CN111653787B - Silicon-based negative electrode three-dimensional network polyacrylic acid binder and preparation method thereof - Google Patents
Silicon-based negative electrode three-dimensional network polyacrylic acid binder and preparation method thereof Download PDFInfo
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- CN111653787B CN111653787B CN202010614009.7A CN202010614009A CN111653787B CN 111653787 B CN111653787 B CN 111653787B CN 202010614009 A CN202010614009 A CN 202010614009A CN 111653787 B CN111653787 B CN 111653787B
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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
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/621—Binders
- H01M4/622—Binders being polymers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F120/00—Homopolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride, ester, amide, imide or nitrile thereof
- C08F120/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F120/04—Acids; Metal salts or ammonium salts thereof
- C08F120/06—Acrylic acid; Methacrylic acid; Metal salts or ammonium salts thereof
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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
- H01M10/052—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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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
A silicon-based negative electrode three-dimensional network polyacrylic acid binder and a preparation method thereof are disclosed, wherein according to the mass parts, 5-13 parts of polyacrylic acid, 20-50 parts of water and 1-5 parts of polyhydric alcohol containing a trihydroxy structure are added into a reaction container, the temperature is raised to 65-80 ℃ after uniform stirring, 0.01-0.1 part of initiator is added, 50-60 parts of water is added after heat preservation reaction is carried out for 60-180 min, and then the mixture is stirred for 180-360 min at 20-50 ℃. According to the invention, the polyhydroxy structure and the carboxyl groups on the polyacrylic acid chains generate network crosslinking through the action of hydrogen bonds, so that the processing performance of the polyacrylic acid binder is improved, the stripping strength of a pole piece is improved when the prepared binder is used for a silicon negative electrode, an active substance is firmly wrapped by a network system, the volume effect of a lithium ion battery in the charging and discharging process is relieved, the service life is prolonged, and the cycle performance is prolonged.
Description
Technical Field
The invention relates to the field of lithium ion battery materials, in particular to a silicon-based negative electrode three-dimensional network polyacrylic acid binder and a preparation method thereof.
Background
With the gradual application of lithium ion batteries in hybrid electric vehicles and pure electric vehicles, people pay more and more attention to the endurance mileage, and the demand for high-energy-density lithium ion batteries is increasing. The theoretical specific capacity of the current commercialized graphite negative electrode material is only 372mAh/g, and the modification space is a bottleneck and cannot meet the market requirement. The new silicon (Si) based negative electrode material has a theoretical specific capacity of 4200mAh/g, high specific capacity and a proper lithium intercalation and deintercalation platform, and is an ideal high-capacity negative electrode material of a lithium ion battery. However, during the charging and discharging process, the volume change of Si reaches more than 300%, and the internal stress generated by the violent volume change easily causes electrode pulverization and peeling, so that the cycling stability is influenced.
In order to solve this problem, new high-efficiency binders have become a focus of research. Polyacrylic acid (PAA) has a molecular structure containing a large number of carboxyl groups (-COOH) and can form covalent bonds with hydroxyl groups (-OH) of an oxide layer on the surface of silicon particles, and has been studied extensively as a silicon-based binder. But the linear PAA molecular chain has stronger rigidity and the processing performance of the pole piece after pulping and coating is poorer.
Disclosure of Invention
In order to overcome the problems in the prior art, the invention aims to provide a silicon-based negative electrode three-dimensional network polyacrylic acid binder and a preparation method thereof, so as to improve the peel strength of a pole piece and prolong the cycle life of a battery.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a silicon-based negative electrode three-dimensional network polyacrylic acid binder comprises the steps of adding 5-13 parts by mass of acrylic acid, 20-50 parts by mass of water and 1-5 parts by mass of polyhydric alcohol containing a trihydroxy structure into a reaction container, stirring for 30-120 min, heating to 65-80 ℃, adding 0.01-0.1 part by mass of an initiator, carrying out heat preservation reaction at 65-80 ℃ for 30-180 min, adding 30-60 parts by mass of water, and stirring for 180-360 min at 20-50 ℃ to obtain the silicon-based negative electrode three-dimensional network polyacrylic acid binder.
The invention is further improved in that the structural formula of the polyhydric alcohol containing the trihydroxy structure is as follows:
wherein R is1Is an alkyl group; r2、R3、R4Is alkyl, alkoxy or cycloalkyl.
In a further development of the invention, R1Is a linear or branched alkyl of C1-C4, R2、R3、R4Is C1 &A C5 linear or branched chain alkyl, a C1-C5 linear or branched chain alkoxy or a C1-C5 naphthenic base.
In a further development of the invention, M is a polyol containing a trihydroxy structurew＝1000～3000。
The invention is further improved in that the initiator is one of potassium persulfate, sodium persulfate, ammonium persulfate and azodiisopropyl imidazoline hydrochloride.
The silicon-based negative electrode three-dimensional network polyacrylic acid binder prepared by the method has the peel strength of 15.5-25.1N/m.
Compared with the prior art, the invention has the following beneficial effects:
the invention introduces the polyhydric alcohol containing the trihydroxy structure, and the hydroxyl on the structure and the carboxyl on the polyacrylic acid chain generate network crosslinking through the action of hydrogen bonds, thereby not only improving the processing performance of the polyacrylic acid binder, but also improving the peeling strength of a pole piece when the binder prepared by the invention is used for a silicon cathode, firmly wrapping an active substance by a network system, relieving the expansion effect in the charge-discharge process of a lithium ion battery, prolonging the service life and prolonging the cycle performance. In the invention, 20-50 parts of water is added for the first time, so as to control the concentration of acrylic acid monomer reaction and enable the molecular weight of polyacrylic acid to be in a certain range. And 30-60 parts of water is added for the second time to dilute the polyacrylic acid binder, so that the cathode can be conveniently homogenized and coated. According to the invention, the polyhydric alcohol containing the trihydroxy structure is introduced, and the polyhydric alcohol containing the trihydroxy structure and the polyacrylic acid chain form a three-dimensional network structure through hydrogen bonds, so that the peeling strength of the linear polyacrylic acid structure and the coating capacity of an active substance are improved, and the ether bond structure can also increase the flexibility of the polyacrylic acid chain and improve the processing performance of the adhesive. The polyacrylic acid molecular chain generated by polypropylene reaction contains more carboxyl (-COOH), polyhydric alcohol (-OH), and polyol, -COOH and-OH form a network system through strong hydrogen bond action, so that active substances are firmly bound, the expansion rate of the pole piece in the charge and discharge process is reduced, and the cycle performance of the battery is improved.
Drawings
All figures and reference numerals in the figures referred to in the present invention are described below.
FIG. 1 is a schematic diagram of the structure of a three-dimensional adhesive prepared according to the present invention.
Fig. 2 shows the cycle performance of the battery.
Detailed Description
The present invention will be described in detail with reference to specific embodiments.
The invention comprises the following steps:
step 1, weighing 5-13 parts of acrylic acid, 20-50 parts of deionized water and 1-5 parts of polyhydric alcohol containing a trihydroxy structure in parts by weight, and stirring in a three-neck flask for 30-120 min to obtain a uniform mixed solution.
The structural formula of the polyhydric alcohol containing the trihydroxy structure is shown as follows:
wherein R is1Is a linear or branched alkyl group of less than or equal to 4 carbon atoms; namely R1Is C1-C4 straight chain or branched chain alkyl.
R2、R3、R4Each independently selected from phenyl, alkyl of less than or equal to 5 carbon atoms, alkoxy of less than or equal to 5 carbon atoms, i.e. R2、R3、R4Is C1-C5 straight chain or branched chain alkyl or R2、R3、R4Is a linear or branched alkoxy group of C1-C5, or R2、R3、R4Is C1-C5 naphthenic base; wherein R is2、R3And R4May be the same or different.
Hydroxyl on the polyhydric alcohol containing a trihydroxy structure and carboxyl on the polyacrylic chain generated by the reaction act through hydrogen bonds:
step 2, heating the uniform mixed solution obtained in the step 1 to 65-80 ℃;
step 3, weighing 0.01-0.1 part of initiator, adding the initiator into the mixed solution obtained in the step 2, and carrying out heat preservation reaction at 65-80 ℃ for 30-180 min; the initiator is one of potassium persulfate, sodium persulfate, ammonium persulfate and azodiisopropyl imidazoline hydrochloride;
and 4, weighing 30-60 parts of deionized water, adding the deionized water into the reactant in the step 3, and stirring the mixture for 180-360 min at the temperature of 20-50 ℃ to obtain uniform and stable mixed liquid, namely the silicon-based negative electrode three-dimensional network polyacrylic acid binder. The three-dimensional structure of the silicon-based negative electrode three-dimensional reticular polyacrylic acid binder prepared by the invention is shown in figure 1.
The polyacrylic acid prepared by the invention contains more carboxyl (-COOH) groups on the molecular chain and is introduced with polyhydroxy (-OH) trihydroxy polyol (M)w1000-3000, as shown in the formula), the-COOH and-OH form a network system through strong hydrogen bond action, so that the active substance is firmly bound, the expansion rate of the pole piece in the charge and discharge process is reduced, and the cycle performance of the battery is improved. Meanwhile, the molecular chain of the polyhydric alcohol with the trihydroxy structure contains a large number of ether bonds, so that the processing performance of the polyacrylic acid adhesive is improved.
The following are specific examples.
Example 1
Weighing 5 parts of acrylic acid, 44 parts of deionized water and 1 part of polyhydric alcohol containing a trihydroxy structure in parts by mass, stirring the mixture in a three-neck flask for 30min to obtain a uniform mixed solution, heating the mixed solution to 65 ℃, adding 0.01 part of potassium persulfate, carrying out heat preservation reaction for 120min, adding 50 parts of deionized water, and stirring the mixture at 50 ℃ for 180min to obtain the silicon-based negative electrode three-dimensional network polyacrylic acid binder. Wherein, the structure of the polyhydric alcohol containing the trihydroxy structure is as follows:
example 2
Weighing 9 parts of acrylic acid, 40 parts of deionized water and 2 parts of polyhydric alcohol containing a trihydroxy structure in parts by mass, stirring in a three-neck flask for 30min to obtain a uniform mixed solution, heating to 70 ℃, adding 0.1 part of sodium persulfate, carrying out heat preservation reaction for 120min, adding 60 parts of deionized water, and stirring at 20 ℃ for 300min to obtain the silicon-based negative electrode three-dimensional network polyacrylic acid binder. Wherein, the structure of the polyhydric alcohol containing the trihydroxy structure is as follows:
example 3
Weighing 6 parts of acrylic acid, 30 parts of deionized water and 4 parts of polyhydric alcohol containing a trihydroxy structure in parts by mass, stirring in a three-neck flask for 60min to obtain a uniform mixed solution, heating to 75 ℃, adding 0.05 part of azodiisopropyl imidazoline hydrochloric acid, reacting for 60min under heat preservation, adding 55 parts of deionized water, and stirring at 30 ℃ for 360min to obtain the silicon-based negative electrode three-dimensional network polyacrylic acid binder. Wherein, the structure of the polyhydric alcohol containing the trihydroxy structure is as follows:
example 4
Weighing 7 parts of acrylic acid, 50 parts of deionized water and 3 parts of polyhydric alcohol containing a trihydroxy structure in parts by mass, stirring for 90min in a three-neck flask to obtain a uniform mixed solution, heating to 80 ℃, adding 0.08 part of potassium persulfate, carrying out heat preservation reaction for 180min, adding 60 parts of deionized water, and stirring for 180min at 50 ℃ to obtain the silicon-based negative electrode three-dimensional network polyacrylic acid binder. Wherein, the structure of the polyhydric alcohol containing the trihydroxy structure is as follows:
example 5
Weighing 13 parts of acrylic acid, 50 parts of deionized water and 2 parts of polyhydric alcohol containing a trihydroxy structure in parts by weight, stirring for 50min to obtain a uniform mixed solution in a three-neck flask, heating to 75 ℃, adding 0.06 part of ammonium persulfate, carrying out heat preservation reaction for 180min, adding 60 parts of deionized water, and stirring for 300min at 20 ℃ to obtain the silicon-based negative electrode three-dimensional network polyacrylic acid binder. Wherein, the structure of the polyhydric alcohol containing the trihydroxy structure is as follows:
example 6
Weighing 12 parts of acrylic acid, 40 parts of deionized water and 1 part of polyhydric alcohol containing a trihydroxy structure in parts by mass, stirring the mixture in a three-neck flask for 120min until the mixture is uniform, heating the mixture to 80 ℃, adding 0.01 part of azodiisopropyl imidazoline hydrochloric acid, reacting the mixture for 120min under heat preservation, adding 50 parts of deionized water, and stirring the mixture for 180min at 50 ℃ to obtain the silicon-based negative electrode three-dimensional network polyacrylic acid binder. Wherein, the structure of the polyhydric alcohol containing the trihydroxy structure is as follows:
example 7
Weighing 9 parts of acrylic acid, 40 parts of deionized water and 1 part of polyhydric alcohol with a trihydroxy structure according to the mass parts, and stirring for 40min to obtain a uniform mixed solution in a three-neck flask; heating to 85 ℃, adding 0.01 part of ammonium persulfate, and reacting for 30min under heat preservation; then 50 parts of deionized water is added, and the mixture is stirred for 300min at 25 ℃, so that the silicon-based negative three-dimensional reticular polyacrylic acid binder is obtained. Wherein, the structure of the polyhydric alcohol containing the trihydroxy structure is as follows:
example 8
Weighing 10 parts of acrylic acid, 20 parts of deionized water and 5 parts of polyhydric alcohol containing a trihydroxy structure in parts by weight, stirring the mixture in a three-neck flask for 400min until the mixture is uniform, heating the mixture to 67 ℃, adding 0.03 part of azodiisopropyl imidazoline hydrochloric acid, reacting the mixture for 150min under heat preservation, adding 30 parts of deionized water, and stirring the mixture for 250min at 40 ℃ to obtain the silicon-based negative electrode three-dimensional network polyacrylic acid binder. Wherein, the structure of the polyhydric alcohol containing the trihydroxy structure is as follows:
the aqueous binder prepared in the above example 1 is applied to the preparation of a negative electrode plate. The conductive paste is prepared from a current collector and negative electrode paste loaded on the current collector, wherein the negative electrode paste is prepared by mixing a negative electrode active material, a conductive additive and the aqueous binder prepared by the method, and the mass ratio of the negative electrode active material to the conductive additive to the aqueous binder is 80: 10: 10. a secondary battery is characterized by comprising a positive pole piece, a separation film, electrolyte and the negative pole piece required by the above. And the pole piece is made into a battery, and the peel strength of the pole piece and the cycle performance of the battery are tested. Referring to fig. 2, it can be seen from fig. 2 that the life of the cells prepared using the three-dimensional network binder is much improved relative to the comparative CMC binder. Under the condition of the same capacity retention rate, the three-dimensional network adhesive has more circulation loops.
TABLE 1 Peel Strength values of the three-dimensional network polyacrylic acid Binders and conventional Binders obtained in Table 1
Claims (2)
1. The preparation method of the silicon-based negative electrode three-dimensional network polyacrylic acid binder is characterized by adding 5-13 parts by mass of acrylic acid, 20-50 parts by mass of water and 1-5 parts by mass of polyhydric alcohol containing a trihydroxy structure into a reaction vessel, stirring for 30-120 min, heating to 65-80 ℃, adding 0.01-0.1 part by mass of an initiator, carrying out heat preservation reaction at 65-80 ℃ for 30-180 min, adding 30-60 parts by mass of water, and stirring for 180-360 min at 20-50 ℃ to obtain the silicon-based negative electrode three-dimensional network polyacrylic acid binder;
the structural formula of the polyhydric alcohol containing the trihydroxy structure is as follows:
wherein R is1Is a linear or branched alkyl of C1-C4, R2、R3、R4Is C1-C5 straight chain or branched chain alkyl, C1-C5 straight chain or branched chain alkoxy or C1-C5 naphthenic base;
the initiator is one of potassium persulfate, sodium persulfate, ammonium persulfate and azodiisopropyl imidazoline hydrochloride;
m of polyhydric alcohols containing trihydroxy structurew＝1000～3000。
2. The silicon-based negative electrode three-dimensional network polyacrylic acid binder prepared by the method of claim 1, wherein the peel strength of the silicon-based negative electrode three-dimensional network polyacrylic acid binder is 15.5-25.1N/m.
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