CN111769322B - Solvent-free all-solid-state polymer electrolyte and preparation method thereof - Google Patents
Solvent-free all-solid-state polymer electrolyte and preparation method thereof Download PDFInfo
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- CN111769322B CN111769322B CN202010579191.7A CN202010579191A CN111769322B CN 111769322 B CN111769322 B CN 111769322B CN 202010579191 A CN202010579191 A CN 202010579191A CN 111769322 B CN111769322 B CN 111769322B
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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
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- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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Abstract
The invention discloses a solvent-free all-solid polymer electrolyte and a preparation method thereof, wherein the solvent-free all-solid polymer electrolyte comprises the following raw materials: diisocyanate, lithium salt, comb-shaped macromolecular polyol, a chain extender and a catalyst; the solvent-free all-solid-state polymer electrolyte is prepared simply and efficiently by carrying out prepolymerization reaction on isocyanate, pectinate macromolecular polyol and lithium salt, and adding a micromolecule chain extender and a catalyst for chain extension. The preparation method does not use any organic solvent in the preparation process, the product is simple and easy to obtain, and the prepared polymer electrolyte has excellent mechanical property and also has good ionic conductivity and battery performance.
Description
Technical Field
The invention relates to the technical field of lithium ion all-solid-state polymer electrolytes, in particular to a solvent-free all-solid-state polymer electrolyte and a preparation method thereof.
Background
Lithium batteries have high energy density and portability, and are the most widely used commercial energy storage systems. Although the traditional liquid lithium ion battery has good ionic conductivity and wettability, the traditional liquid lithium ion battery also has the safety problems of poor thermal stability, flammability, easy liquid leakage and the like. The use of a solid electrolyte instead of a liquid electrolyte is an effective solution to the above problems. The mainstream solid electrolytes at present mainly include two main types, namely solid polymer electrolytes and inorganic ceramic electrolytes. All-solid polymer electrolytes, such as PEO (polyethylene oxide), PAN (polyacrylonitrile), PU (polyurethane), PC (polycarbonate), etc., generally have good flexibility, stable interface, easy operability, but have low lithium ion conductivity at low temperature. Therefore, the design and preparation of the composite solid electrolyte organically combines the polymer electrolyte, the inorganic electrolyte and even the liquid electrolyte to realize the functional hybridization of each component, and becomes an effective way for improving the performance of the solid electrolyte. In addition, conventional methods for preparing polymer electrolytes include melt casting methods, sol-gel methods, in-situ formation methods, etc., but these methods use organic solvents more or less during the preparation process, and have safety problems.
Disclosure of Invention
Based on the technical problems in the background art, the invention provides a solvent-free all-solid-state polymer electrolyte and a preparation method thereof.
The invention provides a solvent-free all-solid-state polymer electrolyte, which is characterized by comprising the following raw materials: diisocyanate, lithium salt, comb-shaped macromolecular polyol, a chain extender and a catalyst. Wherein the mass ratio of diisocyanate to comb-shaped macromolecular polyol is (0.2-0.8): 1, the mass ratio of the lithium salt to the comb-shaped macromolecular polyol is (0.1-0.5): 1. the mass ratio of the chain extender to the catalyst to the comb-shaped macromolecular polyol is (50-150): (0.5-5): 1000.
preferably, the comb-shaped macromolecular polyol is at least one of trimethylolpropane-polyethylene glycol monomethyl ether with the number average molecular weight of 1000, 2000 and 3000.
Preferably, the lithium salt is at least one of lithium perchlorate, lithium bistrifluoromethanesulfonylimide, lithium carbonate and lithium hexafluorophosphate.
Preferably, the diisocyanate is at least one of toluene diisocyanate, diphenylmethane diisocyanate, isophorone diisocyanate, and hexamethylene diisocyanate.
Preferably, the chain extender is at least one of ethylenediamine, diethylenetriamine, 1, 4-butanediol and diethylene glycol; preferably, the chain extender is 1, 4-butanediol.
Preferably, the catalyst is at least one of N, N-dimethylcyclohexylamine, bis (2-dimethylaminoethyl) ether, triethanolamine and stannous octoate; preferably, the catalyst is stannous octoate.
The preparation method of the solvent-free all-solid-state polymer electrolyte comprises the steps of mixing the comb-shaped macromolecular polyol and the lithium salt, heating and dissolving the mixture, adding the diisocyanate to perform a prepolymerization reaction, adding the micromolecular chain extender and the catalyst to perform a chain extension reaction, and then placing the mixture in a mold to cure and dry the mixture to obtain the solvent-free all-solid-state polymer electrolyte.
Preferably, the preparation method of the solvent-free all-solid polymer electrolyte comprises the following steps:
s1, adding lithium salt into the comb-shaped macromolecular polyol, heating and stirring at 60-100 ℃ until the lithium salt is completely dissolved, and then adding diisocyanate to react for 1-4 hours at constant temperature;
s2, cooling the material prepared in the step S1 to 30-50 ℃, adding a chain extender and a catalyst, and heating to 50-70 ℃ for reaction for 0.5-2 hours;
s3, pouring the material prepared in the step S2 into a polytetrafluoroethylene mold, curing at 100-140 ℃ for 2-8 h, and then placing at 60-100 ℃ for vacuum drying for 8-16 h to obtain the finished product.
The invention has the following beneficial effects:
1. PU (polyurethane elastomer) is a block copolymer comprising soft and hard segments, belonging to a class of elastomers of high strength and low crystallinity. The soft and hard segments are thermodynamically incompatible, so that the hydrogen bonding effect between the segments is promoted, and the ionic conductivity of the polymer electrolyte is obviously improved;
2. the trimethylolpropane-polyethylene glycol monomethyl ether has a special comb-shaped side chain structure and can be complexed with a large amount of lithium salt, and the addition of the lithium salt can improve the ionic conductivity of the prepared polymer matrix.
3. According to the invention, no organic solvent is used in the preparation process, the problems of harm to human bodies, environmental pollution and the like do not exist, the prepared polymer electrolyte has good flexibility, the breaking elongation of the adhesive film can reach 100-400%, the tensile strength can reach 5-20 MPa, and the adhesive film has excellent mechanical properties.
Drawings
FIG. 1 is a stress-strain curve of the samples of examples 1-4.
FIG. 2 is a graph showing the relationship between the ionic conductivity and the temperature Arrhenius of the samples in examples 1 to 4.
Fig. 3 is a first charge-discharge curve diagram of the button lithium ion battery assembled by the samples of examples 1-4.
FIG. 4 is a graph showing the cycle charge and discharge test of the battery assembled with the all-solid polymer electrolyte prepared in examples 1 to 4.
Detailed Description
The technical solution of the present invention will be described in detail below with reference to specific examples.
Example 1
The solvent-free all-solid-state polymer electrolyte is prepared by the following specific steps:
s1, adding 10g of lithium perchlorate and 30g of trimethylolpropane-polyethylene glycol monomethyl ether into a four-neck flask provided with a polytetrafluoroethylene stirring rod, a spherical condenser and a thermometer, heating and stirring at 90 ℃ until the lithium perchlorate is completely dissolved, and then adding 10.09g of hexamethylene diisocyanate to react for 2.5 hours at constant temperature;
s2, cooling the material prepared in the step S1 to 40 ℃ by using ice water, then adding 2.8g of diethylene glycol and 0.043g of stannous octoate, heating to 60 ℃ and reacting for 1 h;
s3, pouring the material prepared in the step S2 into a polytetrafluoroethylene mold, curing for 4 hours at 120 ℃, and then vacuum-drying for 12 hours at 80 ℃ to obtain the polytetrafluoroethylene composite material.
Example 2
The solvent-free all-solid-state polymer electrolyte is prepared by the following specific steps:
s1, adding 10g of lithium perchlorate and 30g of trimethylolpropane-polyethylene glycol monomethyl ether into a four-neck flask provided with a polytetrafluoroethylene stirring rod, a spherical condenser and a thermometer, heating and stirring at 80 ℃ until lithium salt is completely dissolved, and then adding 10.45g of toluene diisocyanate to react for 2.5 hours at constant temperature;
s2, cooling the material prepared in the step S1 to 40 ℃ by using ice water, then adding 2.8g of diethylene glycol and 0.043g of stannous octoate, heating to 60 ℃ and reacting for 1 h;
s3, pouring the material prepared in the step S2 into a polytetrafluoroethylene mold, curing for 4 hours at 120 ℃, and then vacuum-drying for 12 hours at 80 ℃ to obtain the polytetrafluoroethylene composite material.
Example 3
The solvent-free all-solid-state polymer electrolyte is prepared by the following specific steps:
s1, adding 10g of lithium perchlorate and 30g of trimethylolpropane-polyethylene glycol monomethyl ether into a four-neck flask provided with a polytetrafluoroethylene stirring rod, a spherical condenser and a thermometer, heating and stirring at 80 ℃ until the lithium perchlorate is completely dissolved, and then adding 15.01g of diphenylmethane diisocyanate to react for 2.5 hours at constant temperature;
s2, cooling the material prepared in the step S1 to 40 ℃ by using ice water, then adding 2.8g of diethylene glycol and 0.048g of stannous octoate, heating to 60 ℃ and reacting for 1 h;
s3, pouring the material prepared in the step S2 into a polytetrafluoroethylene mold, curing for 4 hours at 120 ℃, and then vacuum-drying for 12 hours at 80 ℃ to obtain the polytetrafluoroethylene composite material.
Example 4
The solvent-free all-solid-state polymer electrolyte is prepared by the following specific steps:
s1, adding 10g of lithium perchlorate and 30g of trimethylolpropane-polyethylene glycol monomethyl ether into a four-neck flask provided with a polytetrafluoroethylene stirring rod, a spherical condenser and a thermometer, heating and stirring at 90 ℃ until the lithium salt is completely dissolved, and then adding 13.33g of isophorone diisocyanate to react for 2.5 hours at constant temperature;
s2, cooling the material prepared in the step S1 to 40 ℃ by using ice water, then adding 2.8g of diethylene glycol and 0.046g of stannous octoate, heating to 60 ℃ and reacting for 1 h;
s3, pouring the material prepared in the step S2 into a polytetrafluoroethylene mold, curing for 4 hours at 120 ℃, and then vacuum-drying for 12 hours at 80 ℃ to obtain the polytetrafluoroethylene composite material.
Example 5
The preparation method of the solvent-free all-solid-state polymer electrolyte comprises the following specific steps:
s1, adding 10g of lithium carbonate and 100g of trimethylolpropane-polyethylene glycol monomethyl ether into a four-neck flask provided with a polytetrafluoroethylene stirring rod, a spherical condenser tube and a thermometer, heating and stirring at 60 ℃ until the lithium salt is completely dissolved, and then adding 20g of isophorone diisocyanate to react for 1 hour at constant temperature;
s2, cooling the material prepared in the step S1 to 30 ℃ by using ice water, then adding 5g of diethylene glycol and 0.05g of stannous octoate, heating to 50 ℃ and reacting for 0.5 h;
s3, pouring the material prepared in the step S2 into a polytetrafluoroethylene mold, curing for 2 hours at 100 ℃, and then drying for 8 hours in vacuum at 60 ℃ to obtain the polytetrafluoroethylene composite material.
Example 6
The solvent-free all-solid-state polymer electrolyte is prepared by the following specific steps:
s1, adding 5g of lithium hexafluorophosphate and 10g of trimethylolpropane-polyethylene glycol monomethyl ether into a four-neck flask provided with a polytetrafluoroethylene stirring rod, a spherical condenser tube and a thermometer, heating and stirring at 100 ℃ until the lithium salt is completely dissolved, and then adding 8g of isophorone diisocyanate to react for 4 hours at constant temperature;
s2, cooling the material prepared in the step S1 to 50 ℃ by using ice water, then adding 1.5g of diethylene glycol and 0.05g of stannous octoate, heating to 70 ℃ and reacting for 2 hours;
s3, pouring the material prepared in the step S2 into a polytetrafluoroethylene mold, curing at 140 ℃ for 8 hours, and then vacuum-drying at 100 ℃ for 16 hours to obtain the polytetrafluoroethylene composite material.
The solvent-free all-solid polymer electrolyte samples prepared in examples 1 to 4 were subjected to performance tests, and the results are shown in fig. 1 to 4.
Fig. 1 shows stress-strain curves for various example samples. As can be seen from the figure, the tensile strength of the all-solid polymer electrolyte adhesive film prepared in example 1 reaches 15.4MPa, and the elongation at break reaches 180.3%; the tensile strength of the all-solid-state polymer electrolyte adhesive film prepared in the embodiment 2 reaches 12.2MPa, and the elongation at break reaches 352.4%; the tensile strength of the all-solid-state polymer electrolyte adhesive film prepared in the embodiment 3 reaches 13.8MPa, and the elongation at break reaches 245.6%; the tensile strength of the all-solid-state polymer electrolyte adhesive film prepared in example 4 reaches 10.3MPa, and the elongation at break reaches 291.4%. From the test results, the all-solid polymer electrolyte prepared according to the present invention has good mechanical strength.
FIG. 2 is a graph of the ionic conductivity versus temperature Arrhenius for various examples. The theory of the ionic conductivity of polymer electrolytes as a function of temperature can be described by the Arrhenius equation. The Arrhenius formula is expressed as σ ═ σ0exp (-Ea/KT), wherein σ is the ionic conductivity of the polymer electrolyte, and σ0To indicate the pre-factor, Ea is the activation energy, K is the boltzmann constant, and T is the test temperature. Plots of lg (. sigma.) vs. 1000/T were fitted to FIG. 2. The conductivity of the all-solid-state polymer electrolyte is mainly realized by the molecular chain motion and the complexation-dissociation action of polymer-lithium ions. The temperature is increased, so that the mobility of polymer molecular chain segments can be improved, the number of conductive carriers is increased, and the conductivity of the electrolyte is effectively improved. It can be seen from FIG. 2 that the ionic conductivities of the examples reached a maximum of 7.8X 10, respectively, when the test temperature was 100 deg.C-4s/cm、6.6×10-4s/cm、2.5×10-4s/cm、3.2×10-5s/cm。
Fig. 3 is a first charge-discharge curve diagram of the assembled button lithium ion battery, the test voltage range is 2.2-4.0V, the test current is 0.2C, and the temperature is 60 ℃. The first charge-discharge efficiencies of the examples 1 to 4 were 99.3%, 98.9%, 98.5%, and 98.3% in order, and the discharge capacities were 140.8mAh/g, 134.2mAh/g, 136.6mAh/g, and 131.8mAh/g in order, and the test results showed that the all-solid polymer electrolyte prepared by the present invention had a higher battery capacity.
FIG. 4 is a graph showing the cycle charge and discharge test of the battery assembled with the all-solid polymer electrolyte prepared in examples 1 to 4, wherein the test current is 1C and the temperature is 60 ℃. As can be seen from fig. 4, the capacity retention rates of the solvent-free all-solid-state polymer electrolytes obtained in examples 1 to 4 after 300 times of cyclic discharge are 96.1%, 97.6%, 96.3% and 94.5% in sequence, and the capacity has small amplitude attenuation, which indicates that the solvent-free all-solid-state polymer electrolyte obtained in the present invention has good cycle stability.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (6)
1. A preparation method of solvent-free type all-solid-state polymer electrolyte is characterized in that firstly, comb-shaped macromolecular polyol and lithium salt are mixed and heated to be dissolved, diisocyanate is added for prepolymerization reaction, and finally, micromolecule chain extender and catalyst are added for chain extension reaction, and then the mixture is placed in a mold for curing and drying to obtain the solvent-free type all-solid-state polymer electrolyte;
the preparation method of the solvent-free all-solid polymer electrolyte comprises the following steps:
s1, adding lithium salt into the comb-shaped macromolecular polyol, heating and stirring at 60-100 ℃ until the lithium salt is completely dissolved, and then adding diisocyanate to react for 1-4 hours at constant temperature;
s2, cooling the material prepared in the step S1 to 30-50 ℃, adding a chain extender and a catalyst, and heating to 50-70 ℃ for reaction for 0.5-2 hours;
s3, pouring the material prepared in the step S2 into a polytetrafluoroethylene mold, curing at 100-140 ℃ for 2-8 h, and then placing at 60-100 ℃ for vacuum drying for 8-16 h to obtain the finished product;
the solvent-free all-solid-state polymer electrolyte comprises the following raw materials: diisocyanate, lithium salt, comb-shaped macromolecular polyol, a chain extender and a catalyst; wherein the mass ratio of diisocyanate to comb-shaped macromolecular polyol is (0.2-0.8): 1, the mass ratio of the lithium salt to the comb-shaped macromolecular polyol is (0.1-0.5): 1; the mass ratio of the chain extender to the catalyst to the comb-shaped macromolecular polyol is (50-150): (0.5-5): 1000.
2. the method for preparing a solvent-free all-solid polymer electrolyte according to claim 1, wherein the comb-like macromolecular polyol is at least one of trimethylolpropane-polyethylene glycol monomethyl ether having a number average molecular weight of 1000, 2000, 3000.
3. The method for preparing a solvent-free all-solid polymer electrolyte according to claim 1 or 2, wherein the lithium salt is at least one of lithium perchlorate, lithium bistrifluoromethanesulfonylimide, lithium carbonate, and lithium hexafluorophosphate.
4. The method for preparing a solvent-free all-solid polymer electrolyte according to claim 1 or 2, wherein the diisocyanate is at least one of toluene diisocyanate, diphenylmethane diisocyanate, isophorone diisocyanate, and hexamethylene diisocyanate.
5. The method for preparing a solvent-free all-solid polymer electrolyte according to claim 1 or 2, wherein the chain extender is at least one of ethylenediamine, diethylenetriamine, 1, 4-butanediol, and diethylene glycol.
6. The method for preparing a solvent-free all-solid polymer electrolyte according to claim 1 or 2, wherein the catalyst is at least one of N, N-dimethylcyclohexylamine, bis (2-dimethylaminoethyl) ether, triethanolamine, and stannous octoate.
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| CN112745474B (en) * | 2020-12-29 | 2022-06-07 | 合肥国轩高科动力能源有限公司 | Preparation method of all-solid-state polymer electrolyte and prepared product |
| CN112759700B (en) * | 2021-01-22 | 2021-10-22 | 浙江大学 | All-solid-state ion-conductive elastomer and preparation and application thereof |
| CN112920365B (en) * | 2021-01-28 | 2022-07-05 | 合肥国轩高科动力能源有限公司 | Preparation method of anionic-nonionic aqueous polyurethane polymer electrolyte |
| CN113929918B (en) * | 2021-09-02 | 2023-01-10 | 西安理工大学 | Supermolecule electrolyte and preparation method thereof |
| CN115627146B (en) * | 2022-10-07 | 2023-08-29 | 宁波捷傲创益新材料有限公司 | Preparation method of adhesive for aluminum plastic film |
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