CN115133122B - Preparation method and application of lithium ion battery electrolyte - Google Patents
Preparation method and application of lithium ion battery electrolyte Download PDFInfo
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- CN115133122B CN115133122B CN202211040752.1A CN202211040752A CN115133122B CN 115133122 B CN115133122 B CN 115133122B CN 202211040752 A CN202211040752 A CN 202211040752A CN 115133122 B CN115133122 B CN 115133122B
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- H—ELECTRICITY
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- 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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- 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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Abstract
The invention provides a preparation method and application of a lithium ion battery electrolyte, and relates to the field of battery electrolytes, wherein the lithium ion battery electrolyte is a gel polymer electrolyte and comprises the following components in parts by weight: 10-15 parts of a polymer film matrix, 50-100 parts of acetonitrile, 5-10 parts of lithium hexafluorophosphate, 10-15 parts of allyl modified hydrotalcite and 3-6 parts of a plasticizer, wherein the polymer film matrix is polyvinyl formal, the allyl amine modified hydrotalcite is hydrotalcite containing allyl functional groups and obtained by modifying allyl amine, the plasticizer is polydimethylsiloxane, and the allyl amine modified hydrotalcite and the polyvinyl formal are subjected to an olefinic reaction and crosslinking, so that the invention has the beneficial effects that: the hydrotalcite material has a layered structure, so that the transmission of lithium ions is enhanced, lithium hexafluorophosphate has high ionic conductivity, polyvinyl formal is a polymer film matrix, pores are large, and the ionic conductivity of the gel polymer electrolyte is synergistically improved.
Description
Technical Field
The invention relates to the technical field of battery electrolytes, in particular to a preparation method and application of a lithium ion battery electrolyte.
Background
With the increasing exhaustion of non-renewable resources, these energy sources will generate a certain degree of environmental pollution during the use process, and therefore, there is a need to find a clean, green and high-energy-density energy storage medium, and among various clean secondary energy sources, a lithium ion battery is the most concerned one.
The traditional lithium ion battery generally uses an organic solvent containing lithium salt as an electrolyte, and although the electrolyte has high ionic conductivity and is beneficial to the transmission of lithium ions in the battery, the compatibility of metal lithium and liquid electrolyte is poor, lithium dendrite can be generated in the charge-discharge cycle of the battery, and a bulge is easily formed to penetrate through a diaphragm, so that the volatilization and leakage of the electrolyte can be caused, the expansion and even explosion of the battery can be possibly caused, and the potential safety hazard is potential great.
Disclosure of Invention
The invention provides a lithium ion battery electrolyte, which is a gel polymer electrolyte and comprises the following components in parts by weight: 10-15 parts of a polymer film matrix, 50-100 parts of acetonitrile, 5-10 parts of lithium hexafluorophosphate, 10-15 parts of allyl modified hydrotalcite and 3-6 parts of a plasticizer, wherein the polymer film matrix is polyvinyl formal, the allyl amine modified hydrotalcite is hydrotalcite containing allyl functional groups and obtained by modifying allyl amine, the plasticizer is polydimethylsiloxane, and the allyl amine modified hydrotalcite and the polyvinyl formal are subjected to an ene reaction and crosslinking.
The preparation method of the lithium ion battery electrolyte is characterized by comprising the following steps:
(1) Dissolving polyvinyl formal in acetonitrile, performing ultrasonic dispersion, and uniformly stirring to obtain a solution;
(2) Weighing 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride into a reactor, adding ultrapure water, fully stirring, then adding N-hydroxysuccinimide, fully stirring, and performing ultrasonic treatment to obtain a carboxyl activation solution;
(3) Adding hydrotalcite and ultrapure water into a reactor, adding the carboxyl activating solution prepared in the step (2) while stirring, adding allylamine after uniformly mixing, reacting to obtain allylamine modified hydrotalcite, centrifuging, washing with water to remove the activating solution, and storing for later use;
(4) Adding lithium hexafluorophosphate, allyl amine modified hydrotalcite and polydimethylsiloxane into the solution prepared in the step (1) according to weight components, and uniformly stirring to form slurry;
(5) And coating the slurry on a glass plate to form a liquid film, and drying the liquid film in vacuum to obtain the lithium ion battery electrolyte.
Preferably, the ultrasonic dispersion time in the step (1) is 10-30min, the stirring time is 6-10h, and the stirring temperature is 40-60 ℃.
Preferably, the mass ratio of 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride to N-hydroxysuccinimide to ultrapure water in the step (2) is 4.5-5.5:0.003-0.004:5-8, and the ultrasonic time is 10-15min.
Preferably, the mass ratio of the hydrotalcite, the ultrapure water and the allylamine in the step (3) is 30-80:80-100:1.5-1.8, the reaction time is 3.5-4h, the centrifugal speed is 8000-9000rpm, and the centrifugal time is 3-6min.
Preferably, the mass ratio of the hydrotalcite to the carboxyl activating solution in the step (3) is 30-80:4-6.
Preferably, the stirring time in the step (4) is 6-10h, and the stirring temperature is 40-65 ℃.
Preferably, the temperature of vacuum drying in the step (5) is 50-100 ℃, and the vacuum drying time is 8-24h.
The reaction mechanism and the beneficial effects of the invention are as follows:
(1) A lithium ion battery electrolyte is a gel polymer electrolyte, which is prepared by stirring and coating allylamine modified hydrotalcite, lithium hexafluorophosphate, polymer film matrix polyvinyl formal, acetonitrile and plasticizer polydimethylsiloxane, wherein the allylamine modified hydrotalcite and the polyvinyl formal are subjected to alkene reaction and crosslinking.
(2) A lithium ion battery electrolyte, hydrotalcite material has lamellar structure, which enhances the transmission of lithium ions, lithium hexafluorophosphate has high ionic conductivity, polyvinyl formal is polymer film matrix, the pores are large, and the ionic conductivity of gel polymer electrolyte is synergistically improved.
(3) A lithium ion battery electrolyte is prepared as adding inorganic hydrotalcite into polyvinyl formal polymer, forming novel gel polymer electrolyte by interaction of two, raising mechanical stability of polymer electrolyte by inorganic hydrotalcite and promoting dissociation of lithium salt by synergistic action between inorganic hydrotalcite and lithium salt.
Detailed Description
The invention is further described below in connection with specific embodiments, which are intended to illustrate, but not to limit the invention further. The technical means used in the following examples are conventional means well known to those skilled in the art, and all the raw materials are general-purpose materials.
Example 1
A preparation method of an electrolyte of a lithium ion battery comprises the following steps:
(1) Dissolving 10g of polyvinyl formal in 50g of acetonitrile, uniformly stirring after ultrasonic dispersion, setting the ultrasonic dispersion time to be 10min, the stirring time to be 6h and the stirring temperature to be 40 ℃ to obtain a solution;
(2) Weighing 4.5mg of 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride into a reactor, adding 5g of ultrapure water into the reactor, fully stirring, then adding 3mg of N-hydroxysuccinimide into the mixed solution, fully stirring, and performing ultrasonic treatment for 10min to obtain a carboxyl activation solution;
(3) Adding 30g of hydrotalcite and 80g of ultrapure water into a reactor, stirring and adding 4g of carboxyl activating solution prepared in the step (2), uniformly mixing, adding 1.5g of allylamine, reacting for 3.5h to obtain allylamine modified hydrotalcite, centrifuging, washing with water to remove the activating solution, and storing for later use, wherein the centrifugal speed is 8000rpm, and the centrifugal time is 3min;
(4) Adding 5g of lithium hexafluorophosphate, 10g of allylamine modified hydrotalcite and 3g of polydimethylsiloxane into the solution prepared in the step (1), and uniformly stirring for 6 hours at the stirring temperature of 40 ℃ to form slurry;
(5) And coating the slurry on a glass plate to form a liquid film, and carrying out vacuum drying on the liquid film at the temperature of 50 ℃ for 8h to obtain the lithium ion battery electrolyte.
Example 2
A preparation method of an electrolyte of a lithium ion battery comprises the following steps:
(1) Dissolving 11g of polyvinyl formal in 60g of acetonitrile, uniformly stirring after ultrasonic dispersion, setting the ultrasonic dispersion time to be 15min, the stirring time to be 7h and the stirring temperature to be 45 ℃ to obtain a solution;
(2) Weighing 4.8mg of 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride into a reactor, adding 6g of ultrapure water into the reactor, fully stirring, then adding 3.2mg of N-hydroxysuccinimide into the mixed solution, fully stirring, and performing ultrasonic treatment for 11min to obtain a carboxyl activating solution;
(3) Adding 40g of hydrotalcite and 85g of ultrapure water into a reactor, stirring and adding 5g of carboxyl activating solution prepared in the step (2), uniformly mixing, adding 1.6g of allylamine, reacting for 3.6h to obtain allylamine modified hydrotalcite, centrifuging, washing with water to remove the activating solution, and storing for later use, wherein the centrifugal speed is 8200rpm, and the centrifugal time is 4min;
(4) Adding 6g of lithium hexafluorophosphate, 11g of allylamine modified hydrotalcite and 4g of polydimethylsiloxane into the solution prepared in the step (1), and uniformly stirring for 7h at the stirring temperature of 45 ℃ to form slurry;
(5) And coating the slurry on a glass plate to form a liquid film, and carrying out vacuum drying on the liquid film at the temperature of 60 ℃ for 10h to obtain the lithium ion battery electrolyte.
Example 3
A preparation method of an electrolyte of a lithium ion battery comprises the following steps:
(1) Dissolving 12g of polyvinyl formal in 70g of acetonitrile, uniformly stirring after ultrasonic dispersion, setting the ultrasonic dispersion time to be 20min, the stirring time to be 8h and the stirring temperature to be 55 ℃ to obtain a solution;
(2) Weighing 5mg of 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride into a reactor, adding 7g of ultrapure water into the reactor, fully stirring, then adding 3.3mg of N-hydroxysuccinimide into the mixed solution, fully stirring, and performing ultrasonic treatment for 12min to obtain a carboxyl activation solution;
(3) Adding 50g of hydrotalcite and 90g of ultrapure water into a reactor, stirring and adding 5.5g of carboxyl activating solution prepared in the step (2), uniformly mixing, adding 1.7g of allylamine, reacting for 3.8h to obtain allylamine modified hydrotalcite, centrifuging, washing with water to remove the activating solution, and storing for later use, wherein the centrifugal speed is 8500rpm, and the centrifugation time is 5min;
(4) Adding 9g of lithium hexafluorophosphate, 13g of allylamine modified hydrotalcite and 5g of polydimethylsiloxane into the solution prepared in the step (1), and uniformly stirring for 8h at the stirring temperature of 45 ℃ to form slurry;
(5) And coating the slurry on a glass plate to form a liquid film, and carrying out vacuum drying on the liquid film at the temperature of 80 ℃ for 15h to obtain the lithium ion battery electrolyte.
Example 4
A preparation method of an electrolyte of a lithium ion battery comprises the following steps:
(1) Dissolving 15g of polyvinyl formal in 100g of acetonitrile, uniformly stirring after ultrasonic dispersion, setting the ultrasonic dispersion time to be 30min, the stirring time to be 10h and the stirring temperature to be 60 ℃ to obtain a solution;
(2) Weighing 5.5mg of 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride into a reactor, adding 8g of ultrapure water into the reactor, fully stirring, then adding 4 mg of N-hydroxysuccinimide into the mixed solution, fully stirring, and performing ultrasonic treatment for 13min to obtain a carboxyl activation solution;
(3) Adding 80g of hydrotalcite and 100g of ultrapure water into a reactor, stirring and adding 6g of carboxyl activating solution prepared in the step (2), uniformly mixing, adding 1.8g of allylamine, reacting for 4h to obtain allylamine modified hydrotalcite, centrifuging, washing with water to remove the activating solution, and storing for later use, wherein the centrifugal speed is 9000rpm, and the centrifugal time is 6min;
(4) Adding 10g of lithium hexafluorophosphate, 15g of allylamine modified hydrotalcite and 6g of polydimethylsiloxane into the solution prepared in the step (1), and uniformly stirring for 10h at the stirring temperature of 65 ℃ to form slurry;
(5) And coating the slurry on a glass plate to form a liquid film, and carrying out vacuum drying on the liquid film at the temperature of 100 ℃ for 24 hours to obtain the lithium ion battery electrolyte.
Comparative example 1
A preparation method of an electrolyte of a lithium ion battery comprises the following steps:
(1) Dissolving 10g of polyvinyl formal in 50g of acetonitrile, uniformly stirring after ultrasonic dispersion, setting the ultrasonic dispersion time to be 10min, the stirring time to be 6h and the stirring temperature to be 40 ℃ to obtain a solution;
(2) Weighing 4.5mg of 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride into a reactor, adding 5ml of ultrapure water into the reactor, fully stirring, then adding 3mg of N-hydroxysuccinimide into the mixed solution, fully stirring, then carrying out ultrasonic treatment for 10min to obtain carboxyl activation solution, adding 30g of hydrotalcite and 80g of ultrapure water into the reactor, adding the carboxyl activation solution while stirring, uniformly mixing, adding 1.5g of allylamine, reacting for 3.5h to obtain allylamine modified hydrotalcite, centrifuging, washing with water to remove the activation solution, and storing for later use, wherein the centrifugal speed is 8000rpm, and the centrifugation time is 3min;
(3) Adding 5g of lithium trifluoromethanesulfonate, 10g of allylamine modified hydrotalcite and 3g of polydimethylsiloxane into the solution prepared in the step (1), and uniformly stirring for 6 hours at the stirring temperature of 40 ℃ to form slurry;
(4) And coating the slurry on a glass plate to form a liquid film, and carrying out vacuum drying on the liquid film at the temperature of 50 ℃ for 8h to obtain the lithium ion battery electrolyte.
Comparative example 2
A preparation method of an electrolyte of a lithium ion battery comprises the following steps:
(1) Dissolving 10g of polyvinyl formal in 50g of acetonitrile, uniformly stirring after ultrasonic dispersion, setting the ultrasonic dispersion time to be 10min, the stirring time to be 6h and the stirring temperature to be 40 ℃ to obtain a solution;
(2) Adding 5g of lithium hexafluorophosphate, 10g of titanium dioxide and 3g of polydimethylsiloxane into the solution prepared in the step (1), and uniformly stirring for 6h at the stirring temperature of 40 ℃ to form slurry;
(3) Coating the slurry on a glass plate to form a liquid film;
(4) And (3) drying the liquid film in vacuum at the temperature of 50 ℃ for 8 hours to obtain the lithium ion battery electrolyte.
The mass ratio of the raw materials of the lithium ion battery electrolytes prepared in the examples and the comparative examples is shown in table 1, and the unit is g.
TABLE 1
The performance of the lithium ion battery electrolytes prepared in the examples and the comparative examples is characterized:
film thickness: the thickness of the gel polymer electrolyte was measured using a micrometer (precision 0.01 mm), and 5 points on any sample were averaged.
Ionic conductivity: the electrolyte is clamped by two pieces of stainless steel and placed in a 2032 type battery case, and the conductivity of the lithium ion is measured by adopting an electrochemical alternating current impedance spectrum by adopting a formula of sigma = L/ARb, wherein L is the thickness of the electrolyte, A is the room temperature area of a stainless steel sheet, and Rb is the measured impedance.
Electrochemical window: an electrolyte is clamped by a stainless steel sheet and a lithium sheet, the stainless steel sheet and the lithium sheet are placed in a 2032 type battery case, an electrochemical window is used for carrying out linear volt-ampere scanning measurement by an electrochemical workstation, the initial potential is 2.5V, the maximum potential is 5.5V, and the scanning speed is 1mV/s. The test results are listed in table 2:
TABLE 2
As can be seen from the results in Table 2, the gel polymer electrolyte prepared according to the present invention has a lithium ion conductivity in the range of 3X 10 at room temperature -4 -6×10 -4 S/cm, and meanwhile, the polymer electrolyte shows excellent high-voltage resistance, the electrochemical window range is 4.5-5.1V, and the requirement of a high-voltage lithium ion battery can be met. The ionic conductivity of the gel polymer electrolytes of examples 1 to 4 increased as the mass of allylamine-modified hydrotalcite and lithium hexafluorophosphate was increased, the lithium salt added in comparative example 1 was lithium trifluoromethanesulfonate, which was inferior in lithium ion conductivity as compared with lithium hexafluorophosphate, and the inorganic substance in comparative example 2 was titanium dioxide, which did not have a layered structure, was slow in ion transmission rate, and was inferior in lithium ion conductivity. The lithium ion conductivities of comparative example 1 and comparative example 2 were inferior to those of examples 1 to 4, indicating that the gel polymer electrolytes prepared according to the present invention have higher lithium ion conductivities.
The method for testing the performance of the battery comprises the following steps:
(1) Preparing a positive plate: dissolving polyvinylidene fluoride in N, N-2-methyl pyrrolidone at a concentration of 0.1mol/L, mixing the polyvinylidene fluoride, the positive electrode active material and the conductive carbon black in a mass ratio of 10. Uniformly coating the obtained slurry on an aluminum foil with the thickness of 100 mu m, drying at 60 ℃, drying in a vacuum oven at 120 ℃, rolling, punching, weighing, continuously drying in the vacuum oven at 120 ℃, and placing in a glove box for later use;
(2) Preparing a negative plate: dissolving polyvinylidene fluoride in N, N-2-methyl pyrrolidone, wherein the concentration is 0.1mol/L, mixing polyvinylidene fluoride, a negative electrode active material and conductive carbon black according to the mass ratio of 10 to 80, grinding for at least 1 hour, uniformly coating the obtained slurry on a copper foil, wherein the thickness is 100 mu m, drying at 60 ℃, drying in a 120 ℃ vacuum oven, rolling, punching, weighing, continuously drying in the 120 ℃ vacuum oven, and placing in a glove box for later use;
(3) Assembling the gel polymer electrolyte, the positive plate and the negative plate prepared in the examples and the comparative examples into a battery;
(4) And testing the charge and discharge performance of the battery.
The test method is as follows: the constant current charge-discharge cycle was carried out between 0.01 and 1.5V using a LAND cell charge-discharge instrument with a current density of 250mA/g (0.25C rate), and the results of rate capability and long cycle performance are shown in Table 3:
TABLE 3
As can be seen from the results of table 3, the coulombic efficiencies of the gel polymer electrolytes prepared in examples 1 to 4 increased as the mass of lithium hexafluorophosphate and allylamine-modified hydrotalcite increased. The capacity can be kept above 90mAh/g under the condition of 100 times of circulation, and the good long-circulation stability is shown under the condition of high voltage. The lithium salt added to the gel polymer electrolyte prepared in comparative example 1 was lithium trifluoromethanesulfonate, which was poor in lithium ion conductivity, and the coulombic efficiency of the assembled lithium ion battery was low because the ionic conductivity of lithium trifluoromethanesulfonate was inferior to that of lithium hexafluorophosphate, and the inorganic substance in the gel polymer electrolyte prepared in comparative example 2 was titanium dioxide, which did not have a layered structure, and was slow in ion transmission rate, poor in lithium ion conductivity, and low in coulombic efficiency of the assembled lithium ion battery. The lithium ion batteries of comparative examples 1 and 2, both of which had poorer capacity and coulombic efficiency than those of example 1, demonstrate that the lithium ion batteries assembled with the gel polymer electrolyte prepared according to the present invention had higher capacity and coulombic efficiency.
Finally, it should be noted that: the above embodiments are only used to illustrate the present invention and do not limit the technical solutions described in the present invention; it will be understood by those skilled in the art that the present invention may be modified and equivalents may be substituted; all such modifications and variations are intended to be included herein within the scope of this disclosure and the present invention and protected by the following claims.
Claims (8)
1. The lithium ion battery electrolyte is a gel polymer electrolyte and comprises the following components in parts by weight: 10-15 parts of a polymer film matrix, 50-100 parts of acetonitrile, 5-10 parts of lithium hexafluorophosphate, 10-15 parts of allylamine modified hydrotalcite and 3-6 parts of a plasticizer, wherein the polymer film matrix is polyvinyl formal, the allylamine modified hydrotalcite is hydrotalcite containing allyl functional groups, the plasticizer is polydimethylsiloxane, and the allylamine modified hydrotalcite and the polyvinyl formal are subjected to an ene reaction and crosslinking.
2. A method of preparing the lithium ion battery electrolyte of claim 1, comprising the steps of:
(1) Dissolving polyvinyl formal in acetonitrile according to weight components, and after ultrasonic dispersion, uniformly stirring to obtain a solution;
(2) Weighing 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride into a reactor, adding ultrapure water, fully stirring, then adding N-hydroxysuccinimide, fully stirring, and performing ultrasonic treatment to obtain a carboxyl activation solution;
(3) Adding hydrotalcite and ultrapure water into a reactor, adding the carboxyl activating solution prepared in the step (2) while stirring, adding allylamine after uniformly mixing, reacting to obtain allylamine modified hydrotalcite, centrifuging, washing with water to remove the activating solution, and storing for later use;
(4) Adding lithium hexafluorophosphate, allyl amine modified hydrotalcite and polydimethylsiloxane into the solution prepared in the step (1) according to weight components, and uniformly stirring to form slurry;
(5) And coating the slurry on a glass plate to form a liquid film, and drying the liquid film in vacuum to obtain the lithium ion battery electrolyte.
3. The preparation method of the lithium ion battery electrolyte according to claim 2, wherein the ultrasonic dispersion time in the step (1) is 10-30min, the stirring time is 6-10h, and the stirring temperature is 40-60 ℃.
4. The method for preparing the electrolyte of the lithium ion battery according to claim 2, wherein the mass ratio of 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride, N-hydroxysuccinimide and ultrapure water in the step (2) is 4.5-5.5:0.003-0.004:5-8, and the ultrasonic time is 10-15min.
5. The method for preparing the lithium ion battery electrolyte according to claim 2, wherein the mass ratio of the hydrotalcite, the ultrapure water and the allylamine in the step (3) is 30-80:80-100:1.5-1.8, the reaction time is 3.5-4h, the centrifugal speed is 8000-9000rpm, and the centrifugal time is 3-6min.
6. The method for preparing the lithium ion battery electrolyte according to claim 2, wherein the mass ratio of the hydrotalcite to the carboxyl activating solution in the step (3) is 30-80:4-6.
7. The method for preparing the lithium ion battery electrolyte according to claim 2, wherein the stirring time in the step (4) is 6-10h, and the stirring temperature is 40-65 ℃.
8. The method for preparing the lithium ion battery electrolyte according to claim 2, wherein the temperature of the vacuum drying in the step (5) is 50-100 ℃, and the vacuum drying time is 8-24h.
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