CN116082683A - Preparation method and application of fluorene polyester and polyethyl acrylate-chloroethyl ether based all-organic blending composite material - Google Patents
Preparation method and application of fluorene polyester and polyethyl acrylate-chloroethyl ether based all-organic blending composite material Download PDFInfo
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- NIHNNTQXNPWCJQ-UHFFFAOYSA-N fluorene Chemical compound C1=CC=C2CC3=CC=CC=C3C2=C1 NIHNNTQXNPWCJQ-UHFFFAOYSA-N 0.000 title claims abstract description 166
- 229920000728 polyester Polymers 0.000 title claims abstract description 71
- 239000002131 composite material Substances 0.000 title claims abstract description 52
- 238000002156 mixing Methods 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims abstract description 102
- 229920000120 polyethyl acrylate Polymers 0.000 claims abstract description 62
- 239000011521 glass Substances 0.000 claims abstract description 31
- 239000000758 substrate Substances 0.000 claims abstract description 31
- 239000000243 solution Substances 0.000 claims abstract description 26
- 239000011259 mixed solution Substances 0.000 claims abstract description 18
- 239000000843 powder Substances 0.000 claims abstract description 16
- 238000010438 heat treatment Methods 0.000 claims abstract description 10
- 238000003756 stirring Methods 0.000 claims abstract description 10
- 238000000034 method Methods 0.000 claims abstract description 8
- 239000011248 coating agent Substances 0.000 claims abstract description 5
- 238000000576 coating method Methods 0.000 claims abstract description 5
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 claims description 11
- 238000004321 preservation Methods 0.000 claims description 10
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- 239000003990 capacitor Substances 0.000 claims description 3
- 239000004745 nonwoven fabric Substances 0.000 claims description 3
- 239000010408 film Substances 0.000 claims 1
- 239000010409 thin film Substances 0.000 claims 1
- 230000015556 catabolic process Effects 0.000 abstract description 18
- 229920000642 polymer Polymers 0.000 abstract description 8
- 239000000178 monomer Substances 0.000 abstract description 3
- 238000009413 insulation Methods 0.000 abstract description 2
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 40
- 239000000203 mixture Substances 0.000 description 13
- 229920006267 polyester film Polymers 0.000 description 12
- 238000001816 cooling Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000002329 infrared spectrum Methods 0.000 description 2
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 2
- 229920002125 Sokalan® Polymers 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-M acrylate group Chemical group C(C=C)(=O)[O-] NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000003989 dielectric material Substances 0.000 description 1
- 238000005553 drilling Methods 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000004584 polyacrylic acid Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
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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
- H01G4/18—Organic dielectrics of synthetic material, e.g. derivatives of cellulose
-
- 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
-
- 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
- C08J2367/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
-
- 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
- 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
- C08J2433/08—Homopolymers or copolymers of acrylic acid esters
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- Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Power Engineering (AREA)
- Health & Medical Sciences (AREA)
- Materials Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
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Abstract
A preparation method and application of a fluorene polyester and polyethyl acrylate-chloroethyl ether based all-organic blending composite material relate to the technical field of fluorene polyester insulation. The invention aims to solve the problems that the traditional linear polymer monomer is low in dielectric constant, low in breakdown field strength or incapable of having both high dielectric constant and high breakdown field strength. The method comprises the following steps: adding fluorene polyester powder into a poly (ethyl acrylate) -chlorodiethyl ether solution a, mechanically stirring for 9-10 h, vacuumizing the mixed solution, uniformly coating the mixed solution on a pretreated glass substrate, heating to 75-80 ℃ and preserving heat for 11-12 h, heating to 115-120 ℃ and preserving heat for 9-10 h, and stripping the film on the glass substrate to obtain the fluorene polyester and poly (ethyl acrylate) -chlorodiethyl ether-based all-organic blending composite material. The invention can obtain a preparation method and application of a fluorene polyester and polyethyl acrylate-chlorodiethyl ether all-organic blending composite material.
Description
Technical Field
The invention relates to the technical field of fluorene polyester insulation, in particular to a preparation method and application of a fluorene polyester and polyethyl acrylate-chloroethyl ether based all-organic blending high-breakdown-strength composite material.
Background
The polymer medium has the advantages of easy processing, low dielectric loss, quick charge and discharge and the like, is widely applied to the aspects of energy storage, conversion, utilization and the like, and particularly has wide application in the fields of automobiles in the field of hybrid power, oil drilling and aerospace. However, with the development of miniaturization of power electronics, polymer dielectrics are facing increasingly harsh operating environments. Among them, the biggest challenge is to achieve high breakdown strength compatible with low dielectric losses. At present, the traditional linear polymer monomer generally faces the problems of low dielectric constant and low breakdown field strength, and fluorene polyester has the characteristics of high breakdown strength and low dielectric loss as a linear dielectric polymer, so that the fluorene polyester has wide prospects.
Disclosure of Invention
The invention aims to solve the problems that the traditional linear polymer monomer is low in dielectric constant and breakdown field strength or cannot have both high dielectric constant and high breakdown field strength, and provides a preparation method and application of a fluorene polyester and polyethyl acrylate-chloroethyl ether based all-organic blending composite material.
The preparation method of the fluorene polyester and polyethyl acrylate-chloroethyl ether based all-organic blending composite material comprises the following steps:
step one: preparing a polyethyl acrylate-chlorodiethyl ether solution;
adding the polyethyl acrylate-chloroethyl ether into N, N-dimethyl acetamide solution, magnetically stirring for 23-24 h at the temperature of 45-50 ℃ to obtain a polyethyl acrylate-chloroethyl ether solution a, wherein the ratio of the mass of the polyethyl acrylate-chloroethyl ether to the volume of the N, N-dimethyl acetamide solution is (0.02-0.1) g:7mL;
step two: preparing a fluorene polyester and polyethyl acrylate-chloroethyl ether based all-organic blending composite material;
adding fluorene polyester powder into a poly (ethyl acrylate) -chlorodiethyl ether solution a, and mechanically stirring for 9-10 h to obtain a mixed solution c, wherein the mass ratio of the fluorene polyester powder to the poly (ethyl acrylate) -chlorodiethyl ether in the mixed solution c is (0.7-0.78): (0.02-0.1); and (3) vacuumizing the mixed solution c, uniformly coating the mixed solution on one surface of the pretreated glass substrate, then placing the glass substrate in a high-temperature blast drying oven, heating to 75-80 ℃, preserving heat for 11-12 h at the temperature of 75-80 ℃, heating to 115-120 ℃ after the heat preservation is finished, continuing to preserve heat for 9-10 h at the temperature of 115-120 ℃, and stripping a film on the glass substrate after the heat preservation is finished to obtain the fluorene polyester and polyethyl acrylate-chlorodiethyl ether based all-organic blending composite material, wherein the mass fraction of the polyethyl acrylate-chlorodiethyl ether in the fluorene polyester and polyethyl acrylate-chlorodiethyl ether based all-organic blending composite material is 2.5-12.5%.
The application of the fluorene polyester and polyethyl acrylate-chloroethyl ether based all-organic blending composite material in the dielectric capacitor.
The invention has the beneficial effects that:
(1) According to the preparation method of the fluorene polyester and polyethyl acrylate-chloroethyl ether based all-organic blending composite material, firstly, the polyethyl acrylate-chloroethyl ether is added into N, N-dimethylacetamide solution, and the polyethyl acrylate-chloroethyl ether is difficult to dissolve, so that the stirring is required to be fully carried out at the temperature of 45-50 ℃. And then preparing a blend film by using a solution blending method, adding fluorene polyester powder into the mixed solution of the poly (ethyl acrylate) and the chlorodiethyl ether, and mechanically stirring for 9-10 hours.
In the past, a polymer composite material is formed by introducing a nano material with charge blocking transportation into a polymer matrix, and the preparation process is generally complex, and defects are easy to be introduced to reduce the breakdown field intensity. The poly (ethyl acrylate) -chloroethyl ether adopted by the invention has good dispersibility in fluorene polyester, the dielectric constant of the fluorene polyester and poly (ethyl acrylate) -chloroethyl ether-based all-organic blend composite film is higher than that of a pure fluorene polyester composite film, the breakdown performance is greatly improved, and the problem that the composite material cannot have both high dielectric constant and high breakdown field strength is solved.
(2) The fluorene polyester and polyethyl acrylate-chlorodiethyl ether all-organic blending composite material prepared by the process has excellent dielectric property and breakdown property, reduces loss, and can be widely applied to the advanced fields of electric, electronic, new energy automobiles and the like. The preparation method is simple in process, economical, practical, effective in resource saving, suitable for large-scale industrial production and capable of providing a good strategy for developing new all-organic insulating materials.
The invention can obtain a preparation method and application of a fluorene polyester and polyethyl acrylate-chlorodiethyl ether all-organic blending composite material.
Drawings
FIG. 1 is an infrared spectrum of a fluorene polyester and poly (ethyl acrylate) -chloroethyl ether-based all-organic blend composite material with different mass fractions, wherein a represents the mass fraction of poly (ethyl acrylate) -chloroethyl ether as 2.5%, b represents the mass fraction of poly (ethyl acrylate) -chloroethyl ether as 5%, c represents the mass fraction of poly (ethyl acrylate) -chloroethyl ether as 7.5%, d represents the mass fraction of poly (ethyl acrylate) -chloroethyl ether as 10%, e represents the mass fraction of poly (ethyl acrylate) -chloroethyl ether as 12.5%, and f represents a pure fluorene polyester film;
fig. 2 is a distribution diagram of the breakdown field strength weibull plot of the fluorene polyester and poly (ethyl acrylate) -chlorodiethyl ether all-organic blend composite material with different mass fractions, ■ for a pure fluorene polyester film, for a poly (ethyl acrylate) -chlorodiethyl ether mass fraction of 2.5%, for a poly (ethyl acrylate) -chlorodiethyl ether mass fraction of 5%,
representing 7.5% of the mass fraction of the ethyl polyacrylate-chloroethyl ether, representing 10% of the mass fraction of the ethyl polyacrylate-chloroethyl ether, and representing 12.5% of the mass fraction of the ethyl polyacrylate-chloroethyl ether;
FIG. 3 is a graph showing the dielectric constant test of fluorene polyesters of different mass fractions of poly (ethyl acrylate) -chloroethyl ether and poly (ethyl acrylate) -chloroethyl ether-based all-organic blend composite material, ■ represents a pure fluorene polyester film, while one represents the mass fraction of poly (ethyl acrylate) -chloroethyl ether as 2.5%, while the other represents the mass fraction of poly (ethyl acrylate) -chloroethyl ether as 5%,
representing 7.5% of the mass fraction of the ethyl polyacrylate-chloroethyl ether, representing 10% of the mass fraction of the ethyl polyacrylate-chloroethyl ether, and representing 12.5% of the mass fraction of the ethyl polyacrylate-chloroethyl ether;
fig. 4 is a graph showing dielectric loss test of fluorene polyester and poly (ethyl acrylate) -chloroethyl ether based all-organic blend composite material with different mass fractions, ■ shows a pure fluorene polyester film, while the one shows that the mass fraction of poly (ethyl acrylate) -chloroethyl ether is 2.5%, the one shows that the mass fraction of poly (ethyl acrylate) -chloroethyl ether is 5%,
representing 7.5% of the mass fraction of the ethyl polyacrylate-chloroethyl ether, representing 10% of the mass fraction of the ethyl polyacrylate-chloroethyl ether, and representing 12.5% of the mass fraction of the ethyl polyacrylate-chloroethyl ether;
fig. 5 is a conductivity test chart of fluorene polyester and poly (ethyl acrylate) -chloroethyl ether based all-organic blend composite material with different mass fractions, ■ representing pure fluorene polyester film, with the mass fraction of poly (ethyl acrylate) -chloroethyl ether being 2.5%, with the mass fraction of poly (ethyl acrylate) -chloroethyl ether being 5%,
the mass fraction of the ethyl polyacrylate-chloroethyl ether is 7.5%, the mass fraction of the ethyl polyacrylate-chloroethyl ether is 10%, and the mass fraction of the ethyl polyacrylate-chloroethyl ether is 12.5%.
Detailed Description
The first embodiment is as follows: the preparation method of the fluorene polyester and polyethyl acrylate-chlorodiethyl ether based all-organic blending composite material comprises the following steps:
step one: preparing a polyethyl acrylate-chlorodiethyl ether solution;
adding the polyethyl acrylate-chloroethyl ether into N, N-dimethyl acetamide solution, magnetically stirring for 23-24 h at the temperature of 45-50 ℃ to obtain a polyethyl acrylate-chloroethyl ether solution a, wherein the ratio of the mass of the polyethyl acrylate-chloroethyl ether to the volume of the N, N-dimethyl acetamide solution is (0.02-0.1) g:7mL;
step two: preparing a fluorene polyester and polyethyl acrylate-chloroethyl ether based all-organic blending composite material;
adding fluorene polyester powder into a poly (ethyl acrylate) -chlorodiethyl ether solution a, and mechanically stirring for 9-10 h to obtain a mixed solution c, wherein the mass ratio of the fluorene polyester powder to the poly (ethyl acrylate) -chlorodiethyl ether in the mixed solution c is (0.7-0.78): (0.02-0.1); and (3) vacuumizing the mixed solution c, uniformly coating the mixed solution on one surface of the pretreated glass substrate, then placing the glass substrate in a high-temperature blast drying oven, heating to 75-80 ℃, preserving heat for 11-12 h at the temperature of 75-80 ℃, heating to 115-120 ℃ after the heat preservation is finished, continuing to preserve heat for 9-10 h at the temperature of 115-120 ℃, and stripping a film on the glass substrate after the heat preservation is finished to obtain the fluorene polyester and polyethyl acrylate-chlorodiethyl ether based all-organic blending composite material, wherein the mass fraction of the polyethyl acrylate-chlorodiethyl ether in the fluorene polyester and polyethyl acrylate-chlorodiethyl ether based all-organic blending composite material is 2.5-12.5%.
The second embodiment is as follows: the present embodiment differs from the specific embodiment in that: in the first step, the polyethyl acrylate-chloroethyl ether is dried for 3 to 4 hours in a vacuum environment at the temperature of 40 to 50 ℃ before being used.
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: the pretreated glass substrate in the second step is treated according to the following steps: the glass substrate is firstly cleaned by deionized water for 1 to 3 times, is cleaned by non-woven fabrics, is then washed by absolute ethyl alcohol for 1 to 2 times, and is dried for 30 to 40 minutes at 50 to 60 ℃ to obtain the pretreated glass substrate.
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: and step two, after the heat preservation is finished, the glass substrate is placed in deionized water for cooling.
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: after the glass substrate was placed in deionized water, the film was peeled off immediately.
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: the ratio of the mass of the poly ethyl acrylate-chloroethyl ether, the mass of the fluorene polyester powder to the volume of the N, N-dimethylacetamide solution was (0.02 g:0.78g:7 ml), (0.04 g:0.76g:7 ml), (0.06 g:0.74g:7 ml), (0.08 g:0.72g:7 ml) or (0.1 g:0.7g:7 ml).
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 mass fraction of the poly (ethyl acrylate) -chlorodiethyl ether in the fluorene polyester and poly (ethyl acrylate) -chlorodiethyl ether-based all-organic blending composite material is 2.5%, 5%, 7.5%, 10% or 12.5%.
Other steps are the same as those of embodiments one to six.
Eighth embodiment: the embodiment relates to application of a fluorene polyester and polyethyl acrylate-chlorodiethyl ether based all-organic blending 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 fluorene polyester and polyethyl acrylate-chloroethyl ether based all-organic blending composite material comprises the following steps:
step one: preparing a polyethyl acrylate-chlorodiethyl ether solution;
the polyethyl acrylate-chloroethyl ether is firstly dried for 4 hours under the vacuum environment of 50 ℃, then 0.02g of polyethyl acrylate-chloroethyl ether is added into 7mL of N, N-dimethylacetamide solution, and the mixture is magnetically stirred for 24 hours under the temperature of 50 ℃ to obtain the polyethyl acrylate-chloroethyl ether solution a.
The polyethyl acrylate-chloroethyl ether is acrylate rubber (ACM), and the product name is
AR71, purchased from Japanese rayleigh Corporation (Zeon Corporation).
The chemical structural formula of the polyethyl acrylate-chloroethyl ether is as follows:
step two: preparing a fluorene polyester and polyethyl acrylate-chloroethyl ether based all-organic blending composite material;
firstly preparing a piece of high-temperature resistant glass with the size of 200mm multiplied by 16mm multiplied by 4mm as a substrate, cleaning the glass substrate with deionized water for 3 times, wiping the glass substrate with non-woven fabrics, then washing the glass substrate with absolute ethyl alcohol for 2 times, and drying the glass substrate at 60 ℃ for 30min to obtain the pretreated glass substrate.
Adding 0.78g of fluorene polyester powder into the ethyl polyacrylate-chlorodiethyl ether solution a, and mechanically stirring for 9-10 h to obtain a mixed solution c; and (3) vacuumizing the mixed solution c, uniformly coating the mixed solution on one surface of the pretreated glass substrate, then placing the glass substrate in a high-temperature blast drying oven, heating to 80 ℃, preserving heat at the temperature of 80 ℃ for 12 hours, heating to 120 ℃ after the heat preservation is finished, continuously preserving heat at the temperature of 120 ℃ for 10 hours, cooling the glass substrate in deionized water after the heat preservation is finished, immediately stripping the film from the glass substrate to obtain the fluorene polyester and polyethyl acrylate-chlorodiethyl ether based all-organic blending composite material, wherein the mass fraction of polyethyl acrylate-chlorodiethyl ether in the fluorene polyester and polyethyl acrylate-chlorodiethyl ether based all-organic blending composite material is 2.5%.
Example 2: in this embodiment, the amount of the ethyl polyacrylate-chloroethyl ether is 0.04g, the amount of the fluorene polyester powder is 0.76g, and the mass fraction of the ethyl polyacrylate-chloroethyl ether is 5%. Other experimental conditions were the same as in example 1.
Example 3: in this embodiment, the amount of the ethyl polyacrylate-chloroethyl ether is 0.06g, the amount of the fluorene polyester powder is 0.74g, and the mass fraction of the ethyl polyacrylate-chloroethyl ether is 7.5%. Other experimental conditions were the same as in example 1.
Example 4: in this embodiment, the amount of the ethyl polyacrylate-chloroethyl ether is 0.08g, the amount of the fluorene polyester powder is 0.72g, and the mass fraction of the ethyl polyacrylate-chloroethyl ether is 10%. Other experimental conditions were the same as in example 1.
Example 5: in this embodiment, the amount of the ethyl polyacrylate-chloroethyl ether is 0.1g, the amount of the fluorene polyester powder is 0.7g, and the mass fraction of the ethyl polyacrylate-chloroethyl ether is 12.5%. Other experimental conditions were the same as in example 1.
Example 6: in this example, step one was not performed, and in step two, the ethyl polyacrylate-chloroethyl ether solution a was not added, and the fluorene polyester powder was reacted only with the N, N-dimethylacetamide solution. Other experimental conditions were the same as in example 1.
FIG. 1 is an infrared spectrum of a fluorene polyester and poly (ethyl acrylate) -chloroethyl ether-based all-organic blend composite material with different mass fractions, wherein a represents the mass fraction of poly (ethyl acrylate) -chloroethyl ether to be 2.5%, b represents the mass fraction of poly (ethyl acrylate) -chloroethyl ether to be 5%, c represents the mass fraction of poly (ethyl acrylate) -chloroethyl ether to be 7.5%, d represents the mass fraction of poly (ethyl acrylate) -chloroethyl ether to be 10%, e represents the mass fraction of poly (ethyl acrylate) -chloroethyl ether to be 12.5%, and f represents a pure fluorene polyester film. As shown in FIG. 1, at a wavelength of 3060cm -1 The C-H vibration peak on benzene ring is shown in the specification, and along with the polyacrylic acid BThe peak value is gradually reduced when the ester-chloroethyl ether is added, which proves that the addition of the polyethyl acrylate-chloroethyl ether effectively inhibits the C-H vibration on the benzene ring.
Fig. 2 is a distribution diagram of the breakdown field strength weibull plot of the fluorene polyester and poly (ethyl acrylate) -chlorodiethyl ether all-organic blend composite material with different mass fractions, ■ for a pure fluorene polyester film, for a poly (ethyl acrylate) -chlorodiethyl ether mass fraction of 2.5%, for a poly (ethyl acrylate) -chlorodiethyl ether mass fraction of 5%,
the mass fraction of the ethyl polyacrylate-chloroethyl ether is 7.5%, the mass fraction of the ethyl polyacrylate-chloroethyl ether is 10%, and the mass fraction of the ethyl polyacrylate-chloroethyl ether is 12.5%. As shown in fig. 2, as the mass fraction of the poly ethyl acrylate-chloroethyl ether increases, the breakdown field strength increases and then decreases. The breakdown field intensity of the pure fluorene polyester film is 489kV/mm, when the mass fraction of the poly (ethyl acrylate) -chlorodiethyl ether is 2.5%, the highest value of the breakdown field intensity is 536kV/mm, and compared with the pure fluorene polyester film, the breakdown field intensity is improved by 9.6%. The addition of a small amount of polyethyl acrylate-chloroethyl ether can inhibit the movement of carriers in the material, and greatly improve the breakdown field intensity.
FIG. 3 is a graph showing the dielectric constant test of fluorene polyesters of different mass fractions of poly (ethyl acrylate) -chloroethyl ether and poly (ethyl acrylate) -chloroethyl ether-based all-organic blend composite material, ■ represents a pure fluorene polyester film, while one represents the mass fraction of poly (ethyl acrylate) -chloroethyl ether as 2.5%, while the other represents the mass fraction of poly (ethyl acrylate) -chloroethyl ether as 5%,
the mass fraction of the ethyl polyacrylate-chloroethyl ether is 7.5%, the mass fraction of the ethyl polyacrylate-chloroethyl ether is 10%, and the mass fraction of the ethyl polyacrylate-chloroethyl ether is 12.5%. As shown in fig. 3, the dielectric constant was uniformly increased as the mass fraction of the ethyl polyacrylate-chlorodiethyl ether was increased.
Fig. 4 is a graph showing dielectric loss test of fluorene polyester and poly (ethyl acrylate) -chloroethyl ether based all-organic blend composite material with different mass fractions, ■ shows a pure fluorene polyester film, while the one shows that the mass fraction of poly (ethyl acrylate) -chloroethyl ether is 2.5%, the one shows that the mass fraction of poly (ethyl acrylate) -chloroethyl ether is 5%,
the mass fraction of the ethyl polyacrylate-chloroethyl ether is 7.5%, the mass fraction of the ethyl polyacrylate-chloroethyl ether is 10%, and the mass fraction of the ethyl polyacrylate-chloroethyl ether is 12.5%. As shown in fig. 4, the dielectric loss slightly increased with the mass fraction of the ethyl polyacrylate-chloroethyl ether. It is notable that the change in dielectric loss is very small when the mass fraction of the poly ethyl acrylate-chloroethyl ether is 2.5%.
Fig. 5 is a conductivity test chart of fluorene polyester and poly (ethyl acrylate) -chloroethyl ether based all-organic blend composite material with different mass fractions, ■ representing pure fluorene polyester film, with the mass fraction of poly (ethyl acrylate) -chloroethyl ether being 2.5%, with the mass fraction of poly (ethyl acrylate) -chloroethyl ether being 5%,
the mass fraction of the ethyl polyacrylate-chloroethyl ether is 7.5%, the mass fraction of the ethyl polyacrylate-chloroethyl ether is 10%, and the mass fraction of the ethyl polyacrylate-chloroethyl ether is 12.5%. As shown in fig. 5, the conductivity increased only slightly with increasing mass fraction of poly ethyl acrylate-chloroethyl ether. />
Claims (8)
1. The preparation method of the fluorene polyester and polyethyl acrylate-chloroethyl ether all-organic blending composite material is characterized by comprising the following steps of:
step one: preparing a polyethyl acrylate-chlorodiethyl ether solution;
adding the polyethyl acrylate-chloroethyl ether into N, N-dimethyl acetamide solution, magnetically stirring for 23-24 h at the temperature of 45-50 ℃ to obtain a polyethyl acrylate-chloroethyl ether solution a, wherein the ratio of the mass of the polyethyl acrylate-chloroethyl ether to the volume of the N, N-dimethyl acetamide solution is (0.02-0.1) g:7mL;
step two: preparing a fluorene polyester and polyethyl acrylate-chloroethyl ether based all-organic blending composite material;
adding fluorene polyester powder into a poly (ethyl acrylate) -chlorodiethyl ether solution a, and mechanically stirring for 9-10 h to obtain a mixed solution c, wherein the mass ratio of the fluorene polyester powder to the poly (ethyl acrylate) -chlorodiethyl ether in the mixed solution c is (0.7-0.78): (0.02-0.1); and (3) vacuumizing the mixed solution c, uniformly coating the mixed solution on one surface of the pretreated glass substrate, then placing the glass substrate in a high-temperature blast drying oven, heating to 75-80 ℃, preserving heat for 11-12 h at the temperature of 75-80 ℃, heating to 115-120 ℃ after the heat preservation is finished, continuing to preserve heat for 9-10 h at the temperature of 115-120 ℃, and stripping a film on the glass substrate after the heat preservation is finished to obtain the fluorene polyester and polyethyl acrylate-chlorodiethyl ether based all-organic blending composite material, wherein the mass fraction of the polyethyl acrylate-chlorodiethyl ether in the fluorene polyester and polyethyl acrylate-chlorodiethyl ether based all-organic blending composite material is 2.5-12.5%.
2. The preparation method of the fluorene polyester and poly (ethyl acrylate) -chlorodiethyl ether based all-organic blending composite material according to claim 1, wherein the poly (ethyl acrylate) -chlorodiethyl ether is dried for 3-4 hours in a vacuum environment at 40-50 ℃ before being used in the step one.
3. The method for preparing the fluorene polyester and polyethyl acrylate-chlorodiethyl ether all-organic blending composite material according to claim 1, wherein the glass substrate pretreated in the second step is treated according to the following steps: the glass substrate is firstly cleaned by deionized water for 1 to 3 times, is cleaned by non-woven fabrics, is then washed by absolute ethyl alcohol for 1 to 2 times, and is dried for 30 to 40 minutes at 50 to 60 ℃ to obtain the pretreated glass substrate.
4. The method for preparing the fluorene polyester and polyethyl acrylate-chlorodiethyl ether all-organic blending composite material according to claim 1, wherein the glass substrate is cooled in deionized water after the heat preservation in the second step is finished.
5. The method for preparing a fluorene polyester and poly (ethyl acrylate) -chlorodiethyl ether based all-organic blended composite material according to claim 4, wherein the thin film is peeled off immediately after the glass substrate is placed in deionized water.
6. The preparation method of the fluorene polyester and poly (ethyl acrylate) -chloroethyl ether all-organic blending composite material according to claim 1, wherein the ratio of the mass of poly (ethyl acrylate) -chloroethyl ether, the mass of fluorene polyester powder and the volume of the N, N-dimethylacetamide solution is (0.02 g:0.78g:7 mL), (0.04 g:0.76g:7 mL) (0.06 g:0.74g:7 mL), (0.08 g:0.72g:7 mL) or (0.1 g:0.7g:7 mL).
7. The preparation method of the fluorene polyester and poly (ethyl acrylate) -chlorodiethyl ether-based all-organic blending composite material according to claim 1 or 6, wherein the mass fraction of poly (ethyl acrylate) -chlorodiethyl ether in the fluorene polyester and poly (ethyl acrylate) -chlorodiethyl ether-based all-organic blending composite material is 2.5%, 5%, 7.5%, 10% or 12.5%.
8. The use of a fluorene polyester and poly (ethyl acrylate) -chlorodiethyl ether based all-organic blended composite material prepared by the method as claimed in any one of claims 1-7, characterized in that the use of the fluorene polyester and poly (ethyl acrylate) -chlorodiethyl ether based all-organic blended composite material in dielectric capacitors.
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