CN111129581A - Lithium battery gel electrolyte and preparation method thereof - Google Patents
Lithium battery gel electrolyte and preparation method thereof Download PDFInfo
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- CN111129581A CN111129581A CN201911161502.1A CN201911161502A CN111129581A CN 111129581 A CN111129581 A CN 111129581A CN 201911161502 A CN201911161502 A CN 201911161502A CN 111129581 A CN111129581 A CN 111129581A
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- coupling agent
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
- H01M10/0564—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of organic materials only
- H01M10/0565—Polymeric materials, e.g. gel-type or solid-type
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/058—Construction or manufacture
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M2300/00—Electrolytes
- H01M2300/0088—Composites
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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
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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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
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Abstract
The invention discloses a lithium battery gel electrolyte and a preparation method thereof, belonging to the technical field of lithium battery materials. The product developed by the invention comprises 60-100 parts of coupling agent modified sepiolite, 8-10 parts of lithium salt and 30-40 parts of solvent. When the product is prepared, mixing sepiolite and water for pulping, adding strong acid for acidification, roasting to prepare acidified sepiolite, then modifying the acidified sepiolite by using a silane coupling agent, mixing the coupling agent modified sepiolite, lithium salt and a solvent for ball milling, and standing to prepare the lithium battery gel electrolyte. The product obtained by the invention has good ionic conductivity, can resist high voltage of more than 4.2V, and has wide application prospect.
Description
Technical Field
The invention relates to the technical field of battery materials, in particular to a lithium battery gel-state electrolyte and a preparation method thereof.
Background
In electrochemical devices such as primary batteries, secondary batteries, dye-sensitized solar cells, perovskite solar cells, intelligent windows and the like, an ion conductive electrolyte between two electrodes is a mass transfer unit in the device and is an essential component of the device. High conductivity and good physical properties are the basic requirements for practical devices on electrolytes. The liquid electrolyte has high conductivity, but the application of the liquid electrolyte is limited by the fluidity of the liquid electrolyte, the solid electrolyte has good physical properties, but the ion migration is limited, and the gel electrolyte has high conductivity close to that of the liquid electrolyte and good physical properties, and is a solid electrolyte with wide application. Gel electrolytes prepared from various polymers can be applied to lithium ion secondary batteries, but the electrochemical conversion efficiency is still obviously lower than that of lithium batteries with liquid electrolytes, and a high molecular material for the gel electrolyte needs to be continuously searched.
The gel electrolyte is composed of three essential components of conductive particles, a solvent and a polymer. The polymer is a support material of the gel electrolyte, which not only provides a channel for ion transmission, but also ensures the physical properties of the material. The solvent in the gel electrolyte has two functions, firstly, the solvent is provided for the separation of conductive positive and negative ions, and the electrostatic capacity can be weakened only when the positive and negative ions are respectively surrounded by the solvent and combined; secondly, the polymer is swelled, and the high molecular carbon chains are separated to generate gaps to provide ion migration channels, so the polymer is also called as a plasticizer. As the solvent, carbonates, amides, etc. are usually used.
With the requirement of high energy density of lithium batteries, higher requirements are put forward on the high voltage resistance of electrolytes, and as gel-state electrolytes, the requirements of polymer frameworks and the high voltage resistance of electrolytes retained in the frameworks are also improved, so that how to improve the high voltage resistance of the gel-state electrolytes from the raw material end is one of the problems to be solved urgently by those skilled in the art.
Disclosure of Invention
The invention aims to provide a lithium battery gel-state electrolyte and a preparation method thereof, which aim to solve the defects that the existing polymer gel-state electrolyte is low in ionic conductivity and cannot tolerate high voltage.
In order to achieve the purpose, the invention provides the following technical scheme:
a lithium battery gel electrolyte comprises the following raw materials in parts by weight: 60-100 parts of coupling agent modified sepiolite, 8-10 parts of lithium salt and 30-40 parts of solvent.
The technical scheme of the invention is that the sepiolite is used as a matrix to construct an organic-inorganic composite gel system, the sepiolite is of a layered silicate structure, interlayer water and exchangeable cations are filled between layers of the sepiolite, non-Newtonian liquid type thixotropic gel can be formed in a solution, the inorganic gel can form a space network structure, and a grafted organic silicon chain segment can be beneficial to the constraint and retention of an organic solvent, so that a large amount of free organic solvent is constrained in the layered silicate structure, and the application obtains higher viscosity, thereby being beneficial to the transmission of lithium ions in the layered structure; and the inorganic gel structure has good high-voltage resistance.
Further, the sepiolite modified by the coupling agent is sepiolite modified by a silane coupling agent.
Further, the silane coupling agent is any one of a silane coupling agent KH-550, a silane coupling agent KH-560 and a silane coupling agent KH-570.
Further, the sepiolite is acid-treated sepiolite; the acid is any one of hydrochloric acid, sulfuric acid and nitric acid.
The technical scheme of the invention is that the sepiolite is treated by acid, and the hydrogen ions and the magnesium ions in the sepiolite interlayer structure are subjected to ion exchange, so that an Si-O skeleton is converted into Si-OH, the Si-OH has strong interaction force, and a stable hydrogen bond is more easily formed, thereby being beneficial to the formation of a gel structure.
Further, the lithium salt is any one of lithium perchlorate, lithium tetrafluoroborate and lithium hexafluorophosphate.
Further, the solvent is any one of ethylene carbonate, propylene carbonate and DMF.
A preparation method of a gel-state electrolyte of a patent lithium battery comprises the following specific preparation steps:
(1) preparing raw materials;
(2) pulping: adding water into sepiolite to prepare a suspension with the concentration of 8-20 g/L;
(3) acidifying: adding acid into the suspension, adjusting the pH value to 1.0-2.0, performing hydrothermal reaction, separating, and drying to obtain acidified sepiolite;
(4) modifying a coupling agent: dispersing the acidified sepiolite into an absolute ethyl alcohol solution of a silane coupling agent, heating and refluxing for reaction, centrifugally separating, and drying to obtain coupling agent modified sepiolite;
(5) preparation: and ball-milling and mixing the coupling agent modified sepiolite, the lithium salt and the solvent, and standing to obtain the gel-state electrolyte of the lithium battery.
Further, the preparation method of the lithium battery gel electrolyte comprises the following specific preparation steps:
(1) preparing raw materials;
(2) pulping: adding water into sepiolite to prepare a suspension with the concentration of 10-12%;
(3) acidifying: adding hydrochloric acid with the mass fraction of 10% into the suspension, adjusting the pH to 1.0, performing hydrothermal reaction, separating, drying and roasting to obtain acidified sepiolite;
(4) modifying a coupling agent: dispersing the acidified sepiolite into an absolute ethyl alcohol solution of a silane coupling agent, heating and refluxing for reaction, centrifugally separating, and drying to obtain coupling agent modified sepiolite;
(5) preparation: and ball-milling and mixing the coupling agent modified sepiolite, the lithium salt and the solvent, and standing to obtain the gel-state electrolyte of the lithium battery.
According to the technical scheme, the sepiolite serves as an inorganic gelling framework, the organic functional group is introduced into the framework through the grafting coupling agent, the interlayer structures are sheared through high-energy ball milling, a gelling system is damaged, and the fluidity is improved, so that lithium salt and an organic solvent are effectively deposited into the interlayer structures of the sepiolite, the Si-OH are enabled to form gel structures again through the hydrogen bond acting force between each other through the subsequent standing process, the lithium salt and the organic solvent are bound in the interlayer structures, and the inorganic layered structures are higher in ion transmission efficiency compared with the traditional polymers while the good high-voltage resistance performance of the inorganic gelling system is utilized.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Mixing sepiolite and water, pouring the mixture into a beaker to prepare a suspension with the concentration of 10-12%, ultrasonically dispersing for 1-3 hours, adding acid into the suspension, adjusting the pH to 1.0-2.0, transferring the suspension into a hydrothermal kettle, carrying out hydrothermal stirring reaction for 1-3 hours at the temperature of 170-180 ℃ and the pressure of 2.0-5.0 MPa and the stirring speed of 300-800 r/min, carrying out centrifugal separation, collecting a filter cake, washing the filter cake with deionized water for 3-5 times, drying the washed filter cake to constant weight at the temperature of 105-110 ℃, and thus obtaining a dried filter cake; then transferring the dried filter cake into a tubular furnace, roasting for 1-3 h at the temperature of 200-300 ℃, cooling to room temperature along with the furnace, and discharging to obtain acidified sepiolite; sequentially taking 10-20 parts of acidified sepiolite, 1-10 parts of silane coupling agent and 100-200 parts of absolute ethyl alcohol according to parts by weight, firstly dissolving the silane coupling agent in the absolute ethyl alcohol, then adding the acidified sepiolite into an absolute ethyl alcohol solution of the silane coupling agent, heating to 80 ℃, carrying out reflux reaction for 1-3 hours, carrying out centrifugal separation, collecting a filter cake, and drying to remove the solvent to obtain the coupling agent modified sepiolite; according to the weight parts, 60-100 parts of coupling agent modified sepiolite, 8-10 parts of lithium salt and 30-40 parts of solvent are sequentially mixed and poured into a ball milling tank, and the mass ratio of ball materials is 10: 1-30: adding ball milling beads into the mixture 1, performing ball milling and mixing for 4-6 hours, discharging, and standing in a closed manner for 8-12 hours to obtain the lithium battery gel electrolyte. The silane coupling agent is any one of a silane coupling agent KH-550, a silane coupling agent KH-560 and a silane coupling agent KH-570. The acid is any one of hydrochloric acid, sulfuric acid and nitric acid. The lithium salt is any one of lithium perchlorate, lithium tetrafluoroborate and lithium hexafluorophosphate. The solvent is any one of ethylene carbonate, propylene carbonate and DMF.
Example 1
Mixing sepiolite and water, pouring the mixture into a beaker to prepare a suspension with the concentration of 10%, ultrasonically dispersing for 1h, adding hydrochloric acid with the mass fraction of 10% into the suspension, adjusting the pH to 1.0, transferring the suspension into a hydrothermal kettle, carrying out hydrothermal stirring reaction for 1h at the temperature of 170 ℃ and the pressure of 2.0MPa and the stirring speed of 300r/min, carrying out centrifugal separation, collecting a filter cake, washing the filter cake for 3 times by using deionized water, and drying the washed filter cake to constant weight at the temperature of 105 ℃ to obtain a dried filter cake; then transferring the dried filter cake into a tubular furnace, roasting for 1h at the temperature of 200 ℃, cooling to room temperature along with the furnace, and discharging to obtain acidified sepiolite; sequentially taking 10 parts of acidified sepiolite, 1 part of silane coupling agent and 100 parts of absolute ethyl alcohol according to parts by weight, firstly dissolving the silane coupling agent in the absolute ethyl alcohol, then adding the acidified sepiolite into the absolute ethyl alcohol solution of the silane coupling agent, heating to 80 ℃, carrying out reflux reaction for 1h, carrying out centrifugal separation, collecting a filter cake, and drying to remove the solvent to obtain the coupling agent modified sepiolite; according to the weight portion, 60 portions of coupling agent modified sepiolite, 8 portions of lithium salt and 30 portions of solvent are mixed and poured into a ball milling tank, and the mass ratio of ball materials is 10: 1 adding ball milling beads, performing ball milling and mixing for 4 hours, discharging, and hermetically standing for 8 hours to obtain the lithium battery gel electrolyte. The silane coupling agent is a silane coupling agent KH-550. The lithium salt is lithium perchlorate. The solvent is ethylene carbonate.
Example 2
Mixing sepiolite and water, pouring the mixture into a beaker to prepare suspension with the concentration of 11%, ultrasonically dispersing for 2 hours, adding 5% sulfuric acid by mass into the suspension, adjusting the pH to 1.5, transferring the suspension into a hydrothermal kettle, carrying out hydrothermal stirring reaction for 2 hours at the temperature of 175 ℃, the pressure of 3.0MPa and the stirring speed of 500r/min, carrying out centrifugal separation, collecting a filter cake, washing the filter cake for 4 times by using deionized water, and drying the washed filter cake to constant weight at the temperature of 108 ℃ to obtain a dried filter cake; then the dried filter cake is moved into a tubular furnace, is roasted for 2 hours at the temperature of 260 ℃, is cooled to the room temperature along with the furnace, and is discharged to obtain the acidified sepiolite; taking 15 parts of acidified sepiolite, 5 parts of silane coupling agent and 150 parts of absolute ethyl alcohol in sequence according to parts by weight, firstly dissolving the silane coupling agent in the absolute ethyl alcohol, then adding the acidified sepiolite into the absolute ethyl alcohol solution of the silane coupling agent, heating to 80 ℃, carrying out reflux reaction for 2 hours, carrying out centrifugal separation, collecting filter cakes, and drying to remove the solvent to obtain coupling agent modified sepiolite; according to the weight parts, 80 parts of coupling agent modified sepiolite, 9 parts of lithium salt and 35 parts of solvent are sequentially mixed and poured into a ball milling tank, and the mass ratio of ball materials is 20: 1 adding ball milling beads, performing ball milling and mixing for 5 hours, discharging, and hermetically standing for 10 hours to obtain the lithium battery gel electrolyte. The silane coupling agent is a silane coupling agent KH-560. The lithium salt is lithium tetrafluoroborate. The solvent is propylene carbonate.
Example 3
Mixing sepiolite and water, pouring the mixture into a beaker to prepare a suspension with the concentration of 12%, ultrasonically dispersing the suspension for 3 hours, adding nitric acid with the mass fraction of 3% into the suspension, adjusting the pH to 2.0, transferring the suspension into a hydrothermal kettle, carrying out hydrothermal stirring reaction for 3 hours at the temperature of 180 ℃ and the pressure of 5.0MPa and the stirring speed of 800r/min, carrying out centrifugal separation, collecting a filter cake, washing the filter cake for 5 times by using deionized water, and drying the washed filter cake to constant weight at the temperature of 110 ℃ to obtain a dried filter cake; then the dried filter cake is moved into a tubular furnace, is roasted for 3 hours at the temperature of 300 ℃, is cooled to the room temperature along with the furnace, and is discharged to obtain the acidified sepiolite; sequentially taking 20 parts of acidified sepiolite, 10 parts of silane coupling agent and 200 parts of absolute ethyl alcohol according to parts by weight, dissolving the silane coupling agent in the absolute ethyl alcohol, adding the acidified sepiolite into the absolute ethyl alcohol solution of the silane coupling agent, heating to 80 ℃, carrying out reflux reaction for 3 hours, carrying out centrifugal separation, collecting a filter cake, and drying to remove the solvent to obtain coupling agent modified sepiolite; according to the weight parts, 100 parts of coupling agent modified sepiolite, 10 parts of lithium salt and 40 parts of solvent are mixed and poured into a ball milling tank, and the mass ratio of ball materials is 30: 1 adding ball milling beads, performing ball milling and mixing for 6 hours, discharging, and hermetically standing for 12 hours to obtain the lithium battery gel electrolyte. The silane coupling agent is a silane coupling agent KH-570. The lithium salt is lithium hexafluorophosphate. The solvent is DMF.
Comparative example 1
This comparative example differs from example 1 in that: the sepiolite was used without acidification, and the remaining conditions were unchanged.
Comparative example 2
This comparative example differs from example 1 in that: the sepiolite is not grafted with the coupling agent, and the other conditions are not changed.
Comparative example 3
This comparative example differs from example 1 in that: preparing an organogel electrolyte by taking PMMA as a polymer, DMF as an organic solvent and lithium hexafluorophosphate as a lithium salt; wherein the dosage of PMMA is 0.17g/mL, and the dosage of lithium hexafluorophosphate is 0.16 g/mL.
The products obtained in examples 1 to 3 and comparative examples 1 to 3 were subjected to performance tests, and the specific test methods and test results were as follows:
since the prepared electrolyte is in a gel state, it can be directly tested by a conductivity meter. The electrodes used for the test were platinum electrodes. Specific test results are shown in table 1;
lithium iron phosphate is used as a positive electrode active material, graphite is used as a negative electrode active material, the lithium iron phosphate and the graphite are assembled into a secondary battery with the product, the charging and discharging cycle is carried out at the voltage of 4.5V, after the cycle is carried out for 100 times, the attenuation rate of the energy density of the battery is tested, the higher the attenuation rate is, the worse the high-voltage resistance of the electrolyte is, and the specific test results are shown in Table 1:
table 1: product performance test results
| conductivity/mS/cm | Attenuation ratio% | |
| Example 1 | 6.8 | 5.1 |
| Example 2 | 7.2 | 5.3 |
| Example 3 | 8.1 | 4.9 |
| Comparative example 1 | 5.5 | 10.6 |
| Comparative example 2 | 2.3 | 15.2 |
| Comparative example 3 | 1.2 | 55.6 |
As can be seen from the test results in table 1, in comparative example 3, since a common organic gel system is used, the conductivity is low and the battery cannot withstand high voltage, and after charge and discharge cycles are performed under high voltage conditions, the battery performance rapidly decays.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein, and any reference thereto is therefore intended to be embraced therein.
Claims (8)
1. The lithium battery gel electrolyte is characterized by comprising the following raw materials in parts by weight: 60-100 parts of coupling agent modified sepiolite, 8-10 parts of lithium salt and 30-40 parts of solvent.
2. The gel-state electrolyte for lithium batteries according to claim 1, wherein said sepiolite modified with a coupling agent is a sepiolite modified with a silane coupling agent.
3. The gel-state electrolyte for lithium batteries as claimed in claim 1, wherein said silane coupling agent is any one of silane coupling agent KH-550, silane coupling agent KH-560, and silane coupling agent KH-570.
4. The lithium battery gel electrolyte as claimed in claim 1 or 2, wherein the sepiolite is an acid-treated sepiolite; the acid is any one of hydrochloric acid, sulfuric acid and nitric acid.
5. The gel electrolyte for lithium battery as claimed in claim 1, wherein the lithium salt is any one of lithium perchlorate, lithium tetrafluoroborate and lithium hexafluorophosphate.
6. The gel electrolyte for lithium batteries according to claim 1, wherein said solvent is any one of ethylene carbonate, propylene carbonate, and DMF.
7. A preparation method of a gel-state electrolyte of a patent lithium battery is characterized by comprising the following specific preparation steps:
(1) preparing raw materials;
(2) pulping: adding water into sepiolite to prepare a suspension with the concentration of 8-20 g/L;
(3) acidifying: adding acid into the suspension, adjusting the pH value to 1.0-2.0, performing hydrothermal reaction, separating, and drying to obtain acidified sepiolite;
(4) modifying a coupling agent: dispersing the acidified sepiolite into an absolute ethyl alcohol solution of a silane coupling agent, heating and refluxing for reaction, centrifugally separating, and drying to obtain coupling agent modified sepiolite;
(5) preparation: and ball-milling and mixing the coupling agent modified sepiolite, the lithium salt and the solvent, and standing to obtain the gel-state electrolyte of the lithium battery.
8. The method for preparing the gel-state electrolyte for a lithium battery according to claim 7, which comprises the following steps:
(1) preparing raw materials;
(2) pulping: adding water into sepiolite to prepare a suspension with the concentration of 10-12%;
(3) acidifying: adding hydrochloric acid with the mass fraction of 10% into the suspension, adjusting the pH to 1.0, performing hydrothermal reaction, separating, drying and roasting to obtain acidified sepiolite;
(4) modifying a coupling agent: dispersing the acidified sepiolite into an absolute ethyl alcohol solution of a silane coupling agent, heating and refluxing for reaction, centrifugally separating, and drying to obtain coupling agent modified sepiolite;
(5) preparation: and ball-milling and mixing the coupling agent modified sepiolite, the lithium salt and the solvent, and standing to obtain the gel-state electrolyte of the lithium battery.
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Application publication date: 20200508 |
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