CN116285184A - Preparation method and application of all-organic four-item blended energy storage composite material - Google Patents
Preparation method and application of all-organic four-item blended energy storage composite material Download PDFInfo
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- CN116285184A CN116285184A CN202310284215.XA CN202310284215A CN116285184A CN 116285184 A CN116285184 A CN 116285184A CN 202310284215 A CN202310284215 A CN 202310284215A CN 116285184 A CN116285184 A CN 116285184A
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- 239000002131 composite material Substances 0.000 title claims abstract description 75
- 238000004146 energy storage Methods 0.000 title claims abstract description 66
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 229920002981 polyvinylidene fluoride Polymers 0.000 claims abstract description 64
- 239000002033 PVDF binder Substances 0.000 claims abstract description 59
- 229920005569 poly(vinylidene fluoride-co-hexafluoropropylene) Polymers 0.000 claims abstract description 55
- 229920003229 poly(methyl methacrylate) Polymers 0.000 claims abstract description 48
- 239000004926 polymethyl methacrylate Substances 0.000 claims abstract description 48
- 239000011259 mixed solution Substances 0.000 claims abstract description 43
- 229920000120 polyethyl acrylate Polymers 0.000 claims abstract description 25
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims abstract description 23
- 239000000758 substrate Substances 0.000 claims abstract description 23
- 238000002156 mixing Methods 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 12
- 238000003756 stirring Methods 0.000 claims abstract description 10
- 239000011248 coating agent Substances 0.000 claims abstract description 6
- 238000000576 coating method Methods 0.000 claims abstract description 6
- 239000000243 solution Substances 0.000 claims description 12
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 claims description 9
- ZNSMNVMLTJELDZ-UHFFFAOYSA-N Bis(2-chloroethyl)ether Chemical compound ClCCOCCCl ZNSMNVMLTJELDZ-UHFFFAOYSA-N 0.000 claims description 5
- 239000003990 capacitor Substances 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- 239000011521 glass Substances 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 238000003760 magnetic stirring Methods 0.000 claims description 2
- 238000010907 mechanical stirring Methods 0.000 claims 1
- 229920000642 polymer Polymers 0.000 abstract description 10
- 229920006254 polymer film Polymers 0.000 abstract description 2
- 229920001971 elastomer Polymers 0.000 description 11
- 230000000052 comparative effect Effects 0.000 description 10
- 229920002595 Dielectric elastomer Polymers 0.000 description 5
- 239000007787 solid Substances 0.000 description 5
- 229920001577 copolymer Polymers 0.000 description 3
- 230000007423 decrease Effects 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 239000003989 dielectric material Substances 0.000 description 2
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- 238000002329 infrared spectrum Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 229920000915 polyvinyl chloride Polymers 0.000 description 2
- 239000004800 polyvinyl chloride Substances 0.000 description 2
- BQCIDUSAKPWEOX-UHFFFAOYSA-N 1,1-Difluoroethene Chemical group FC(F)=C BQCIDUSAKPWEOX-UHFFFAOYSA-N 0.000 description 1
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical group COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-M acrylate group Chemical group C(C=C)(=O)[O-] NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 description 1
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- 238000005516 engineering process Methods 0.000 description 1
- 239000011256 inorganic filler Substances 0.000 description 1
- 229910003475 inorganic filler Inorganic materials 0.000 description 1
- 125000005395 methacrylic acid group Chemical group 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
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- 238000001291 vacuum drying Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G4/00—Fixed capacitors; Processes of their manufacture
- H01G4/002—Details
- H01G4/018—Dielectrics
- H01G4/06—Solid dielectrics
- H01G4/14—Organic dielectrics
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2327/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers
- C08J2327/02—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment
- C08J2327/12—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
- C08J2327/16—Homopolymers or copolymers of vinylidene fluoride
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2333/00—Characterised by the use of homopolymers or copolymers 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 of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
- C08J2333/04—Characterised by the use of homopolymers or copolymers 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 of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers esters
- C08J2333/06—Characterised by the use of homopolymers or copolymers 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 of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers esters of esters containing only carbon, hydrogen, and oxygen, the oxygen atom being present only as part of the carboxyl radical
- C08J2333/08—Homopolymers or copolymers of acrylic acid esters
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2333/00—Characterised by the use of homopolymers or copolymers 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 of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
- C08J2333/04—Characterised by the use of homopolymers or copolymers 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 of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers esters
- C08J2333/06—Characterised by the use of homopolymers or copolymers 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 of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers esters of esters containing only carbon, hydrogen, and oxygen, the oxygen atom being present only as part of the carboxyl radical
- C08J2333/10—Homopolymers or copolymers of methacrylic acid esters
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- C08J2427/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers
- C08J2427/02—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment
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- C08J2433/00—Characterised by the use of homopolymers or copolymers 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 of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
- C08J2433/04—Characterised by the use of homopolymers or copolymers 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 of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers esters
- C08J2433/06—Characterised by the use of homopolymers or copolymers 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 of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers esters of esters containing only carbon, hydrogen, and oxygen, the oxygen atom being present only as part of the carboxyl radical
- C08J2433/10—Homopolymers or copolymers of methacrylic acid esters
- C08J2433/12—Homopolymers or copolymers of methyl methacrylate
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Abstract
A preparation method and application of a full-organic four-item blended energy storage composite material relate to the technical field of polyvinylidene fluoride polymer energy storage. The invention aims to solve the problems of dielectric loss and conductivity increase and charge and discharge efficiency reduction of the traditional pure polyvinylidene fluoride polymer film. The method comprises the following steps: adding polyvinylidene fluoride-hexafluoropropylene copolymer, polyvinylidene fluoride and polymethyl methacrylate into the mixed solution a of polyethyl acrylate and chlorodiethyl ether, and uniformly stirring to obtain a mixed solution b; then vacuumizing the mixed solution b to obtain a mixed solution c; and uniformly coating the mixed solution c on one surface of the pretreated substrate, and stripping the film on the substrate after curing to obtain the all-organic four-item blended energy storage composite material. The invention can obtain a preparation method and application of the all-organic four-item blending energy storage composite material.
Description
Technical Field
The invention relates to the technical field of energy storage of polyvinylidene fluoride polymers, in particular to a preparation method and application of an all-organic four-item blending energy storage composite material.
Background
With the continuous development of modern electronic and power system technologies, polymer dielectrics have higher energy storage density and higher breakdown strength, so that polymer-based film capacitors have more and more important application values in the field of modern electronic and power systems. Despite the great efforts made to improve the energy storage and properties of polymer composites, it remains a great challenge to improve the energy storage properties of polymer composites on the premise of large-scale industrial production. Meanwhile, researchers found that the molecular formula main chain contains (CH 2 CF 2 ) n The polyvinylidene fluoride-based polymer has been widely used in the fields of physics, chemistry and engineering because of its good thermal stability, oxidation resistance, radiation resistance, piezoelectricity and thermoelectric properties. In particular, in the aspect of dielectric capacitors, the high discharge energy density has a huge application prospect. However, in high frequency electrical systems, dielectric losses typically occur in the polymer composite, resulting in a decrease in the energy storage properties of the polymer composite. The prior researches mainly focus on doping nano inorganic filler, but the problems of obviously increased dielectric loss and conductivity and reduced charge-discharge efficiency of the composite film are not solved effectively.
Disclosure of Invention
The invention aims to solve the problems of dielectric loss and conductivity increase and charge and discharge efficiency reduction of the traditional pure polyvinylidene fluoride polymer film, and provides a preparation method and application of an all-organic four-item blended energy storage composite material.
The preparation method of the all-organic four-item blending energy storage composite material comprises the following steps:
step one: preparing a mixed solution of polyethyl acrylate and chloroethyl ether;
adding the polyethyl acrylate-chloroethyl ether into the N, N-dimethylacetamide solution, and magnetically stirring until the polyethyl acrylate-chloroethyl ether is completely dissolved to obtain a polyethyl acrylate-chloroethyl ether mixed solution a;
step two: preparing a polyvinylidene fluoride-hexafluoropropylene copolymer/polyvinylidene fluoride/polyethyl acrylate-chloroethyl ether/polymethyl methacrylate four-item blending energy storage composite material;
adding polyvinylidene fluoride-hexafluoropropylene copolymer, polyvinylidene fluoride and polymethyl methacrylate into the mixed solution a of polyethyl acrylate and chlorodiethyl ether, and uniformly stirring to obtain a mixed solution b; then vacuumizing the mixed solution b to obtain a mixed solution c; uniformly coating the mixed solution c on one surface of the pretreated substrate, and stripping a film on the substrate after curing to obtain the all-organic four-item blended energy storage composite material, wherein the mass fraction ratio of polyvinylidene fluoride-hexafluoropropylene copolymer, polyvinylidene fluoride, polyethyl acrylate-chloroethyl ether and polymethyl methacrylate in the all-organic four-item blended energy storage composite material is (25-35): (25-35): (15-25): (15-25).
An application of an all-organic four-item blended energy storage composite material in dielectrics and capacitors.
The invention has the beneficial effects that:
(1) According to the preparation method of the all-organic four-item blending energy storage composite material based on polyvinylidene fluoride-hexafluoropropylene copolymer/polyvinylidene fluoride/polyethyl acrylate-chloroethyl ether/polymethyl methacrylate, firstly, polyethyl acrylate-chloroethyl ether is added into N, N-dimethylacetamide solution, and because the polyethyl acrylate-chloroethyl ether rubber dielectric elastomer is relatively difficult to dissolve, the polyethyl acrylate-chloroethyl ether rubber dielectric elastomer needs to be fully stirred at the temperature of about 50 ℃. And then preparing a composite film by using a solution blending method, taking polyvinylidene fluoride and polyvinylidene fluoride-hexafluoropropylene copolymer as a matrix, adding a solution of polyethyl acrylate-chloroethyl ether and polymethyl methacrylate into the matrix, and preparing the composite film by using a solution blending method.
In the preparation of all-organic polymer blends, compatibility between organics is a primary concern. The invention adopts the poly ethyl acrylate-chloroethyl ether and polymethyl methacrylate to have good dispersion in the polyvinylidene fluoride and the polyvinylidene fluoride-hexafluoropropylene copolymer, and the dielectric constant of the all-organic four-item blended energy storage composite material is slightly lower than that of the pure polyvinylidene fluoride-hexafluoropropylene copolymer and the polyvinylidene fluoride film, but the dielectric loss of the all-organic four-item blended energy storage composite material is greatly improved compared with that of the pure polyvinylidene fluoride-hexafluoropropylene copolymer and the pure polyvinylidene fluoride film, thus solving the problem that the energy storage density and the energy storage efficiency of the pure polyvinylidene fluoride-hexafluoropropylene copolymer and the pure polyvinylidene fluoride film are lower and realizing the remarkable improvement of the energy storage performance.
(2) The all-organic four-item blended energy storage composite material prepared by the process has excellent dielectric property and energy storage property, and can be widely applied to advanced fields such as electric, electronic and new energy automobiles. The preparation method is simple in process, economical, practical, effective in saving of resources, suitable for large-scale industrial production and capable of providing an effective strategy for developing a new application way of the all-organic energy storage composite medium.
The invention can obtain a preparation method and application of the all-organic four-item blending energy storage composite material.
Drawings
FIG. 1 is an infrared spectrum of an all-organic four-item blended energy storage composite material based on polyvinylidene fluoride-hexafluoropropylene copolymer/polyvinylidene fluoride/polyethyl acrylate-chloroethyl ether/polymethyl methacrylate of the present invention, a represents a pure polyvinylidene fluoride-hexafluoropropylene copolymer-based composite film in comparative example 1, b represents a pure polyvinylidene fluoride-based composite film in comparative example 2, c represents the mass fraction of polyvinylidene fluoride-hexafluoropropylene copolymer, polyvinylidene fluoride, polyethyl acrylate-chloroethyl ether and polymethyl methacrylate in example 1 of 35%, 15% and 15%, d represents the mass fraction of polyvinylidene fluoride-hexafluoropropylene copolymer, polyvinylidene fluoride, polyethyl acrylate-chloroethyl ether and polymethyl methacrylate in example 2 of 30%, 20% and 20%, e represents the mass fraction of polyvinylidene fluoride-hexafluoropropylene copolymer, polyvinylidene fluoride, polyethyl acrylate-chloroethyl ether and polymethyl methacrylate in example 3 of 25%, 25% and 25%;
FIG. 2 is a graph of discharge energy density for an all-organic four-term blended energy storage composite of the present invention, diamond-solid indicating a pure polyvinylidene fluoride-hexafluoropropylene copolymer based composite film in comparative example 1, +.,the mass fractions of polyvinylidene fluoride-hexafluoropropylene copolymer, polyvinylidene fluoride, polyethyl acrylate-chloroethyl ether and polymethyl methacrylate in example 1 are 35%, 15% and 15%, respectively, the mass fractions of polyvinylidene fluoride-hexafluoropropylene copolymer, polyvinylidene fluoride, polyethyl acrylate-chloroethyl ether and polymethyl methacrylate in example 2 are 30%, 20% and 20%, respectively, and the mass fractions of polyvinylidene fluoride-hexafluoropropylene copolymer, polyvinylidene fluoride, polyethyl acrylate-chloroethyl ether and polymethyl methacrylate in example 3 are 25%, 25% and 25%, respectively;
FIG. 3 is a graph of charge and discharge efficiency of an all-organic four-item blended energy storage composite of the present invention, diamond-solid indicating a pure polyvinylidene fluoride-hexafluoropropylene copolymer based composite film in comparative example 1, +.,the mass fractions of polyvinylidene fluoride-hexafluoropropylene copolymer, polyvinylidene fluoride, polyethyl acrylate-chloroethyl ether and polymethyl methacrylate in example 1 are 35%, 15% and 15%, respectively, the mass fractions of polyvinylidene fluoride-hexafluoropropylene copolymer, polyvinylidene fluoride, polyethyl acrylate-chloroethyl ether and polymethyl methacrylate in example 2 are 30%, 20% and 20%, respectively, and the mass fractions of polyvinylidene fluoride-hexafluoropropylene copolymer, polyvinylidene fluoride, polyethyl acrylate-chloroethyl ether and polymethyl methacrylate in example 3 are 25%, 25% and 25%, respectively;
FIG. 4 is a graph of the dielectric constant test of an all-organic four-item blended energy storage composite of the present invention, diamond-solid indicating a pure polyvinylidene fluoride-hexafluoropropylene copolymer based composite film in comparative example 1, +.,the mass fractions of polyvinylidene fluoride-hexafluoropropylene copolymer, polyvinylidene fluoride, polyethyl acrylate-chloroethyl ether and polymethyl methacrylate in example 1 are 35%, 15% and 15%, respectively, the mass fractions of polyvinylidene fluoride-hexafluoropropylene copolymer, polyvinylidene fluoride, polyethyl acrylate-chloroethyl ether and polymethyl methacrylate in example 2 are 30%, 20% and 20%, respectively, and the mass fractions of polyvinylidene fluoride-hexafluoropropylene copolymer, polyvinylidene fluoride, polyethyl acrylate-chloroethyl ether and polymethyl methacrylate in example 3 are 25%, 25% and 25%, respectively;
FIG. 5 is a graph showing the dielectric loss test of an all-organic four-item blended energy storage composite of the present invention, diamond-solid indicating the pure polyvinylidene fluoride-hexafluoropropylene copolymer based composite film of comparative example 1, +.,the mass fractions of polyvinylidene fluoride-hexafluoropropylene copolymer, polyvinylidene fluoride, polyethyl acrylate-chloroethyl ether and polymethyl methacrylate in example 1 are 35%, 15% and 15%, respectively, the mass fractions of polyvinylidene fluoride-hexafluoropropylene copolymer, polyvinylidene fluoride, polyethyl acrylate-chloroethyl ether and polymethyl methacrylate in example 2 are 30%, 20% and 20%, respectively, and the mass fractions of polyvinylidene fluoride-hexafluoropropylene copolymer, polyvinylidene fluoride, polyethyl acrylate-chloroethyl ether and polymethyl methacrylate in example 3 are 25%, 25% and 25%, respectively;
FIG. 6 is a graph showing conductivity measurements of an all-organic four-term blended energy storage composite according to the present invention, the diamond-solid state representing the neat polymer in comparative example 1Vinylidene fluoride-hexafluoropropylene copolymer based composite film, +.shows the pure polyvinylidene fluoride based composite film of comparative example 2,the mass fractions of polyvinylidene fluoride-hexafluoropropylene copolymer, polyvinylidene fluoride, polyethyl acrylate-chloroethyl ether and polymethyl methacrylate in example 1 were shown to be 35%, 15% and 15% in this order, the mass fractions of polyvinylidene fluoride-hexafluoropropylene copolymer, polyvinylidene fluoride, polyethyl acrylate-chloroethyl ether and polymethyl methacrylate in example 2 were shown to be 30%, 20% and 20% in this order, and the mass fractions of polyvinylidene fluoride-hexafluoropropylene copolymer, polyvinylidene fluoride, polyethyl acrylate-chloroethyl ether and polymethyl methacrylate in example 3 were shown to be 25%, 25% and 25% in this order.
Detailed Description
The first embodiment is as follows: the preparation method of the all-organic four-item blending energy storage composite material comprises the following steps:
step one: preparing a mixed solution of polyethyl acrylate and chloroethyl ether;
adding the polyethyl acrylate-chloroethyl ether into the N, N-dimethylacetamide solution, and magnetically stirring until the polyethyl acrylate-chloroethyl ether is completely dissolved to obtain a polyethyl acrylate-chloroethyl ether mixed solution a;
step two: preparing a polyvinylidene fluoride-hexafluoropropylene copolymer/polyvinylidene fluoride/polyethyl acrylate-chloroethyl ether/polymethyl methacrylate four-item blending energy storage composite material;
adding polyvinylidene fluoride-hexafluoropropylene copolymer, polyvinylidene fluoride and polymethyl methacrylate into the mixed solution a of polyethyl acrylate and chlorodiethyl ether, and uniformly stirring to obtain a mixed solution b; then vacuumizing the mixed solution b to obtain a mixed solution c; uniformly coating the mixed solution c on one surface of the pretreated substrate, and stripping a film on the substrate after curing to obtain the all-organic four-item blended energy storage composite material, wherein the mass fraction ratio of polyvinylidene fluoride-hexafluoropropylene copolymer, polyvinylidene fluoride, polyethyl acrylate-chloroethyl ether and polymethyl methacrylate in the all-organic four-item blended energy storage composite material is (25-35): (25-35): (15-25): (15-25).
The second embodiment is as follows: the present embodiment differs from the specific embodiment in that: in the first step, before the polyethyl acrylate-chloroethyl ether is added into the N, N-dimethyl acetamide solution, the mixture is dried in vacuum for 6 to 7 hours at the temperature of between 50 and 60 ℃.
The other steps are the same as in the first embodiment.
And a third specific embodiment: the present embodiment differs from the first or second embodiment in that: in the first step, the ratio of the mass of the polyethyl acrylate-chloroethyl ether to the volume of the N, N-dimethylacetamide solution is (0.15-0.25) g: (9-10) mL.
Other steps are the same as those of the first or second embodiment.
The specific embodiment IV is as follows: one difference between this embodiment and the first to third embodiments is that: in the first step, magnetic stirring is carried out for 23-24 hours at the temperature of 45-55 ℃.
Other steps are the same as those of the first to third embodiments.
Fifth embodiment: one to four differences between the present embodiment and the specific embodiment are: and step two, adding polyvinylidene fluoride-hexafluoropropylene copolymer, polyvinylidene fluoride and polymethyl methacrylate into the mixed solution a of polyethyl acrylate and chlorodiethyl ether, and mechanically stirring for 23-24 hours to obtain a mixed solution b.
Other steps are the same as those of the first to fourth embodiments.
Specific embodiment six: the present embodiment differs from the first to fifth embodiments in that: and step two, vacuumizing the mixed solution b for 4 to 5 hours to obtain a mixed solution c.
Other steps are the same as those of the first to fifth embodiments.
Seventh embodiment: one difference between the present embodiment and the first to sixth embodiments is that: the pretreated substrate in the second step is processed according to the following steps: the substrate is firstly cleaned by deionized water for 1 to 3 times, then cleaned by dust-free paper, then cleaned by absolute ethyl alcohol for 3 to 5 times, and finally dried for 1 to 2 hours at 50 to 60 ℃ to obtain the pretreated substrate, wherein the substrate is a high-temperature-resistant glass plate.
Other steps are the same as those of embodiments one to six.
Eighth embodiment: one difference between the present embodiment and the first to seventh embodiments is that: and step two, uniformly coating the mixed solution c on one surface of the pretreated substrate, and curing for 10-12 hours at 75-85 ℃.
Other steps are the same as those of embodiments one to seven.
Detailed description nine: one of the differences between this embodiment and the first to eighth embodiments is: in the second step, the mass fraction ratio of the polyvinylidene fluoride-hexafluoropropylene copolymer, the polyvinylidene fluoride, the polyethyl acrylate-chloroethyl ether and the polymethyl methacrylate in the all-organic four-item blended energy storage composite material is (35:35:15:15), (30:30:20:20) or (25:25:25).
Other steps are the same as those of embodiments one to eight.
Detailed description ten: the embodiment relates to an application of an all-organic four-item blended energy storage composite material, and the application of the all-organic four-item blended energy storage composite material in a dielectric capacitor.
The following examples are used to verify the benefits of the present invention:
example 1: the preparation method of the all-organic four-item blending energy storage composite material comprises the following steps:
step one: preparing a mixed solution of polyethyl acrylate and chloroethyl ether;
firstly, vacuum drying the poly (ethyl acrylate) -chlorodiethyl ether at 60 ℃ for 7 hours, then adding 0.25g of poly (ethyl acrylate) -chlorodiethyl ether into 10mL of N, N-dimethylacetamide solution, and magnetically stirring for 24 hours at 50 ℃ until the poly (ethyl acrylate) -chlorodiethyl ether is completely dissolved, thus obtaining a poly (ethyl acrylate) -chlorodiethyl ether mixed solution a.
Step two: and preparing the polyvinylidene fluoride-hexafluoropropylene copolymer/polyvinylidene fluoride/polyethyl acrylate-chloroethyl ether/polymethyl methacrylate four-item blending energy storage composite material.
A high temperature resistant glass plate with the size of 200mm multiplied by 16mm multiplied by 4mm is prepared, the substrate is cleaned with deionized water for 2 times before use, then is wiped clean with dust-free paper, is cleaned with absolute ethyl alcohol for 3 times, and finally is dried for 1h at 50 ℃ to obtain the pretreated substrate.
Adding polyvinylidene fluoride-hexafluoropropylene copolymer, polyvinylidene fluoride and polymethyl methacrylate into the mixed solution a of polyethyl acrylate and chlorodiethyl ether, and mechanically stirring for 24 hours to obtain a mixed solution b; then vacuumizing the mixed solution b for 5 hours to obtain a mixed solution c; and uniformly coating the mixed solution c on one surface of the pretreated substrate, curing for 10 hours at 80 ℃, then putting the substrate into deionized water at 25 ℃, cooling, immediately peeling the film on the substrate, and obtaining the all-organic four-item blended energy storage composite material, wherein the mass fractions of polyvinylidene fluoride-hexafluoropropylene copolymer, polyvinylidene fluoride, polyethyl acrylate-chloroethyl ether and polymethyl methacrylate in the all-organic four-item blended energy storage composite material are 35%, 15% and 15% in sequence.
The CAS number of the polyvinylidene fluoride-hexafluoropropylene copolymer is 9011-17-0, and the property is particles;
the CAS number of the polyvinylidene fluoride is 24937-79-9, and the property is powder;
the CAS number of the polymethyl methacrylate is 9011-14-7, and the property is particles;
the polyvinylidene fluoride-hexafluoropropylene copolymer, polyvinylidene fluoride and polymethyl methacrylate were purchased from aladine Biochemical technologies Co., ltd.
The polyethyl acrylate-chloroethyl ether is acrylate rubber (ACM), and the product name isAR71, purchased from Japanese rayleigh Corporation (Zeon Corporation).
The chemical structural formula of the polyethyl acrylate-chloroethyl ether is as follows:
example 2: in this example, the mass fractions of the four materials of polyvinylidene fluoride-hexafluoropropylene copolymer, polyvinylidene fluoride, polyethyl acrylate-chloroethyl ether and polymethyl methacrylate are 30%, 20% and 20% in order. Other experimental conditions were the same as in example 1.
Example 3: in this example, the mass fractions of the four materials of polyvinylidene fluoride-hexafluoropropylene copolymer, polyvinylidene fluoride, polyethyl acrylate-chloroethyl ether and polymethyl methacrylate are 25%, 25% and 25% in order. Other experimental conditions were the same as in example 1.
Comparative example 1: in this example, step one of example 1 was not performed, and polymethyl methacrylate and polyvinylidene fluoride were not added in step two. Other experimental conditions were the same as in example 1.
Comparative example 2: in this example, step one of example 1 was not performed, and polymethyl methacrylate and polyvinylidene fluoride-hexafluoropropylene copolymer were not added in step two. Other experimental conditions were the same as in example 1.
FIG. 1 is an infrared spectrum of an all-organic four-term blended energy storage composite material based on polyvinylidene fluoride-hexafluoropropylene copolymer/polyvinylidene fluoride/polyethyl acrylate-chloroethyl ether/polymethyl methacrylate of the present invention; as shown in FIG. 1, the addition of the dielectric elastomer of the poly (ethyl acrylate) -chloroethyl ether rubber resulted in a composite at 1725cm -1 A peak appears at the wavelength, which represents the vibrational band of the carboalkyl group (c=o) of the methacrylic monomer in polyethyl acrylate-chloroethyl ether.
FIG. 2 is a graph of discharge energy density for an all-organic four-item blended energy storage composite of the present invention; as shown in fig. 2, as the mass fraction of the ethyl polyacrylate-chloroethyl ether increases, the discharge energy density increases and then decreases. The discharge energy density of the pure polyvinylidene fluoride-hexafluoropropylene copolymer film is 7.7J/cm 3 The discharge energy density of the pure polyvinylidene fluoride film is 12.9J/cm 3 When poly (ethyl acrylate) -chloroThe discharge energy density was 16.9J/cm when the mass fraction of diethyl ether/polymethyl methacrylate was 15%/15% 3 The discharge energy density is increased by 119% compared with the pure polyvinylidene fluoride-hexafluoropropylene copolymer film, and is increased by 31% compared with the pure polyvinylidene fluoride film.
FIG. 3 is a graph of charge and discharge efficiency of the all-organic four-item blended energy storage composite of the present invention; as shown in fig. 3, as the mass fraction of the poly (ethyl acrylate) -poly (vinyl chloride) rubber increases, the charge-discharge efficiency increases and then decreases, and in an electric field of 360MV/m, the charge-discharge efficiency of the pure poly (vinylidene fluoride) -poly (hexafluoropropylene copolymer) film is 45.7%, the charge-discharge efficiency of the pure poly (vinylidene fluoride) film is 52.4%, and when the mass fraction of the poly (ethyl acrylate) -poly (vinyl chloride) -poly (methyl methacrylate) is 15%/15%, the charge-discharge efficiency is 71%, which are 155% and 135% of the charge-discharge efficiency of the pure poly (vinylidene fluoride) -poly (hexafluoropropylene copolymer) film and the poly (vinylidene fluoride) film, respectively.
FIG. 4 is a graph of dielectric constant measurements for an all-organic four-item blended energy storage composite according to the present invention; as shown in fig. 4, the dielectric constant of the polyvinylidene fluoride and the poly (ethyl acrylate) -chloroethyl ether rubber composite material is continuously decreased as the mass fraction of the poly (ethyl acrylate) -chloroethyl ether rubber is increased.
FIG. 5 is a graph of dielectric loss measurements for an all-organic four-item blended energy storage composite of the present invention; as shown in FIG. 5, as the dielectric elastomer fraction of the poly (ethyl acrylate) -chloroethyl ether rubber increases, the dielectric loss of the poly (vinylidene fluoride) -poly (ethyl acrylate) -chloroethyl ether rubber composite material is slightly improved, but at 10 2 ~10 5 All below 0.1 at Hz.
FIG. 6 is a conductivity test chart of an all-organic four-item blended energy storage composite of the present invention; as shown in fig. 6, the dielectric loss of the polyvinylidene fluoride and the poly (ethyl acrylate) -chloroethyl ether rubber composite material is only slightly improved with the increase of the dielectric elastomer mass fraction of the poly (ethyl acrylate) -chloroethyl ether rubber.
Claims (10)
1. The preparation method of the all-organic four-item blending energy storage composite material is characterized by comprising the following steps of:
step one: preparing a mixed solution of polyethyl acrylate and chloroethyl ether;
adding the polyethyl acrylate-chloroethyl ether into the N, N-dimethylacetamide solution, and magnetically stirring until the polyethyl acrylate-chloroethyl ether is completely dissolved to obtain a polyethyl acrylate-chloroethyl ether mixed solution a;
step two: preparing a polyvinylidene fluoride-hexafluoropropylene copolymer/polyvinylidene fluoride/polyethyl acrylate-chloroethyl ether/polymethyl methacrylate four-item blending energy storage composite material;
adding polyvinylidene fluoride-hexafluoropropylene copolymer, polyvinylidene fluoride and polymethyl methacrylate into the mixed solution a of polyethyl acrylate and chlorodiethyl ether, and uniformly stirring to obtain a mixed solution b; then vacuumizing the mixed solution b to obtain a mixed solution c; uniformly coating the mixed solution c on one surface of the pretreated substrate, and stripping a film on the substrate after curing to obtain the all-organic four-item blended energy storage composite material, wherein the mass fraction ratio of polyvinylidene fluoride-hexafluoropropylene copolymer, polyvinylidene fluoride, polyethyl acrylate-chloroethyl ether and polymethyl methacrylate in the all-organic four-item blended energy storage composite material is (25-35): (25-35): (15-25): (15-25).
2. The method for preparing the all-organic four-item blended energy storage composite material according to claim 1, wherein in the step one, before the polyethyl acrylate-chloroethyl ether is added into the N, N-dimethylacetamide solution, the mixture is dried in vacuum for 6 to 7 hours at 50 to 60 ℃.
3. The method for preparing the all-organic four-item blended energy storage composite material according to claim 1, wherein the ratio of the mass of the polyethyl acrylate-chloroethyl ether to the volume of the N, N-dimethylacetamide solution in the step one is (0.15-0.25) g: (9-10) mL.
4. The method for preparing the all-organic four-item blended energy storage composite material according to claim 1, wherein in the first step, magnetic stirring is performed for 23-24 hours at the temperature of 45-55 ℃.
5. The preparation method of the all-organic four-item blended energy storage composite material is characterized in that in the second step, polyvinylidene fluoride-hexafluoropropylene copolymer, polyvinylidene fluoride and polymethyl methacrylate are added into a mixed solution a of polyethyl acrylate and chloroethyl ether, and the mixed solution b is obtained after mechanical stirring for 23-24 hours.
6. The preparation method of the all-organic four-item blending energy storage composite material is characterized in that in the second step, the mixed solution b is vacuumized for 4-5 hours to obtain a mixed solution c.
7. The method for preparing the all-organic four-item blended energy storage composite material according to claim 1, wherein the pretreated substrate in the second step is treated according to the following steps: the substrate is firstly cleaned by deionized water for 1 to 3 times, then cleaned by dust-free paper, then cleaned by absolute ethyl alcohol for 3 to 5 times, and finally dried for 1 to 2 hours at 50 to 60 ℃ to obtain the pretreated substrate, wherein the substrate is a high-temperature-resistant glass plate.
8. The method for preparing the all-organic four-item blended energy storage composite material according to claim 1, wherein in the second step, the mixed solution c is uniformly coated on one surface of the pretreated substrate, and is cured for 10-12 hours at 75-85 ℃.
9. The method for preparing the all-organic four-item blended energy storage composite material according to claim 1, wherein the mass fraction ratio of polyvinylidene fluoride-hexafluoropropylene copolymer, polyvinylidene fluoride, polyethyl acrylate-chloroethyl ether and polymethyl methacrylate in the all-organic four-item blended energy storage composite material in the step two is (35:35:15:15), (30:30:20:20) or (25:25:25:25).
10. The use of an all-organic four-term hybrid energy storage composite prepared by the method of any one of claims 1-9, wherein the all-organic four-term hybrid energy storage composite is used in a dielectric capacitor.
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