CN109609977A - The electrode structure and its manufacturing method of extraction lithium and application - Google Patents
The electrode structure and its manufacturing method of extraction lithium and application Download PDFInfo
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- CN109609977A CN109609977A CN201910126639.7A CN201910126639A CN109609977A CN 109609977 A CN109609977 A CN 109609977A CN 201910126639 A CN201910126639 A CN 201910126639A CN 109609977 A CN109609977 A CN 109609977A
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
- C25C7/00—Constructional parts, or assemblies thereof, of cells; Servicing or operating of cells
- C25C7/02—Electrodes; Connections thereof
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
- C25C1/00—Electrolytic production, recovery or refining of metals by electrolysis of solutions
- C25C1/02—Electrolytic production, recovery or refining of metals by electrolysis of solutions of light metals
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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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Abstract
The present invention relates to a kind of electrode structure for extracting lithium and its manufacturing method and application, electrode structure includes collector, and collector includes clamping energization section and active section, and the surface of active section is successively coated with ion sieve coating and selectivity through film from inside to outside；Selectivity uses lithium ion battery film or monovalent cation exchange membrane through film.Electrode structure of the invention is placed in salt lake bittern, it is equipped with the first supporting electrode, application voltage is embedded into ion sieve coating after so that the lithium ion in salt lake bittern is penetrated film by selectivity, electrode structure after obtaining embedding lithium, electrode structure after embedding lithium is placed in supporting electrolyte solution, it is equipped with the second supporting electrode, applying voltage makes embedded ion sieve the lithium ion deintercalation in coating, entered in supporting electrolyte solution by selectivity through after film, realize the separation and extraction to lithium, the present invention, which has the brine of high Mg/Li ratio, preferably proposes lithium effect, it is low to inhale magnesium amount, process of intercalation can be again returned to after the de- lithium of electrode structure to recycle.
Description
Technical field
The invention belongs to chemical metallurgy technical fields, and in particular to it is a kind of extract lithium electrode structure and its manufacturing method and
Using.
Background technique
Lithium metal is a kind of argenteous light metal, and tool has been widely used, and such as prepares lithium battery.With the application neck of lithium
Domain constantly expands, number of applications quicklys increase, and needs to find more vast lithium resource, other than traditional lithium mine, brine is also
The important sources of lithium resource, it is very that brine, which belongs in inland brine lake evaporation residual deposit, which does not evaporate the dry mineral products of liquid containing lithium,
Important lithium resource.In order to extract the lithium in brine, especially salt lake bittern, the method for use mainly has solvent extraction, sinks
The technologies such as shallow lake method, carbonizatin method, ion exchange adsorption.These methods have preferable extraction effect for the brine of low Mg/Li ratio,
But the content of magnesium in many salt lake bitterns is big, and Mg/Li ratio is very high, and Mg/Li ratio is even as high as 40 or more, the extraction for wherein lithium
Just very difficult, existing method is difficult to reach preferable extraction effect.
Also there are relevant technical research, such as CN105506310A in the prior art, discloses one kind and mentioned from brine containing lithium
The method for taking lithium, this method are utilized with the lithium ion in the active adsorbent absorption brine containing lithium of embedding lithium, then according to lithium ion
Battery charging principle, is electrolysed precipitating metal lithium under particular voltage range, and this method compares the existing precipitation method, absorption method, extraction
It is short to follow the example of equal conventional processing routes, it is at low cost, but method, for the brine of high Mg/Li ratio, suction magnesium amount is still higher, influences lithium
Separation and Extraction.
Summary of the invention
For the above-mentioned deficiency of the prior art, the technical problem to be solved in the present invention is to provide a kind of electrode knots for extracting lithium
Structure and its manufacturing method and application, the brine suitable for high Mg/Li ratio mention lithium, when avoiding extracting lithium from the brine of high Mg/Li ratio
The problem of inhaling magnesium amount height, influencing the separation and Extraction efficiency of lithium, acquirement effectively mentions lithium from the brine of high Mg/Li ratio, and it is low to inhale magnesium amount
Effect.
In order to solve the above technical problems, the present invention adopts the following technical scheme:
Extract the electrode structure of lithium, including collector；The collector includes clamping energization section and active section, the active section
Surface is successively coated with ion sieve coating and selectivity through film from inside to outside.
Above-mentioned technical proposal is further improved, the selectivity is handed over through film using lithium ion battery film or monovalent cation
Change film.
Further, the constituent of the ion sieve coating includes ion sieve raw material, helps conductive agent and bonding agent.
Preferably, the ion sieve raw material use ferric phosphate, described to help conductive agent using acetylene black, and the bonding agent is adopted
Use Kynoar.
Further, in the component of the ion sieve coating, ion sieve raw material, the mass ratio for helping conductive agent and bonding agent
For 13~16:1:1.
Further, the material of the collector uses nickel or nickel foam.
The invention further relates to the manufacturing methods of the electrode structure of said extracted lithium, include the following steps:
1) by powdered ion sieve raw material, help conductive agent and bonding agent to be uniformly mixed, by after mixing powder be added dispersion
Slurry is worn into agent, and slurry is attached to the work section surface of collector, is obtained after vacuum drying with ion sieve coating
Electrode；
2) it is coated outside the ion sieve coating of the electrode with ion sieve coating using selectivity through film, obtains the extraction
The electrode structure of lithium.
Further, vacuum drying described in step 1) for dry 10 in 100~130 DEG C of heat preservations in a vacuum drying oven~
12 hours；The dispersing agent uses N-Methyl pyrrolidone；The method of cladding described in step 2 is the mode using hot pressing side
It is sealed fixation.
The invention further relates to the applications of the electrode structure of said extracted lithium, include the following steps:
(1) separation of lithium；It using the electrode structure for extracting lithium, is placed in salt lake bittern, is equipped with the first supporting electrode, apply
Voltage is embedded into ion sieve coating, the electricity after obtaining embedding lithium after so that the lithium ion in salt lake bittern is penetrated film by selectivity
Pole structure realizes the separation to Lithium from Salt Lake Brine；
(2) extraction of lithium；Electrode structure after embedding lithium is placed in supporting electrolyte solution, and is equipped with the second supporting electrode, is applied
Making alive, makes the lithium ion deintercalation in embedded ion sieve coating, is entered in supporting electrolyte solution by selectivity through after film,
Realize the extraction to lithium.
Further, the electrode structure of lithium is extracted described in step (1) as cathode, the first supporting electrode as anode,
The material of first supporting electrode uses graphite；Apply 1.0~1.4V of voltage and maintains 12~16 hours；
Electrode structure after embedding lithium described in step (2) as anode, the second supporting electrode as cathode, the second supporting electrode
Material uses iron；The supporting electrolyte solution uses sodium chloride solution；Apply 0.6~1.0V of voltage and maintenance 12~16 is small
When.
Compared with prior art, the invention has the following beneficial effects:
1, selectivity and higher deintercalation capacity of the electrode structure provided by the invention to lithium ion with height, passes through selectivity
It is low to magnesium ion adsorbance through the setting of film, have to the brine of high Mg/Li ratio and preferably propose lithium effect, has extended cycle life.
2, using electrode structure provided by the invention carry out lithium extraction, have process flow it is short, it is easy to operate, be produced into
This feature low, easy to industrialized production.
3, electrode structure of the invention can again return to process of intercalation after de- lithium and recycle.
Detailed description of the invention
Fig. 1-specific embodiment extracts the structural schematic diagram of the electrode structure of lithium；
Wherein, collector 1 clamps energization section 11, and active section 12, ion sieve coating 2, selectivity is through film 3.
Specific embodiment
Specific embodiments of the present invention will be described in further detail with reference to the accompanying drawing.
Referring to Fig. 1, the electrode structure of the extraction lithium of specific embodiment, including electrode, electrode successively include collection from inside to outside
Fluid 1, ion sieve coating 2 and selectivity penetrate film 3, the strip of the collector 1 of the present embodiment, and the clamping including one is powered
Section 11 and active section 12, ion sieve coating 2 and selectivity are successively coated on the surface of the active section 12 through film 3 from inside to outside
On.The material of the collector 1 uses nickel or nickel foam；The constituent of the ion sieve coating 2 include ion sieve raw material,
Conductive agent and bonding agent are helped, ion sieve raw material help the mass ratio of conductive agent and bonding agent to be 13~16:1:1；The selectivity
Lithium ion battery film or monovalent cation exchange membrane are used through film 3.
The electrode structure for manufacturing said extracted lithium, includes the following steps:
By the weight ratio of 88:6:6 by 8.8g ion-sieve material-ferric phosphate (FePO4), 0.6g help conductive agent-acetylene black and 0.6g
Bonding agent-PVDF(Kynoar) it is uniformly mixed, the powder mixed is added to pure NMP organic solvent (the N- methyl of 9mL
Pyrrolidones) in wear into slurry, by slurry all spraying or brush on nickel screen or foamed nickel current collector, the work of collector
Segment table area is corresponding to it matching, and 120 °C of heat preservations are dried 10-12 hour in a vacuum drying oven, and ion sieve is obtained after cooling and is applied
Layer electrode.
After obtaining ion sieve coated electrode, monovalent cation exchange membrane is can be selected into through film 3(in selectivity, also may be selected
Diaphragm for lithium ion battery) to ion sieve coating 2(pole piece) coat, and edge is sealed using the mode on hot pressing side
It is fixed, so that production obtains the electrode structure of said extracted lithium.
The application of the obtained electrode structure for extracting lithium, includes the following steps:
The obtained electrode structure for extracting lithium is used for salt lake bittern and mentions lithium and as cathode, using graphite as anode, is placed in electrolysis
In slot, 1L salt lake bittern is added, the lithium content 450mg/L of brine, content of magnesium 10000mg/L(Mg/Li ratio is about 22), in electrode
Both ends apply 1.2V voltage, and after maintaining 14 hours, the lithium content of brine is down to 212mg/L, and magnesium is down to 9997mg/L containing lithium, extract
The ion sieve coating of the electrode structure of lithium is 27mg/g to lithium embedded quantity in brine, and the embedded quantity of magnesium is 0.34mg/g, is realized
Effectively from high Mg/Li ratio brine the purpose of separating Li and inhale magnesium amount it is low.
After embedding lithium, using the electrode structure after embedding lithium as anode, using wire netting as cathode, it is placed in the 120g/L's of 500mL
In NaCl solution, apply the voltage of 0.8V at electrode both ends, after maintaining 14 hours, the lithium content in solution is 468.16mg/L,
The abjection amount of lithium is 26.6mg/g in electrode structure after embedding lithium, and the abjection amount of lithium accounts for the 98.35% of embedded quantity, the magnesium in solution
Content is 5.6mg/L, and extracting solution Mg/Li ratio is greatly reduced to about 0.012.
Electrode structure and the application that lithium is extracted according to the present invention may be implemented to the selectivity of lithium ion height and higher
Deintercalation capacity, have extended cycle life；Have to the brine of high Mg/Li ratio and preferably proposes lithium effect, it is low to magnesium ion adsorbance, it adopts
Have the advantages that process flow is short, easy to operate, production cost is low, easy to industrialized production with the extraction that the present invention carries out lithium.
Finally, it is stated that the above examples are only used to illustrate the technical scheme of the present invention and are not limiting, although referring to compared with
Good embodiment describes the invention in detail, those skilled in the art should understand that, it can be to skill of the invention
Art scheme is modified or replaced equivalently, and without departing from the objective and range of technical solution of the present invention, should all be covered at this
In the scope of the claims of invention.
Claims (10)
1. extracting the electrode structure of lithium, including collector；It is characterized by: the collector includes clamping energization section and work
Section, the surface of the active section are successively coated with ion sieve coating and selectivity through film from inside to outside.
2. extracting the electrode structure of lithium according to claim 1, it is characterised in that: the selectivity uses lithium ion through film
Battery membranes or monovalent cation exchange membrane.
3. extracting the electrode structure of lithium according to claim 1, it is characterised in that: the constituent packet of the ion sieve coating
It includes ion sieve raw material, help conductive agent and bonding agent.
4. extracting the electrode structure of lithium according to claim 3, it is characterised in that: the ion sieve raw material use phosphoric acid
Iron, described to help conductive agent using acetylene black, the bonding agent uses Kynoar.
5. extracting the electrode structure of lithium according to claim 3, it is characterised in that: in the component of the ion sieve coating, from
Son sieve raw material help the mass ratio of conductive agent and bonding agent to be 13~16:1:1.
6. any one of -5 electrode structure for extracting lithium according to claim 1, it is characterised in that: the material of the collector is adopted
With nickel or nickel foam.
7. a kind of manufacturing method for the electrode structure for extracting lithium, it is characterised in that: the electrode structure of this method manufacture is wanted for right
The electrode structure for extracting lithium described in any one of 1-6 is sought, is included the following steps:
1) by powdered ion sieve raw material, help conductive agent and bonding agent to be uniformly mixed, by after mixing powder be added dispersion
Slurry is worn into agent, and slurry is attached to the work section surface of collector, is obtained after vacuum drying with ion sieve coating
Electrode；
2) it is coated outside the ion sieve coating of the electrode with ion sieve coating using selectivity through film, obtains the extraction
The electrode structure of lithium.
8. a kind of manufacturing method for the electrode structure for extracting lithium according to claim 7, it is characterised in that: described in step 1)
Vacuum drying is to dry 10~12 hours in 100~130 DEG C of heat preservations in a vacuum drying oven；The dispersing agent uses N- methyl pyrrole
Pyrrolidone；The method of cladding described in step 2 is to be sealed fixation using the mode on hot pressing side.
9. a kind of application for the electrode structure for extracting lithium, it is characterised in that: this application is based on described in any one of claim 1-6
Extraction lithium electrode structure, include the following steps:
1) separation of lithium；It using the electrode structure for extracting lithium, is placed in salt lake bittern, is equipped with the first supporting electrode, apply
Voltage is embedded into ion sieve coating, the electricity after obtaining embedding lithium after so that the lithium ion in salt lake bittern is penetrated film by selectivity
Pole structure realizes the separation to Lithium from Salt Lake Brine；
2) extraction of lithium；Electrode structure after embedding lithium is placed in supporting electrolyte solution, and is equipped with the second supporting electrode, is applied
Voltage, makes the lithium ion deintercalation in embedded ion sieve coating, is entered in supporting electrolyte solution by selectivity through after film, real
Now to the extraction of lithium.
10. a kind of application for the electrode structure for extracting lithium according to claim 9, it is characterised in that: mentioned described in step 1)
Take the electrode structure of lithium as cathode, the first supporting electrode uses graphite as anode, the material of the first supporting electrode；Apply electricity
It presses 1.0~1.4V and maintains 12~16 hours；
Electrode structure after embedding lithium described in step 2 as anode, the second supporting electrode as cathode, the second supporting electrode
Material uses iron；The supporting electrolyte solution uses sodium chloride solution；Apply 0.6~1.0V of voltage and maintenance 12~16 is small
When.
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Cited By (6)
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| CN110820014A (en) * | 2019-12-16 | 2020-02-21 | 山东理工大学 | Method for recovering graphite flakes and metals from waste lithium ion battery negative pole pieces |
| CN111018061A (en) * | 2019-12-30 | 2020-04-17 | 江苏大学 | Ion sieve cathode for electrolytic cell for extracting lithium from lithium-containing aqueous solution and manufacturing method thereof |
| CN111850593A (en) * | 2020-07-08 | 2020-10-30 | 石家庄嘉硕电子技术有限公司 | Lithium extraction automatic control system and control method |
| CN113293300A (en) * | 2021-05-21 | 2021-08-24 | 江苏中南锂业有限公司 | Preparation method of crown ether modified electrode for extracting lithium from salt lake |
| CN115029734A (en) * | 2022-05-19 | 2022-09-09 | 上海交通大学 | Integrated device for extracting lithium from salt lake and measuring lithium based on garnet type solid electrolyte |
| CN115624958A (en) * | 2022-09-23 | 2023-01-20 | 佛山(华南)新材料研究院 | Film for extracting lithium from salt lake brine, preparation method of film and lithium extraction method |
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| CN110820014B (en) * | 2019-12-16 | 2021-04-02 | 山东理工大学 | Method for recovering graphite flakes and metals from waste lithium ion battery negative pole pieces |
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| CN111018061B (en) * | 2019-12-30 | 2021-08-24 | 江苏大学 | Ion sieve cathode for electrolytic cell for extracting lithium from lithium-containing aqueous solution and manufacturing method thereof |
| CN113307334A (en) * | 2019-12-30 | 2021-08-27 | 江苏大学 | Ionic sieve cathode for electrolytic cells for extracting lithium in aqueous solutions containing lithium |
| CN111018061A (en) * | 2019-12-30 | 2020-04-17 | 江苏大学 | Ion sieve cathode for electrolytic cell for extracting lithium from lithium-containing aqueous solution and manufacturing method thereof |
| CN111850593B (en) * | 2020-07-08 | 2021-03-16 | 石家庄嘉硕电子技术有限公司 | Lithium extraction automatic control system and control method |
| CN111850593A (en) * | 2020-07-08 | 2020-10-30 | 石家庄嘉硕电子技术有限公司 | Lithium extraction automatic control system and control method |
| CN113293300A (en) * | 2021-05-21 | 2021-08-24 | 江苏中南锂业有限公司 | Preparation method of crown ether modified electrode for extracting lithium from salt lake |
| CN113293300B (en) * | 2021-05-21 | 2022-04-12 | 江苏中南锂业有限公司 | Preparation method of crown ether modified electrode for extracting lithium from salt lake |
| CN115029734A (en) * | 2022-05-19 | 2022-09-09 | 上海交通大学 | Integrated device for extracting lithium from salt lake and measuring lithium based on garnet type solid electrolyte |
| CN115029734B (en) * | 2022-05-19 | 2024-04-16 | 上海交通大学 | Integrated device for extracting lithium from salt lake and measuring lithium based on garnet type solid electrolyte |
| CN115624958A (en) * | 2022-09-23 | 2023-01-20 | 佛山(华南)新材料研究院 | Film for extracting lithium from salt lake brine, preparation method of film and lithium extraction method |
| CN115624958B (en) * | 2022-09-23 | 2024-05-28 | 佛山(华南)新材料研究院 | Film for extracting lithium from salt lake brine, preparation method thereof and lithium extraction method |
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