CN105948081B - A kind of method that utilization hydridization electric capacity extracts lithium in bittern - Google Patents
A kind of method that utilization hydridization electric capacity extracts lithium in bittern Download PDFInfo
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- CN105948081B CN105948081B CN201610280822.9A CN201610280822A CN105948081B CN 105948081 B CN105948081 B CN 105948081B CN 201610280822 A CN201610280822 A CN 201610280822A CN 105948081 B CN105948081 B CN 105948081B
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- lithium
- activated carbon
- lithium ion
- bittern
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- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 30
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims abstract description 29
- 238000000034 method Methods 0.000 title claims abstract description 27
- 241001131796 Botaurus stellaris Species 0.000 title claims abstract description 18
- 239000000284 extract Substances 0.000 title claims abstract description 11
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 31
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 claims abstract description 24
- 229910001416 lithium ion Inorganic materials 0.000 claims abstract description 24
- 239000011572 manganese Substances 0.000 claims abstract description 15
- 239000000463 material Substances 0.000 claims abstract description 6
- 239000003011 anion exchange membrane Substances 0.000 claims abstract description 5
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical class C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 14
- 239000011230 binding agent Substances 0.000 claims description 11
- 238000010521 absorption reaction Methods 0.000 claims description 10
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 claims description 9
- 239000002002 slurry Substances 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 229910002097 Lithium manganese(III,IV) oxide Inorganic materials 0.000 claims description 5
- 239000006230 acetylene black Substances 0.000 claims description 5
- 239000003990 capacitor Substances 0.000 claims description 5
- 239000004926 polymethyl methacrylate Substances 0.000 claims description 5
- 239000011521 glass Substances 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 4
- 229920005479 Lucite® Polymers 0.000 claims description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 3
- 125000000129 anionic group Chemical group 0.000 claims description 3
- 239000012528 membrane Substances 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 239000000741 silica gel Substances 0.000 claims description 3
- 229910002027 silica gel Inorganic materials 0.000 claims description 3
- 125000006850 spacer group Chemical group 0.000 claims description 3
- 239000002250 absorbent Substances 0.000 claims description 2
- 230000002745 absorbent Effects 0.000 claims description 2
- 239000003610 charcoal Substances 0.000 claims description 2
- 238000004891 communication Methods 0.000 claims description 2
- 238000002425 crystallisation Methods 0.000 claims description 2
- 230000008025 crystallization Effects 0.000 claims description 2
- 229910003002 lithium salt Inorganic materials 0.000 claims description 2
- 159000000002 lithium salts Chemical class 0.000 claims description 2
- 229920003229 poly(methyl methacrylate) Polymers 0.000 claims description 2
- 230000007306 turnover Effects 0.000 claims description 2
- 239000011248 coating agent Substances 0.000 claims 2
- 238000000576 coating method Methods 0.000 claims 2
- 239000000203 mixture Substances 0.000 claims 1
- VASIZKWUTCETSD-UHFFFAOYSA-N oxomanganese Chemical compound [Mn]=O VASIZKWUTCETSD-UHFFFAOYSA-N 0.000 claims 1
- 150000002500 ions Chemical class 0.000 abstract description 7
- 239000003463 adsorbent Substances 0.000 abstract description 6
- 238000001179 sorption measurement Methods 0.000 abstract description 6
- JLVVSXFLKOJNIY-UHFFFAOYSA-N Magnesium ion Chemical compound [Mg+2] JLVVSXFLKOJNIY-UHFFFAOYSA-N 0.000 abstract description 5
- 238000000605 extraction Methods 0.000 abstract description 5
- 229910001425 magnesium ion Inorganic materials 0.000 abstract description 5
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 abstract description 4
- 239000002253 acid Substances 0.000 abstract description 4
- 239000011777 magnesium Substances 0.000 abstract description 4
- 229910052748 manganese Inorganic materials 0.000 abstract description 4
- 230000008439 repair process Effects 0.000 abstract description 3
- 230000007420 reactivation Effects 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 9
- 239000011149 active material Substances 0.000 description 7
- 229910002804 graphite Inorganic materials 0.000 description 7
- 239000010439 graphite Substances 0.000 description 7
- 238000005516 engineering process Methods 0.000 description 4
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical compound [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 description 4
- 150000003839 salts Chemical class 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 238000006479 redox reaction Methods 0.000 description 3
- 229910009343 Li1.33 Mn1.67 O4 Inorganic materials 0.000 description 2
- 238000003795 desorption Methods 0.000 description 2
- 230000005684 electric field Effects 0.000 description 2
- -1 includes seawater Chemical compound 0.000 description 2
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 description 2
- 229910052808 lithium carbonate Inorganic materials 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 2
- 239000004810 polytetrafluoroethylene Substances 0.000 description 2
- 239000013535 sea water Substances 0.000 description 2
- 238000007581 slurry coating method Methods 0.000 description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- 241001466077 Salina Species 0.000 description 1
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 1
- 241001062472 Stokellia anisodon Species 0.000 description 1
- 150000001408 amides Chemical class 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000012267 brine Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- GCICAPWZNUIIDV-UHFFFAOYSA-N lithium magnesium Chemical compound [Li].[Mg] GCICAPWZNUIIDV-UHFFFAOYSA-N 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 description 1
- 238000013112 stability test Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D15/00—Lithium compounds
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Battery Electrode And Active Subsutance (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
A kind of method that utilization hydridization electric capacity extracts lithium in bittern, belongs to energy and material and technical field.This method is based on a pole in hydridization capacitance principle, capacitance module and uses Mn oxide, and another pole uses the activated carbon with anion-exchange membrane, and control is applied to the voltage on electrode, and realization extracts lithium ion in the environment of salt lake bittern high Mg/Li ratio.Extract during lithium ion, the interference of magnesium ion in bittern can be effectively excluded on the premise of not being introduced into other ions.Only need to control applied voltage just can realize enrichment and the adsorbent reactivation of lithium ion, processing procedure is easy, realize the simple and effective extraction of lithium ion.This method single adsorptions amount can reach 3mg/g, and avoid the molten damage of manganese caused by the use of strong acid in regenerative process, improve the stability of adsorbent, and obvious decay is had no after circulate operation 50 times.The extracting method of the lithium ion has wide prospects for commercial application.
Description
Technical field
The present invention relates to a kind of method that utilization hydridization electric capacity extracts lithium in bittern, belong to energy and material and technical field.
Background technology
Lithium and its compound have in terms of motor-car and energy storage industry, metal smelt and its manufacturing industry, aerospace industry
There is important purposes, someone claims lithium to be " the energy source element of 21 century ", it is estimated that the year two thousand twenty lithium demand is up to 320,000 tons.
The source of lithium mainly includes seawater, ore and salt lake bittern.Contain about 2.5 × 10 in Global Seawater altogether14Kilogram
Lithium, but its mean concentration is only 0.17mg/L, mainly takes absorption method to extract, it is less efficient;Ore carry lithium technology more into
Ripe, but if being produced using the technology, China is needed for a long time from Australian import lithium ore, and cost is higher, in addition, entirely
Ball also faces the problem of lithium ore resource is progressively exhausted.Therefore, producing lithium carbonate using salt lake bittern will turn into inevitable.
China is salt lake bittern lithium resource big country, and wherein Caidamu Basin saline lake lithium resource accounts for the whole nation and verified lithium resource
94.1%, the reserves verified at present in basin is 18,000,000 tons, is ranked first in the world;Be distributed mainly on Cha Er Han,
In five salt lakes such as one inner level ground, West Taijinar, East Taijinaier, big bavin denier.In five salt lakes of the above, the general content of lithium chloride
In 2-6 g/L, up to 8 more than g/L.For the salt lake bittern mainly salt pan evaporation used external at present.But
This method is only applicable to the relatively low bittern of Mg/Li ratio and extremely time-consuming, poorly efficient.Another method is that FMC Corp. of the U.S. is directed to
The selective absorption method that Argentinian Hombre Muerto salt lakes are proposed.This method is directed to the characteristics of bittern impurity is less, utilizes tool
There is the adsorbent of ion sieve effect(Such as Mn oxide)Lithium chloride and lithium carbonate are directly extracted from bittern, the technique has production
The characteristics of efficiency high, low production cost, represent the developing direction that following salt lake bittern carries lithium.But ion sieve still have with
Lower problem:1st, there is the molten damage of manganese during the preparation of ion sieve adsorbant and its de- lithium.2nd, ion sieve adsorbent reactivation process is needed
Strong acid is used, is not an environment-friendly process.3rd, easily disturbed in adsorption process by magnesium ion.
Therefore, the redox reaction based on lithium ion Yu lithium active material, constructs a kind of hydridization capacitor, can be effective
Exclude brine lake in magnesium ion interference, efficiently reclaim lithium ion.Distinguish over existing lithium ion recovery technology a variety of scarce
Fall into, the program has extremely strong industrial applications prospect.
The content of the invention
In order to overcome the deficiencies in the prior art, the present invention provides a kind of utilization hydridization electric capacity and extracts lithium in bittern
Method, this method is by hydridization capacitor principle, to applying alive control, to realize absorption and the desorption to lithium ion, and
And can effectively exclude the interference of magnesium ion in water body.
The technical solution adopted by the present invention is:
(1)By Mn oxide, binding agent, conductive black according to 8-10:1:1 ratio is mixed, and adds N, N- dimethyl second
Acid amides, is made slurry;Mn oxide is LiMn2O4、Li1.33Mn1.67O4Or Li1.6Mn1.6O4Through 0.5M HCl soak 12 hours,
Filter and dried product.
(2)By absorbent charcoal material, binding agent, conductive black according to 8-10:1:1 ratio uniform mixing, adds N, N- bis-
Methylacetamide, is made slurry;
Above-mentioned slurry is respectively coated in collector(Graphite cake)On be made electrode, after drying, add on activated carbon electrodes
Plus anion-exchange membrane;
(3)The activated carbon electrodes with anionic membrane and manganese oxide electrode are fixed on lucite spacer respectively,
Poly (methyl methacrylate) plate upper left side remains for the duct of liquid turnover with lower right in advance, and being placed in the middle of two pieces of lucite spacers prevents
The silica gel pad of two electrode contacts and liquid communication space is reserved, will be fixed after two pieces of glass plates alignment;
(4)Bittern is passed through in the module, and using hydridization capacitance principle, the choosing to lithium ion is realized by applying negative voltage
Selecting property is adsorbed.After the completion of absorption, deionized water is passed through in the module, while by applying the lithium that positive voltage makes absorption on electrode
Ion is desorbed the formation lithium solution in deionized water, then the lithium-containing solution is concentrated, and evaporative crystallization is so as to obtain pure lithium salts.
The binding agent is selected from Kynoar, polytetrafluoroethylene (PTFE) or polyvinyl alcohol.
The conductive black is acetylene black, CNT.
The activated carbon is YP-50, active carbon with high specific surface area.
The method that the hydridization capacitance principle extracts lithium is:Lithium active material has redox anti-with the lithium ion in solution
Should, by applying negative voltage to active material electrode, the lithium ion in solution can be made to enter in lithium active material and magnesium
Ion can not enter, and at the same time apply positive voltage to the activated carbon electrodes with anionic membrane, due to the effect meeting of electric field force
Make the Anion-adsorption in solution in the surface of activated carbon so that electric charge realizes the selective absorption of lithium ion in balance solution.Inhale
After the completion of attached, deionized water is passed through in the module, positive voltage is applied to active material electrode, and due to redox reaction, lithium is lived
Property material can release lithium ion into solution, and activated carbon electrodes make the lithium ion of desorption due to the presence of anion-exchange membrane
Activated carbon surface can not be adsorbed onto, at the same time to activated carbon electrodes apply negative electricity, be adsorbed in activated carbon surface it is negatively charged from
Son is released in solution due to the effect of electric field force, and then realizes the extraction of lithium ion.
The negative voltage be to active material electrode apply relative to activated carbon electrodes negative voltage -0.8V~-
4.5V。
The positive voltage is to apply positive voltage 0.8V~4.5V relative to activated carbon electrodes to active material electrode.
This practicality invention beneficial effect be:This method is based on hydridization capacitance principle, can be effectively special from high Mg/Li ratio
In the salina levied, selective extraction goes out lithium ion.By the material with lithium ion with redox reaction with carrying anion
Hydridization capacitor is made in the activated carbon of film, by using hydridization capacitance principle, can effectively extract lithium ion, single adsorptions amount
3mg/g can be reached, and avoids the molten damage of manganese caused by the use of strong acid in regenerative process, the steady of adsorbent is improved
It is qualitative, have no obvious decay after circulate operation 50 times.In addition, compared to the intermittently operated of traditional adsorption method, this method can
Continuous operation, extraction process is simple to operate, is conducive to heavy industrialization application.In a word, compared to conventional method, this method shows
Go out big advantage.
Brief description of the drawings
Fig. 1 is capacitor module.
Fig. 2 is lithium ion selective absorption and stability test figure.
Embodiment
Below by example, the invention will be further described
Embodiment 1
By Mn oxide LiMn2O4With conductive black acetylene black, binding agent Kynoar according to mass ratio 8:1:1 mixing
Uniformly, add DMA and slurry is made is coated on graphite cake and electrode is made.Equally by activated carbon(YP-50)With
Conductive black, binding agent are according to mass ratio 8:1:1 is well mixed, and addition DMA is made slurry and is coated on graphite
Electrode is made on plate.
Embodiment 2
By Mn oxide Li1.33Mn1.67O4With conductive black acetylene black, binding agent Kynoar according to mass ratio 9:1:1
It is well mixed, add DMA and slurry is made is coated on graphite cake electrode is made.Equally by activated carbon(YP-
50)With conductive black, binding agent according to mass ratio 9:1:1 is well mixed, and adds DMA and slurry coating is made
In electrode is made on graphite cake.
Embodiment 3
By Mn oxide Li1.6Mn1.6O4With conductive black acetylene black, binding agent Kynoar according to mass ratio 10:1:1
It is well mixed, add DMA and slurry is made is coated on graphite cake electrode is made.Equally by activated carbon(YP-
50)With conductive black, binding agent according to mass ratio 10:1:1 is well mixed, and adds DMA and slurry coating is made
In electrode is made on graphite cake.
Electrode in embodiment 1 is placed in 80 DEG C of baking ovens, 12h is dried.By dried electrode, 5cm × 6cm is cut into
Size, and activated carbon electrodes end is covered into one layer of anion-exchange membrane, add two electrode assemblings after silica gel pad into module(See
Fig. 1).Under 25 degree of water bath conditions of constant temperature, with 5 ml/min water circulation speed, pass sequentially through 50ml and contain lithium ion and magnesium
The mixed solution and deionized water of ion, apply 1.6V voltages to the electrode of module two, test the selective extraction of the module successively
The ability of lithium.As can be seen from Figure 2, single adsorptions amount can reach 3mg/g, and avoid the use of strong acid in regenerative process and lead
The molten damage of the manganese of cause, improves the stability of adsorbent, and obvious decay is had no after circulate operation 50 times.This method illustrates good
Good selectivity, with stable cycle performance.In a word, this method selective effectively from magnesium lithium mixed solution can extract lithium
Ion, with good industrial applications prospect.
Claims (1)
1. a kind of method that utilization hydridization electric capacity extracts lithium in bittern, it is characterised in that comprise the following steps:
(1)By Mn oxide LiMn2O4, binding agent Kynoar, conductive black acetylene black is according to mass ratio 8:1:1 ratio
Mix, add DMA, slurry is made, manganese oxide electrode is made in coating on a current collector;
(2)By absorbent charcoal material YP-50, binding agent, conductive black according to mass ratio 8:1:1 ratio uniform mixing, adds N,
N- dimethyl acetamides, are made slurry, and activated carbon electrodes are made in coating on a current collector;And added on activated carbon electrodes it is cloudy from
Proton exchange, is made the activated carbon electrodes with anion-exchange membrane;
(3)Assemble capacitor module:The activated carbon electrodes with anionic membrane and manganese oxide electrode are fixed on organic glass respectively
On glass dividing plate, remain for the duct of liquid turnover in advance on poly (methyl methacrylate) plate upper left side and lower right, in two pieces of lucite spacers
Centre places the silica gel pad for preventing two electrode contacts and reserves liquid communication space, will be fixed after two pieces of glass plate alignment;
(4)Bittern is passed through in the module, and using hydridization capacitance principle, the selectivity to lithium ion is realized by applying negative voltage
Absorption;After the completion of absorption, deionized water is passed through in the module, while by applying the lithium ion that positive voltage makes absorption on electrode
It is desorbed in deionized water and forms lithium-containing solution, then the lithium-containing solution is concentrated, evaporative crystallization is so as to obtain pure lithium salts;It is described
Negative voltage is to apply negative voltage -0.8V~-4.5V relative to activated carbon electrodes to manganese oxide electrode;Positive voltage is to manganese oxygen
Compound electrode applies positive voltage 0.8V~4.5V relative to activated carbon electrodes;
The Mn oxide LiMn2O4For LiMn2O412 hours are soaked through 0.5M HCl, filtered and dried product.
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CN109078360B (en) * | 2018-09-11 | 2021-04-02 | 中国科学院青海盐湖研究所 | Sectioning type adsorption and desorption device and application thereof |
CN109179589A (en) * | 2018-09-20 | 2019-01-11 | 同济大学 | The preparation method of carbon coating vanadium phosphate sodium electrode material and its application in hydridization capacitive deionization technology |
CN109607711A (en) * | 2019-01-30 | 2019-04-12 | 东莞理工学院 | A kind of hydridization capacitive deionization desalination module and desalination process |
CN113293285B (en) * | 2021-05-21 | 2022-04-08 | 江苏中南锂业有限公司 | Preparation method of modified lithium extraction electrode with fast ion conductor |
CN113293289B (en) * | 2021-05-21 | 2022-04-12 | 江苏中南锂业有限公司 | Preparation method of hydrophilic lithium extraction electrode |
CN113401944A (en) * | 2021-06-18 | 2021-09-17 | 华中师范大学 | λ-MnO2Nanorod electrode, preparation method and application of nanorod electrode in extraction of lithium in brine |
CN115522071B (en) * | 2022-10-13 | 2023-09-26 | 华东理工大学 | Apparatus and method for activating electrodes |
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