-N 0.000 description 1
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 description 1
- 229910052794 bromium Inorganic materials 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 description 1
- 229910052808 lithium carbonate Inorganic materials 0.000 description 1
- 229910003002 lithium salt Inorganic materials 0.000 description 1
- 159000000002 lithium salts Chemical class 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910001437 manganese ion Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 230000005622 photoelectricity Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000005185 salting out Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 229910001415 sodium ion Inorganic materials 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
- ZMBHCYHQLYEYDV-UHFFFAOYSA-N trioctylphosphine oxide Chemical compound CCCCCCCCP(=O)(CCCCCCCC)CCCCCCCC ZMBHCYHQLYEYDV-UHFFFAOYSA-N 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
- 235000020681 well water Nutrition 0.000 description 1
- 239000002349 well water Substances 0.000 description 1
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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
- 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
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- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention belongs to the technical field of rare and noble metal extraction, and discloses a method for selectively extracting lithium from extraction resin. The method comprises the steps of preparing TOPO extraction resin, absorbing lithium-containing solution and desorbing, wherein the TOPO extraction resin is prepared by uniformly mixing a porous material, TOPO and a solvent, oscillating, stirring, filtering or rotary steaming and drying; placing the lithium-containing solution and the TOPO extraction resin into a container to obtain the TOPO extraction resin for absorbing lithium; adding a desorbent into the TOPO extraction resin for absorbing lithium, mixing and filtering to obtain a pure lithium-containing solution. The method is simple, low in cost, recyclable and good in selective separation and enrichment effect on lithium.
Description
Technical Field
The invention relates to the field of lithium ion extraction, in particular to a method for selectively extracting lithium from a lithium-containing solution.
Background
Lithium is widely used in the industries of batteries, ceramics, glass, lubricants, refrigerating fluids, nuclear industry, photoelectricity and the like. With the continuous development of computers, digital cameras, mobile phones, new energy electric vehicles and the like, the battery industry has become the largest consumer field of lithium. In addition, lithium carbonate is one of effective ways for reducing energy consumption and protecting environment in the ceramic industry, and the demand of lithium is increased. At the same time, various new roles of lithium in glass are being discovered and the demand for lithium in the glass industry will remain increasing. Thus, the glass and ceramic industries have become the second largest consumer area for lithium.
Lithium resources in nature are mainly stored in lithium ores, salt lake brine and seawater. The lithium ore Dan Dili is the first adopted and developed mature method, including high-temperature high-pressure acid leaching method, high-temperature roasting method, etc., and these methods generally have the problems of high energy consumption, high equipment requirement, etc. The technological process of extracting lithium from salt lake bittern and sea water includes mainly evaporation and crystallization separation, salting out, selective semi-permeable membrane process, calcination and leaching, precipitation, solvent extraction, ion exchange, adsorption, etc. The extraction of lithium from brine is mainly limited by impurities such as magnesium, calcium, boron and the like in the brine, and the content of the impurities increases the extraction difficulty of lithium. The adsorption method has great advantages compared with other methods from the aspects of environment and economy, and particularly has more obvious advantages in extracting lithium from low-grade brine or seawater. The key point is to develop an adsorbent with excellent performance, and the adsorbent is required to have extremely high selectivity on lithium so as to eliminate the interference of a large amount of coexisting ions in brine. At present, the adsorbent is mainly inorganic adsorbent, manganese ion sieve, titanium ion sieve and aluminum salt adsorbent. However, these inorganic adsorbents have problems of high dissolution loss rate, poor cycle stability, slow adsorption rate, poor lithium selectivity, and the like.
China is the largest lithium consuming country in the world at present, accounts for more than 50% of the global consumption, and is increased year by year at a rate of 20%, and the reserve and the capacity of lithium resources are far from meeting the market demand. As the consumption of lithium increases year by year, the total amount of lithium resources from ores and salt lakes cannot meet the market's prospective demand for lithium. Because the current lithium resource is in the tension of short supply and short demand, the extraction of the lithium resource from other resources becomes a research hotspot in recent years, a new channel for developing and supplying the lithium resource is developed, and the situation of shortage of strategic metal lithium resources can be relieved to a certain extent. Gas field water, lithium precipitation mother liquor, retired lithium battery, coal-based solid waste or lithium-containing solution generated in other processes are potential lithium resources, and have attracted much attention in recent years. The lithium resources and the salt lake brine have obvious difference in composition characteristics, for example, gas field water and lithium precipitation mother liquor are mainly used for extracting lithium ions and separating sodium ions and bromine ions, lithium-containing solution generated in the processes of retired lithium batteries and coal-based solid waste treatment is often an alkaline system, and the existing inorganic adsorbent cannot be used.
Disclosure of Invention
The invention aims to solve the technical problem of providing a method for extracting lithium from leaching resin. The preparation process is simple and easy to control.
The technical scheme of the invention is that the method for selectively extracting lithium from extraction resin comprises the following steps:
(1) Preparing extraction leaching resin: uniformly mixing a porous material, TOPO and an organic solvent, wherein the mass ratio of the TOPO to the porous material is 0.5-3, the proportion of the TOPO to the organic solvent is 1;
(2) Adsorption: carrying out lithium ion adsorption on the TOPO extraction resin prepared in the step (1) and a lithium-containing solution; the extraction leaching resin: the lithium-containing solution solid-to-liquid ratio is 1;
(3) Desorbing: and (3) desorbing the extraction resin adsorbing lithium in the step (2) by using dilute acid to obtain desorption liquid.
The TOPO is tri-n-octyl phosphine oxide.
In the step (1), the solid-liquid separation method comprises the step of separating the resin from the organic solvent by a filtration or rotary evaporation method. In the dry process, the resin obtained after filtration or rotary evaporation may be dried. The temperature of rotary evaporation is preferably 60-80 ℃.
According to the method for selectively extracting lithium from leaching resin, the porous material in the step (1) is preferably selected from one or more than one of the following materials: polystyrene, polystyrene-divinyl benzene, cross-linked polystyrene ester, polytetrafluoroethylene, polyamino foam plastic, cellulose, silica gel, modified silicide, graphite, graphene and activated carbon.
Further, the porous material in the step (1) is selected from one or more of the following materials: polystyrene, polystyrene-divinyl benzene and cross-linked poly (olefine acid) ester.
According to the method for selectively extracting lithium from the extraction resin, the organic solvent in the step (1) is preferably any one or a combination of more than one of methanol, ethanol, dichloroethane, trichloroethane, cyclohexane and benzene.
According to the method for selectively extracting lithium from leaching resin, the stirring time in the step (1) is preferably 12-24 hours. Preferably, the mass ratio of TOPO to the porous material in the step (1) is 0.5-2:1.
According to the method for selectively extracting lithium from extraction resin, the proportion of the TOPO to the organic solvent is preferably 1.
According to the method for selectively extracting lithium from leaching resin, preferably, in the step (2), the lithium-containing solution is salt lake brine, underground brine, gas field water, seawater, lithium precipitation mother liquor, lithium-containing solution of lithium ore Dan Dili, lithium-containing solution generated by recycling of retired lithium batteries, lithium-containing solution generated by coal-based solid waste treatment and lithium-containing solution generated by other processes.
Preferably, in the step (2), the TOPO extraction resin prepared in the step (1) and a lithium-containing solution are subjected to lithium ion adsorption, and the mixture is contacted for 1-6 hours at room temperature to obtain the TOPO extraction resin for adsorbing lithium; after filtering and water washing, the desorption is waited. Mixing and contacting for 1-6 hours at room temperature, separating solid and liquid, washing with water, and desorbing. The adsorption may be static adsorption or dynamic adsorption.
According to the method for selectively extracting lithium from the extraction resin, the desorbent used in the step (3) is preferably one or a mixture of at least two of dilute hydrochloric acid, dilute sulfuric acid or dilute nitric acid.
Preferably, in the step (3), the desorption solution is obtained by mixing and contacting at room temperature for 2 to 4 hours during the desorption.
Has the advantages that:
the adsorbent can extract lithium from lithium-containing solution with low concentration and high concentration of impurity ions (such as lithium-containing solution such as salt lake brine, well water, seawater and the like) and alkaline system (such as lithium-containing solution generated in the process of lithium precipitation mother liquor, lithium ore or solid waste utilization).
The adsorbent has the advantages of strong medium tolerance, high ion selectivity, high adsorption rate, wide applicable solution system range, simple synthesis process and low cost, avoids the need of using expensive lithium salt as a raw material in the synthesis process of the inorganic lithium adsorption material, and reduces the synthesis cost by more than 40%.
Drawings
FIG. 1 is a schematic view of a process for preparing levextrel resin according to the present invention;
FIG. 2 is a SEM topography of the extraction resin;
FIG. 3 is an infrared image of levextrel resin.
Detailed Description
The invention is described in detail below with reference to the figures and the embodiments. The following examples are only illustrative of the present invention, and the scope of the present invention shall include the full contents of the claims, and not be limited to the following examples.
Example 1:
(1) Preparation of TOPO extraction resin
Weighing 3g of the pretreated polystyrene-based macroporous resin, mixing with 3g of TOPO and 90mL of ethanol, stirring at 25 ℃ for 12 hours, and then carrying out rotary evaporation at 70 ℃ for 2 hours by using a rotary evaporator to dry the polystyrene-based macroporous resin to obtain the TOPO-polystyrene-based levextrel resin.
(2) Adsorption process of lithium solution
50mL of lithium-containing solution (pure lithium solution, li) + The content is 300 mg/L) and 3mL of prepared TOPO extraction resin are mixed for lithium ion adsorption, and the mixture is stirred for 4 hours under the oscillation at the temperature of 25 ℃ to obtain the TOPO extraction resin for adsorbing lithium. And desorbing after filtering and washing.
(3) Desorbing:
desorbing the extracted resin adsorbing lithium with 50mL of 1mol/L hydrochloric acid, and stirring the desorbed resin for 2 hours at 25 ℃ to obtain a desorption solution.
Table 1 shows the adsorption amount of lithium in a pure lithium solution by TOPO extraction resin
Example 2:
(1) Preparation of TOPO extraction resin
Weighing 2g of the pretreated silica porous material, mixing with 3g of TOPO and 100mL of cyclohexane, stirring at 25 ℃ for 12 hours, and filtering to obtain the TOPO-silica porous material extraction resin.
(2) Adsorption process of lithium solution
50mL of lithium-containing solution (pure lithium solution, li) + The content is 300 mg/L) and 3mL of prepared TOPO extraction resin are mixed for lithium ion adsorption, and the mixture is oscillated and stirred for 4 hours at the temperature of 25 ℃ to obtain the TOPO extraction resin for adsorbing lithium. And desorbing after filtering and washing.
(3) Desorbing:
desorbing the extraction resin adsorbing the lithium by 100mL of 0.5mol/L sulfuric acid, and stirring for 2 hours by oscillation to obtain desorption liquid.
Example 3:
(1) Preparation of TOPO extraction resin
Weighing 4g of the pretreated polyamino foam plastic material, mixing with 3g of TOPO and 110mL of methanol, oscillating for 18 hours at 25 ℃, filtering, and drying in vacuum to obtain the TOPO-polyamino foam plastic material extraction resin.
(2) Adsorption process of lithium solution
50mL of lithium-containing solution (pure lithium solution, li) + The content is 300 mg/L) and 3mL of prepared TOPO extraction resin are mixed for lithium ion adsorption, and the mixture is stirred for 4 hours under the oscillation at the temperature of 25 ℃ to obtain the TOPO extraction resin for adsorbing lithium. And desorbing after filtering and washing.
(3) Desorbing:
desorbing the extraction resin adsorbed with lithium with 100mL of 0.5mol/L sulfuric acid, and shaking and mixing at room temperature for 2 hours to obtain desorption liquid.
Example 4:
(1) Preparation of TOPO extraction resin
Weighing 2g of the pretreated polystyrene macroporous resin, mixing with 3g of TOPO and 95mL of methanol, oscillating for 12 hours at 25 ℃, filtering, and performing vacuum drying at 60 ℃ to obtain the TOPO-polystyrene extraction resin.
(2) Adsorption process of lithium solution
50mL of coal-based solid waste is takenLithium-containing solution (solution containing 15% NaOH, li) + The content is 300mg/L, al 3+ The content is 1166.9mg/L, K + The content is 1685.6mg/L, na + The content is 87240mg/L, si 4+ The content is 1204 mg/L) and 3mL of prepared TOPO extraction resin are mixed for lithium ion adsorption, and the mixture is oscillated and mixed for 4 hours at the temperature of 25 ℃ to obtain the TOPO extraction resin for adsorbing lithium. And desorbing after filtering and washing.
(3) Desorbing:
desorbing the extracted resin adsorbed with lithium with 50mL of 1mol/L hydrochloric acid, and stirring under oscillation for 2 hours to obtain a desorption solution.
Table 2 shows the adsorption amount of lithium in the TOPO extraction resin in the coal-based solid waste lithium-containing solution
Example 5:
(1) Preparation of TOPO extraction resin
Weighing 2g of the pretreated cellulose porous material, mixing with 2.5g of TOPO and 80mL of dichloroethane, oscillating for 24 hours at 25 ℃, and filtering to obtain the TOPO-cellulose porous material extraction resin.
(2) Adsorption process of lithium solution
And mixing 50mL of the lithium-containing solution recovered from the retired lithium battery with 5mL of TOPO extraction resin for lithium ion adsorption, and oscillating and stirring for 4 hours at 25 ℃ to obtain the TOPO extraction resin for lithium adsorption.
(3) Desorbing:
desorbing the extraction resin adsorbed with lithium with 100mL of 0.5mol/L sulfuric acid, and stirring for 1 hour under oscillation to obtain desorption liquid.
Table 3 shows the adsorption amount of lithium in the lithium-containing solution recovered from the retired lithium battery by TOPO extraction resin
The method is simple, low in cost, recyclable and good in selective separation and enrichment effect on lithium.
Claims (10)
1. A method for selectively extracting lithium from extraction resin is characterized by comprising the following steps: the method comprises the following steps:
(1) Preparing extraction leaching resin: uniformly mixing a porous material, TOPO and an organic solvent, wherein the mass ratio of the TOPO to the porous material is 0.5-3, the proportion of the TOPO to the organic solvent is 1;
(2) Adsorption: carrying out lithium ion adsorption on the TOPO extraction resin prepared in the step (1) and a lithium-containing solution; the extraction resin: the lithium-containing solution solid-to-liquid ratio is 1;
(3) Desorbing: and (3) desorbing the extraction resin adsorbing lithium in the step (2) by using dilute acid to obtain desorption liquid.
2. The method for selectively extracting lithium from extraction resin according to claim 1, wherein the method comprises the following steps: the porous material in the step (1) is selected from one or more than one of the following materials: polystyrene, polystyrene-divinyl benzene, cross-linked polystyrene ester, polytetrafluoroethylene, polyamino foam plastic, cellulose, silica gel, modified silicide, graphite, graphene and activated carbon.
3. The method for selectively extracting lithium from extraction resin according to claim 2, wherein the method comprises the following steps: the porous material in the step (1) is selected from one or more than one of the following materials: polystyrene, polystyrene-divinyl benzene and cross-linked poly (olefine acid) ester.
4. The method for selectively extracting lithium from levextrel resin according to claim 1, characterized in that: the organic solvent in the step (1) is any one or the combination of more than one of methanol, ethanol, dichloroethane, trichloroethane, cyclohexane and benzene.
5. The method for selectively extracting lithium from extraction resin according to claim 1, wherein the method comprises the following steps: the stirring time in the step (1) is 12-24h; the mass ratio of the TOPO to the porous material in the step (1) is 0.5-2:1.
6. The method for selectively extracting lithium from extraction resin according to claim 1, wherein the method comprises the following steps: the proportion of the TOPO to the organic solvent is 1.
7. The method for selectively extracting lithium from extraction resin according to claim 1, wherein the method comprises the following steps: in the step (2), the lithium-containing solution is salt lake brine, underground brine, gas field water, seawater, lithium precipitation mother liquor, lithium-containing solution of lithium ore Dan Dili, lithium-containing solution generated by recycling retired lithium batteries, lithium-containing solution generated by coal-based solid waste treatment and lithium-containing solution generated by other processes.
8. The method for selectively extracting lithium from extraction resin according to claim 1, wherein the method comprises the following steps: in the step (2), the TOPO extraction resin prepared in the step (1) and a lithium-containing solution are subjected to lithium ion adsorption, and are mixed and contacted for 1-6 hours at room temperature to obtain the TOPO extraction resin for adsorbing lithium; after filtering and water washing, the desorption is waited.
9. The method for selectively extracting lithium from extraction resin according to claim 1, wherein the method comprises the following steps: the desorbent used in the step (3) is one or a mixture of at least two of dilute hydrochloric acid, dilute sulfuric acid or dilute nitric acid.
10. The method for selectively extracting lithium from extraction resin according to claim 1, wherein the method comprises the following steps: in the step (3), during analysis, the desorption solution is obtained by mixing and contacting for 2-4 hours at room temperature.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1936034A (en) * | 2006-09-15 | 2007-03-28 | 中国科学院长春应用化学研究所 | Method for preparing embedding ion liquid and neutral phosphor (phosphine) extractant composite material and its use |
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