CN116903995A - Preparation method and application of epoxy resin all-organic blending heat-resistant composite material - Google Patents
Preparation method and application of epoxy resin all-organic blending heat-resistant composite material Download PDFInfo
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- CN116903995A CN116903995A CN202310918865.5A CN202310918865A CN116903995A CN 116903995 A CN116903995 A CN 116903995A CN 202310918865 A CN202310918865 A CN 202310918865A CN 116903995 A CN116903995 A CN 116903995A
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- 239000003822 epoxy resin Substances 0.000 title claims abstract description 98
- 229920000647 polyepoxide Polymers 0.000 title claims abstract description 98
- 239000002131 composite material Substances 0.000 title claims abstract description 55
- 238000002156 mixing Methods 0.000 title claims abstract description 50
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims abstract description 80
- 238000010438 heat treatment Methods 0.000 claims abstract description 27
- 239000000243 solution Substances 0.000 claims abstract description 27
- 239000000203 mixture Substances 0.000 claims abstract description 23
- 238000000034 method Methods 0.000 claims abstract description 14
- 239000011259 mixed solution Substances 0.000 claims abstract description 13
- 238000003756 stirring Methods 0.000 claims abstract description 12
- VYKXQOYUCMREIS-UHFFFAOYSA-N methylhexahydrophthalic anhydride Chemical compound C1CCCC2C(=O)OC(=O)C21C VYKXQOYUCMREIS-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000001816 cooling Methods 0.000 claims abstract description 7
- 229920000120 polyethyl acrylate Polymers 0.000 claims description 37
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 22
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 claims description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- AHDSRXYHVZECER-UHFFFAOYSA-N 2,4,6-tris[(dimethylamino)methyl]phenol Chemical compound CN(C)CC1=CC(CN(C)C)=C(O)C(CN(C)C)=C1 AHDSRXYHVZECER-UHFFFAOYSA-N 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 3
- 229910052782 aluminium Inorganic materials 0.000 claims description 3
- 239000003990 capacitor Substances 0.000 claims description 3
- 239000003795 chemical substances by application Substances 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 239000011888 foil Substances 0.000 claims description 3
- 239000004745 nonwoven fabric Substances 0.000 claims description 3
- 229920006267 polyester film Polymers 0.000 claims description 3
- LNEPOXFFQSENCJ-UHFFFAOYSA-N haloperidol Chemical compound C1CC(O)(C=2C=CC(Cl)=CC=2)CCN1CCCC(=O)C1=CC=C(F)C=C1 LNEPOXFFQSENCJ-UHFFFAOYSA-N 0.000 abstract description 7
- 239000000463 material Substances 0.000 abstract description 7
- 239000000654 additive Substances 0.000 description 4
- 230000000996 additive effect Effects 0.000 description 4
- 238000001878 scanning electron micrograph Methods 0.000 description 4
- 238000000354 decomposition reaction Methods 0.000 description 3
- 239000004698 Polyethylene Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 239000000945 filler Substances 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 239000011368 organic material Substances 0.000 description 2
- -1 polyethylene Polymers 0.000 description 2
- 229920000573 polyethylene Polymers 0.000 description 2
- 238000002411 thermogravimetry Methods 0.000 description 2
- 229920002595 Dielectric elastomer Polymers 0.000 description 1
- 239000004593 Epoxy Substances 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-M acrylate group Chemical group C(C=C)(=O)[O-] NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 229920001971 elastomer Polymers 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L63/00—Compositions of epoxy resins; Compositions of derivatives of epoxy resins
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/20—Applications use in electrical or conductive gadgets
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Organic Insulating Materials (AREA)
Abstract
A preparation method and application of an epoxy resin all-organic blending heat-resistant composite material relate to the technical field of epoxy resins. The invention aims to solve the problem that the traditional epoxy resin material cannot have good thermal performance and electrical performance. The method comprises the following steps: adding epoxy resin and methyl hexahydrophthalic anhydride into a polyethyl acrylate-chlorodiethyl ether solution, and uniformly mixing to obtain a mixed solution; stirring the mixed solution at 70-80 ℃ for 4-6 hours, and vacuumizing at 70-80 ℃ for 1-2 hours; and (3) uniformly pouring the mixture on a die after vacuumizing, placing the die in a flat vulcanizing machine for gradient heating, cooling to room temperature after heating, and finally demolding to obtain the epoxy resin all-organic blending heat-resistant composite material. The invention can obtain a preparation method and application of an epoxy resin all-organic blending heat-resistant composite material.
Description
Technical Field
The invention relates to the technical field of epoxy resin, in particular to a preparation method and application of an epoxy resin all-organic blending heat-resistant composite material.
Background
Epoxy resins are one of the materials widely used in electric and electronic systems because of their excellent insulation, stable performance, good adhesion, and low cost. However, with the development of power systems and electronics, epoxy resins are facing increasingly harsh operating environments. Among the biggest challenges are the need to improve both the thermal and electrical properties of epoxy resins. The poly (ethyl acrylate) -chloroethyl ether has excellent electric and thermal properties as a dielectric elastomer, but no compatibility attempt with epoxy resin in the field has been reported.
Therefore, the current situation of low thermal and electrical properties faced by conventional epoxy resins requires improvement and breakthrough by technicians.
Disclosure of Invention
The invention aims to solve the problem that the traditional epoxy resin material cannot have good thermal performance and electrical performance, and provides a preparation method and application of an epoxy resin all-organic blending heat-resistant composite material.
The preparation method of the epoxy resin all-organic blending heat-resistant composite material comprises the following steps:
step one, preparing a polyethyl acrylate-chlorodiethyl ether solution:
adding the polyethyl acrylate-chloroethyl ether into an acetone solution, heating to 40-50 ℃, and stirring for 6-8 hours until the polyethyl acrylate-chloroethyl ether is completely dissolved to obtain a polyethyl acrylate-chloroethyl ether solution;
preparing the epoxy resin all-organic blending heat-resistant composite material:
adding epoxy resin and methyl hexahydrophthalic anhydride into the ethyl polyacrylate-chlorodiethyl ether solution obtained in the step one, and uniformly mixing to obtain a mixed solution; stirring the mixed solution at 70-80 ℃ for 4-6 hours, and vacuumizing at 70-80 ℃ for 1-2 hours; uniformly pouring the mixture on a die after vacuumizing, placing the die in a flat vulcanizing machine for gradient heating, cooling to room temperature after heating, and finally demolding to obtain the epoxy resin all-organic blending heat-resistant composite material; the mass of the polyethyl acrylate-chloroethyl ether in the epoxy resin all-organic blending heat-resistant composite material is 1-8% of the mass of the epoxy resin.
An application of an epoxy resin all-organic blending heat-resistant composite material in a dielectric capacitor.
The invention has the beneficial effects that:
(1) The invention relates to a preparation method of an epoxy resin all-organic blending heat-resistant composite material, which comprises the steps of adding polyethyl acrylate-chlorodiethyl ether into an acetone solution, fully stirring the mixture at 50 ℃ because the polyethyl acrylate-chlorodiethyl ether is difficult to dissolve, and preparing a blending film by using a solution blending method. The introduction of fillers with higher heat resistance in the polymeric matrix of epoxy resins generally has an impact on other properties, and is often complicated to prepare, which can easily introduce other defects that lead to reduced properties. The polyethylene acrylate-chloroethyl ether adopted by the invention has good dispersibility in epoxy resin, and the thermal performance and the electrical performance of the epoxy resin blended polyethylene acrylate-chloroethyl ether insulating film are superior to those of a pure epoxy resin material, so that the problem that the thermal performance and the electrical performance of the epoxy resin material are not excellent enough is solved.
(2) The epoxy resin all-organic blending heat-resistant composite material prepared by the method has good electrical property and thermal property, low cost and no obvious degradation of other properties, 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 and effective in saving resources, is suitable for large-scale industrial production, and provides a good strategy for developing new all-organic materials.
The invention can obtain a preparation method and application of an epoxy resin all-organic blending heat-resistant composite material.
Drawings
FIG. 1 is a cross-sectional SEM image of an epoxy resin of example 5 without added polyethyl acrylate-chloroethyl ether;
FIG. 2 is a cross-sectional SEM image of an epoxy resin all-organic blend heat resistant composite with 4% ethyl polyacrylate-chlorodiethyl ether added in example 3;
fig. 3 is a graph showing the dielectric constant test of epoxy resin all-organic blend heat-resistant composite materials with different additive amounts of poly (ethyl acrylate) -chloroethyl ether, ■ shows a pure epoxy resin film, +.,the mass fraction of the poly (ethyl acrylate) -chlorodiethyl ether is 4%, and the mass fraction of the poly (ethyl acrylate) -chlorodiethyl ether is 8%;
fig. 4 is a graph showing dielectric loss test of epoxy resin all-organic blend heat-resistant composite materials with different additive amounts of poly (ethyl acrylate) -chloroethyl ether, ■ shows a pure epoxy resin film, +.,the mass fraction of the poly (ethyl acrylate) -chlorodiethyl ether is 4%, and the mass fraction of the poly (ethyl acrylate) -chlorodiethyl ether is 8%;
fig. 5 is a graph of conductivity tests of epoxy resin all-organic blend heat-resistant composites with different amounts of ethyl polyacrylate-chloroethyl ether, ■ for pure epoxy resin film, +.,the mass fraction of the poly (ethyl acrylate) -chlorodiethyl ether is 4%, and the mass fraction of the poly (ethyl acrylate) -chlorodiethyl ether is 8%;
FIG. 6 is a graph showing the thermogravimetry of epoxy resin all-organic blending heat-resistant composite materials with different addition amounts of poly (ethyl acrylate) -chlorodiethyl ether, wherein a represents that the addition amount of poly (ethyl acrylate) -chlorodiethyl ether is 0%, b represents that the addition amount of poly (ethyl acrylate) -chlorodiethyl ether is 1%, c represents that the addition amount of poly (ethyl acrylate) -chlorodiethyl ether is 2%, d represents that the addition amount of poly (ethyl acrylate) -chlorodiethyl ether is 4%, and e represents that the addition amount of poly (ethyl acrylate) -chlorodiethyl ether is 8%;
fig. 7 is a graph of thermal conductivity measurements of epoxy resin all-organic blend heat resistant composites with varying amounts of ethyl polyacrylate-chloroethyl ether.
Detailed Description
The first embodiment is as follows: the preparation method of the epoxy resin all-organic blending heat-resistant composite material comprises the following steps:
step one, preparing a polyethyl acrylate-chlorodiethyl ether solution:
adding the polyethyl acrylate-chloroethyl ether into an acetone solution, heating to 40-50 ℃, and stirring for 6-8 hours until the polyethyl acrylate-chloroethyl ether is completely dissolved to obtain a polyethyl acrylate-chloroethyl ether solution;
preparing the epoxy resin all-organic blending heat-resistant composite material:
adding epoxy resin and methyl hexahydrophthalic anhydride into the ethyl polyacrylate-chlorodiethyl ether solution obtained in the step one, and uniformly mixing to obtain a mixed solution; stirring the mixed solution at 70-80 ℃ for 4-6 hours, and vacuumizing at 70-80 ℃ for 1-2 hours; uniformly pouring the mixture on a die after vacuumizing, placing the die in a flat vulcanizing machine for gradient heating, cooling to room temperature after heating, and finally demolding to obtain the epoxy resin all-organic blending heat-resistant composite material; the mass of the polyethyl acrylate-chloroethyl ether in the epoxy resin all-organic blending heat-resistant composite material is 1-8% of the mass of the epoxy resin.
The beneficial effect of this embodiment is:
(1) According to the preparation method of the epoxy resin all-organic blending heat-resistant composite material, firstly, the polyethyl acrylate-chloroethyl ether is added into an acetone solution, and because the polyethyl acrylate-chloroethyl ether is difficult to dissolve, the polyethyl acrylate-chloroethyl ether needs to be fully stirred at the temperature of 50 ℃, and then a blending film is prepared by using a solution blending method. The introduction of fillers with higher heat resistance in the polymeric matrix of epoxy resins generally has an impact on other properties, and is often complicated to prepare, which can easily introduce other defects that lead to reduced properties. The thermal performance and the electrical performance of the epoxy resin blended poly (ethyl acrylate) -chloroethyl ether insulating film are superior to those of pure epoxy resin materials, and the problem that the thermal performance and the electrical performance of the epoxy resin materials are not excellent is solved.
(2) The epoxy resin all-organic blending heat-resistant composite material prepared by the method has good electrical property and thermal property, low cost and no obvious degradation of other properties, and can be widely applied to advanced fields such as electric, electronic and new energy automobiles. The preparation method of the embodiment is simple in process, economical, practical, effective in saving of resources, suitable for large-scale industrial production and capable of providing a good strategy for developing new all-organic materials.
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 added into an acetone solution.
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 acetone solution is (0.25-2) g: (35-40) 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 step II, the mass ratio of the epoxy resin to the methyl hexahydrophthalic anhydride to the polyethyl acrylate-chlorodiethyl ether in the polyethyl acrylate-chlorodiethyl ether solution is 25:21.25: (0.25-2).
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: the die in the second step is subjected to the following pretreatment before use: the mold is firstly cleaned by deionized water for 1 to 3 times, then is cleaned by non-woven fabrics, is then washed by absolute ethyl alcohol for 1 to 2 times, is finally dried for 20 to 30 minutes at 50 to 60 ℃, and is sprayed with a release agent after the drying is finished.
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, adding an accelerator DMP-30 before pouring the mixed solution on a die, and stirring for 1-2 min, wherein the adding amount is 0.5-1% of the mass of the epoxy resin, and the epoxy resin is epoxy resin E51.
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: gradient heating as described in step two: firstly, heating the die to 95-105 ℃, and preserving heat for 1.5-2 hours at 95-105 ℃; then heating to 150-160 ℃, and continuously preserving heat for 1.5-2 h at 150-160 ℃; then heating to 170-180 ℃ and keeping the temperature at 170-180 ℃ for 1.5-2 h.
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: step two, when the mould is placed in a flat vulcanizing machine for gradient heating, the mould is coated by using an aluminum foil and a polyester film; and (5) after heating, placing the mixture in a flat vulcanizing machine, and cooling the mixture to room temperature by water.
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: the mass of the polyethyl acrylate-chloroethyl ether in the epoxy resin all-organic blending heat-resistant composite material in the second step is 1%, 2%, 4% or 8% of the mass of the epoxy resin.
Other steps are the same as those of embodiments one to eight.
Detailed description ten: the embodiment relates to an application of an epoxy resin all-organic blending heat-resistant 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 epoxy resin all-organic blending heat-resistant composite material comprises the following steps:
step one, preparing a polyethyl acrylate-chlorodiethyl ether solution:
firstly, drying the polyethyl acrylate-chloroethyl ether for 3 hours in a vacuum environment at 50 ℃ to remove redundant water; then adding 0.25g of dried poly (ethyl acrylate) -chlorodiethyl ether into 40mL of acetone solution, heating to 50 ℃ firstly, and magnetically stirring until the poly (ethyl acrylate) -chlorodiethyl ether is completely dissolved to obtain a poly (ethyl acrylate) -chlorodiethyl ether solution;
the polyethyl acrylate-chloroethyl ether is acrylate rubber (ACM), and the product name isAR71, purchased from Japanese rayleigh Corporation (Zeon Corporation).
Firstly, preparing a mould with the thickness of about 200 micrometers, cleaning the mould with deionized water for 3 times, wiping the mould with non-woven fabrics, washing the mould with absolute ethyl alcohol for 2 times, and finally drying the mould for 30 minutes at 50 ℃ to obtain a clean mould, and spraying a release agent for use.
Preparing the epoxy resin all-organic blending heat-resistant composite material:
adding 25g of epoxy resin E51 and 21.25g of methyl hexahydrophthalic anhydride into the ethyl polyacrylate-chlorodiethyl ether solution obtained in the step one, and uniformly mixing to obtain a mixed solution; stirring the mixed solution at 80 ℃ for 4 hours, vacuumizing at 80 ℃ for 2 hours, adding 0.25g of DMP-30, stirring for 2 minutes, uniformly pouring on a die, placing the die in a vulcanizing press, and coating the die with an aluminum foil and a polyester film to prevent liquid from overflowing; firstly, heating the die to 100 ℃, and preserving heat for 2 hours at 100 ℃; then heating to 160 ℃, and keeping the temperature at 160 ℃ for 2 hours; heating to 180 ℃ and keeping the temperature at 180 ℃ for 2 hours; and after the heat preservation is finished, placing the mixture in a flat vulcanizing machine, cooling the mixture to room temperature by water, and finally demolding the mixture to obtain the epoxy resin all-organic blending heat-resistant composite material.
Example 2: the amount of ethyl polyacrylate-chloroethyl ether added in this example was 2%. Other experimental conditions were the same as in example 1.
Example 3: the amount of ethyl polyacrylate-chloroethyl ether added in this example was 4%. Other experimental conditions were the same as in example 1.
Example 4: the amount of ethyl polyacrylate-chloroethyl ether added in this example was 8%. Other experimental conditions were the same as in example 1.
Example 5: in this example, the first step of example 1 was not performed, and the mixed solution of the epoxy resin E51 and methyl hexahydrophthalic anhydride was prepared directly without adding the polyethyl acrylate-chloroethyl ether in the second step. Other experimental conditions were the same as in example 1.
FIG. 1 is a cross-sectional SEM image of an epoxy resin of example 5 without added polyethyl acrylate-chloroethyl ether; as shown in fig. 1, exhibited a typical brittle fracture morphology.
FIG. 2 is a cross-sectional SEM image of an epoxy resin all-organic blend heat resistant composite with 4% ethyl polyacrylate-chlorodiethyl ether added in example 3; as shown in fig. 2, a significant bend and fold can be seen, indicating that poly (ethyl acrylate) -chloroethyl ether has been added to epoxy E51.
Fig. 3 is a graph showing the dielectric constant test of epoxy resin all-organic blend heat-resistant composite materials with different additive amounts of poly (ethyl acrylate) -chloroethyl ether, ■ shows a pure epoxy resin film, +.,the mass fraction of the ethyl polyacrylate-chloroethyl ether is 4%, and the mass fraction of the ethyl polyacrylate-chloroethyl ether is 8%. As shown in FIG. 3, the dielectric constant is improved with the increase of the poly (ethyl acrylate) -chloroethyl ether, and the dielectric constant is stable at different frequencies and slightly reduced at high frequencies.
Fig. 4 is a graph showing dielectric loss test of epoxy resin all-organic blend heat-resistant composite materials with different additive amounts of poly (ethyl acrylate) -chloroethyl ether, ■ shows a pure epoxy resin film, +.,the mass fraction of the ethyl polyacrylate-chloroethyl ether is 4%, and the mass fraction of the ethyl polyacrylate-chloroethyl ether is 8%. As shown in fig. 4, the dielectric loss did not change significantly with increasing mass fraction of poly ethyl acrylate-chloroethyl ether, so the sample loss was at a lower level. It is noted that when the addition amount of the ethyl polyacrylate-chloroethyl ether is 1%, the dielectric loss is reduced.
Fig. 5 is a graph of conductivity tests of epoxy resin all-organic blend heat-resistant composites with different amounts of ethyl polyacrylate-chloroethyl ether, ■ for pure epoxy resin film, +.,the mass fraction of the ethyl polyacrylate-chloroethyl ether is 4%, and the mass fraction of the ethyl polyacrylate-chloroethyl ether is 8%. As shown in fig. 5, the conductivity did not change significantly with increasing mass fraction of poly ethyl acrylate-chloroethyl ether, so the conductivity of the samples was at a lower level. It is noted that when the addition amount of the ethyl polyacrylate-chloroethyl ether was 1%, the electrical conductivity slightly decreased.
FIG. 6 is a graph showing the thermogravimetry of epoxy resin all-organic blending heat-resistant composite materials with different addition amounts of poly (ethyl acrylate) -chlorodiethyl ether, wherein a represents that the addition amount of poly (ethyl acrylate) -chlorodiethyl ether is 0%, b represents that the addition amount of poly (ethyl acrylate) -chlorodiethyl ether is 1%, c represents that the addition amount of poly (ethyl acrylate) -chlorodiethyl ether is 2%, d represents that the addition amount of poly (ethyl acrylate) -chlorodiethyl ether is 4%, and e represents that the addition amount of poly (ethyl acrylate) -chlorodiethyl ether is 8%. As shown in fig. 6, the sample was decomposed slightly in advance due to the residual acetone solvent. With the increase of the content of the poly (ethyl acrylate) -chloroethyl ether, the thermal stability of the sample is improved, and the 5% decomposition temperature, the 10% decomposition temperature and the 30% decomposition temperature of the sample are improved to different degrees, which indicates that the addition of the poly (ethyl acrylate) -chloroethyl ether improves the thermal stability of the composite material.
FIG. 7 is a graph of thermal conductivity measurements for various mass fractions of poly (ethyl acrylate) -chloroethyl ether epoxy resin all-organic blend heat resistant composites. As shown in FIG. 7, with the increase of the mass fraction of the poly (ethyl acrylate) -chlorodiethyl ether, the heat conductivity coefficient is improved to a certain extent, and when the addition amount of the poly (ethyl acrylate) -chlorodiethyl ether is 8%, the heat conductivity of the composite material is improved by 41.6%.
Claims (10)
1. The preparation method of the epoxy resin all-organic blending heat-resistant 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 an acetone solution, heating to 40-50 ℃, and stirring for 6-8 hours until the polyethyl acrylate-chloroethyl ether is completely dissolved to obtain a polyethyl acrylate-chloroethyl ether solution;
preparing the epoxy resin all-organic blending heat-resistant composite material:
adding epoxy resin and methyl hexahydrophthalic anhydride into the ethyl polyacrylate-chlorodiethyl ether solution obtained in the step one, and uniformly mixing to obtain a mixed solution; stirring the mixed solution at 70-80 ℃ for 4-6 hours, and vacuumizing at 70-80 ℃ for 1-2 hours; uniformly pouring the mixture on a die after vacuumizing, placing the die in a flat vulcanizing machine for gradient heating, cooling to room temperature after heating, and finally demolding to obtain the epoxy resin all-organic blending heat-resistant composite material; the mass of the polyethyl acrylate-chloroethyl ether in the epoxy resin all-organic blending heat-resistant composite material is 1-8% of the mass of the epoxy resin.
2. The method for preparing the epoxy resin all-organic blending heat-resistant composite material according to claim 1, wherein in the step one, the polyethyl acrylate-chloroethyl ether is dried for 3-4 hours in a vacuum environment at 40-50 ℃ before being added into an acetone solution.
3. The method for preparing the epoxy resin all-organic blending heat-resistant composite material according to claim 1 or 2, wherein the ratio of the mass of the polyethyl acrylate-chloroethyl ether to the volume of the acetone solution in the step one is (0.25-2) g: (35-40) mL.
4. The preparation method of the epoxy resin all-organic blending heat-resistant composite material is characterized in that in the step II, the mass ratio of epoxy resin, methyl hexahydrophthalic anhydride and poly (ethyl acrylate) -chlorodiethyl ether in a poly (ethyl acrylate) -chlorodiethyl ether solution is 25:21.25: (0.25-2).
5. The method for preparing the epoxy resin all-organic blending heat-resistant composite material according to claim 1, wherein the die in the second step is subjected to the following pretreatment before use: the mold is firstly cleaned by deionized water for 1 to 3 times, then is cleaned by non-woven fabrics, is then washed by absolute ethyl alcohol for 1 to 2 times, is finally dried for 20 to 30 minutes at 50 to 60 ℃, and is sprayed with a release agent after the drying is finished.
6. The method for preparing the epoxy resin all-organic blending heat-resistant composite material according to claim 1 or 4, wherein the accelerator DMP-30 is added before the mixed solution is poured onto a die in the second step, and the mixture is stirred for 1-2 min, wherein the addition amount of the accelerator DMP-30 is 0.5-1% of the mass of the epoxy resin, and the epoxy resin is epoxy resin E51.
7. The method for preparing the epoxy resin all-organic blending heat-resistant composite material according to claim 1, wherein the gradient heating in the second step is as follows: firstly, heating the die to 95-105 ℃, and preserving heat for 1.5-2 hours at 95-105 ℃; then heating to 150-160 ℃, and continuously preserving heat for 1.5-2 h at 150-160 ℃; then heating to 170-180 ℃ and keeping the temperature at 170-180 ℃ for 1.5-2 h.
8. The method for preparing the epoxy resin all-organic blending heat-resistant composite material, which is characterized in that in the second step, when the mold is placed in a flat vulcanizing machine for gradient heating, the mold is coated by aluminum foil and polyester film; and (5) after heating, placing the mixture in a flat vulcanizing machine, and cooling the mixture to room temperature by water.
9. The method for preparing the epoxy resin all-organic blending heat-resistant composite material according to claim 1, wherein the mass of the poly (ethyl acrylate) -chloroethyl ether in the epoxy resin all-organic blending heat-resistant composite material in the second step is 1%, 2%, 4% or 8% of the mass of the epoxy resin.
10. The use of an epoxy resin all-organic blended heat resistant composite material as claimed in any one of claims 1 to 9, characterized in that the epoxy resin all-organic blended heat resistant composite material is used in dielectric capacitors.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310918865.5A CN116903995B (en) | 2023-07-25 | 2023-07-25 | Preparation method and application of epoxy resin all-organic blending heat-resistant composite material |
Applications Claiming Priority (1)
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