CN113388228A - Resin composition, resin-based composite material, and preparation method and application thereof - Google Patents
Resin composition, resin-based composite material, and preparation method and application thereof Download PDFInfo
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- CN113388228A CN113388228A CN202110721015.7A CN202110721015A CN113388228A CN 113388228 A CN113388228 A CN 113388228A CN 202110721015 A CN202110721015 A CN 202110721015A CN 113388228 A CN113388228 A CN 113388228A
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- 239000000463 material Substances 0.000 title claims abstract description 105
- 239000000805 composite resin Substances 0.000 title claims abstract description 95
- 239000011342 resin composition Substances 0.000 title claims abstract description 66
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 239000011347 resin Substances 0.000 claims abstract description 94
- 229920005989 resin Polymers 0.000 claims abstract description 94
- 239000000945 filler Substances 0.000 claims abstract description 40
- 239000002904 solvent Substances 0.000 claims abstract description 22
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 7
- 239000004744 fabric Substances 0.000 claims description 131
- 239000000835 fiber Substances 0.000 claims description 31
- 239000002245 particle Substances 0.000 claims description 24
- 239000003795 chemical substances by application Substances 0.000 claims description 21
- 238000000034 method Methods 0.000 claims description 7
- 239000007822 coupling agent Substances 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 239000011256 inorganic filler Substances 0.000 claims description 3
- 229910003475 inorganic filler Inorganic materials 0.000 claims description 3
- 238000009210 therapy by ultrasound Methods 0.000 claims description 3
- 238000009940 knitting Methods 0.000 claims 1
- 238000005452 bending Methods 0.000 abstract description 14
- 150000001875 compounds Chemical class 0.000 abstract 1
- 239000003365 glass fiber Substances 0.000 description 100
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 33
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 18
- 230000000052 comparative effect Effects 0.000 description 16
- 238000009941 weaving Methods 0.000 description 16
- 239000011248 coating agent Substances 0.000 description 14
- 238000000576 coating method Methods 0.000 description 14
- 238000001816 cooling Methods 0.000 description 14
- 238000003825 pressing Methods 0.000 description 14
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 12
- 230000009477 glass transition Effects 0.000 description 12
- QGBSISYHAICWAH-UHFFFAOYSA-N dicyandiamide Chemical compound NC(N)=NC#N QGBSISYHAICWAH-UHFFFAOYSA-N 0.000 description 11
- 239000000377 silicon dioxide Substances 0.000 description 9
- ARXJGSRGQADJSQ-UHFFFAOYSA-N 1-methoxypropan-2-ol Chemical compound COCC(C)O ARXJGSRGQADJSQ-UHFFFAOYSA-N 0.000 description 8
- YSWBFLWKAIRHEI-UHFFFAOYSA-N 4,5-dimethyl-1h-imidazole Chemical compound CC=1N=CNC=1C YSWBFLWKAIRHEI-UHFFFAOYSA-N 0.000 description 8
- 239000003822 epoxy resin Substances 0.000 description 7
- 229920000647 polyepoxide Polymers 0.000 description 7
- VXAUWWUXCIMFIM-UHFFFAOYSA-M aluminum;oxygen(2-);hydroxide Chemical compound [OH-].[O-2].[Al+3] VXAUWWUXCIMFIM-UHFFFAOYSA-M 0.000 description 6
- 239000002131 composite material Substances 0.000 description 6
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 4
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 4
- 238000004891 communication Methods 0.000 description 4
- 239000000454 talc Substances 0.000 description 4
- 229910052623 talc Inorganic materials 0.000 description 4
- HZEOUPCNUWSUFL-UHFFFAOYSA-N 4,5,5-trimethyl-4-pentan-3-yl-1H-imidazole Chemical compound C(C)C(C1(N=CNC1(C)C)C)CC HZEOUPCNUWSUFL-UHFFFAOYSA-N 0.000 description 3
- CPHGOBGXZQKCKI-UHFFFAOYSA-N 4,5-diphenyl-1h-imidazole Chemical compound N1C=NC(C=2C=CC=CC=2)=C1C1=CC=CC=C1 CPHGOBGXZQKCKI-UHFFFAOYSA-N 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- LLHKCFNBLRBOGN-UHFFFAOYSA-N propylene glycol methyl ether acetate Chemical compound COCC(C)OC(C)=O LLHKCFNBLRBOGN-UHFFFAOYSA-N 0.000 description 3
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 description 2
- 229910000019 calcium carbonate Inorganic materials 0.000 description 2
- 238000010030 laminating Methods 0.000 description 2
- VYKXQOYUCMREIS-UHFFFAOYSA-N methylhexahydrophthalic anhydride Chemical compound C1CCCC2C(=O)OC(=O)C21C VYKXQOYUCMREIS-UHFFFAOYSA-N 0.000 description 2
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 150000001412 amines Chemical class 0.000 description 1
- 150000008064 anhydrides Chemical class 0.000 description 1
- 239000004841 bisphenol A epoxy resin Substances 0.000 description 1
- 238000005470 impregnation Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000012778 molding material Substances 0.000 description 1
- 229920003986 novolac Polymers 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000012779 reinforcing material Substances 0.000 description 1
- -1 undecanoimidazole Chemical compound 0.000 description 1
Classifications
-
- 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
- C08J5/24—Impregnating materials with prepolymers which can be polymerised in situ, e.g. manufacture of prepregs
-
- 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
- C08J5/04—Reinforcing macromolecular compounds with loose or coherent fibrous material
- C08J5/0405—Reinforcing macromolecular compounds with loose or coherent fibrous material with inorganic fibres
- C08J5/043—Reinforcing macromolecular compounds with loose or coherent fibrous material with inorganic fibres with glass fibres
-
- 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
- C08J2363/00—Characterised by the use of epoxy resins; Derivatives of epoxy resins
-
- 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
- C08J2463/00—Characterised by the use of epoxy resins; Derivatives of epoxy resins
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
- C08K2003/265—Calcium, strontium or barium carbonate
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
- C08K7/14—Glass
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Reinforced Plastic Materials (AREA)
Abstract
The invention relates to a resin composition, a resin-based composite material, a preparation method and application thereof, wherein the resin composition comprises a first resin, a second resin, a filler, an auxiliary agent and a solvent, and the first resin comprises a compound shown in a structural formula (1)Resin A or at least one of resin B with a structural formula shown in formula (2),
in the formula (1), R1Is CaH2aAnd has no branched chain, a is more than or equal to 5 and less than or equal to 30, n is more than or equal to 1 and less than or equal to 10, m is more than or equal to 10 and less than or equal to 100 in the formula (2), t is more than or equal to 0 and less than or equal to 50, the structural formula of the second resin is shown as the formula (3),
Description
Technical Field
The invention relates to the technical field of resin-based composite materials, in particular to a resin composition, a resin-based composite material, and a preparation method and application thereof.
Background
Although the traditional glass fiber reinforced epoxy resin composite material has good mechanical strength such as stretching and bending, the toughness of the traditional glass fiber reinforced epoxy resin composite material is insufficient in the application process due to the fact that an epoxy resin system is brittle after being cured, and particularly obvious creases appear after the traditional glass fiber reinforced epoxy resin composite material is bent by 90 degrees, so that the use requirements of fields such as computers, communication and consumer electronic products (3C electronic products) which have high requirements on the toughness of resin matrix composite materials cannot be met.
Disclosure of Invention
In view of the above, it is necessary to provide a resin composition, a resin-based composite material, a preparation method and an application thereof, wherein the resin-based composite material is resistant to 90 ° bending without damage, has excellent toughness, and can meet the use requirements of the field with higher requirements on the toughness of the resin-based composite material.
A resin composition comprising a first resin, a second resin, a filler, an auxiliary agent, and a solvent, the first resin comprising at least one of resin A or resin B, wherein,
the structural formula of the resin A is shown as a formula (1),
in the formula (1), R1Is CaH2aAnd has no branched chain, a is more than or equal to 5 and less than or equal to 30, and n is more than or equal to 1 and less than or equal to 10;
the structural formula of the resin B is shown as a formula (2),
in the formula (2), m is more than or equal to 10 and less than or equal to 100, and t is more than or equal to 0 and less than or equal to 50;
the structural formula of the second resin is shown as a formula (3),
in the formula (3), x is more than or equal to 0.1 and less than or equal to 10.
In one embodiment, the filler is an inorganic filler, and the particle size of the filler is 2 μm to 20 μm.
In one embodiment, in the resin composition, the first resin is 5 to 40 parts by weight, the second resin is 60 to 95 parts by weight, the filler is 20 to 100 parts by weight, the auxiliary is 0.01 to 52 parts by weight, and the solvent is 10 to 100 parts by weight.
In one embodiment, the filler has a mass 2 to 5 times the mass of the first resin.
In one embodiment, the auxiliary agent comprises at least one of a curing agent and an accelerator.
A method of making a resin-based composite material, comprising:
providing a fiber cloth;
forming the resin composition on the fiber cloth and drying to obtain a prepreg;
overlapping at least two prepregs to form a prepreg layer, covering release films on two sides of the prepreg layer, and curing to obtain a prefabricated product;
and removing the release film in the prefabricated product to obtain the resin-based composite material, wherein the mass fraction of the fiber cloth in the resin-based composite material is 20-65%.
In one embodiment, the fiber cloth is formed by warp and weft yarns through horizontal and vertical weaving, and the single yarn diameter of the warp and weft yarns is 1.5-4 μm.
In one embodiment, the fiber cloth has an elongation at break of 3.5% to 7%;
and/or the mass of the fiber cloth is 20g/m2-110g/m2The thickness is 0.01mm-0.1 mm.
In one embodiment, the fiber cloth is further subjected to a coupling agent treatment and/or an ultrasonic treatment before the resin composition as described above is formed on the fiber cloth and dried.
A resin-based composite material obtained by the preparation method of the resin-based composite material.
Use of a resin-based composite material as described above in an electronic product.
In the resin composition, the first resin, the second resin and the filler are compounded, so that the resin-based composite material prepared from the resin composition is resistant to 90-degree bending without damage, has excellent toughness, and simultaneously has excellent mechanical property, high glass transition temperature and low thermal expansion coefficient. Furthermore, the resin-based composite material can meet the use requirements of fields with higher toughness requirements, such as computer products, communication products, consumer electronics products and the like.
Detailed Description
The resin composition, resin-based composite material, and preparation method and application thereof provided by the present invention will be further described below.
In order to improve the toughness of a resin-based composite material and enable the resin-based composite material to achieve the effect of resisting 90-degree bending without damage, the resin composition provided by the invention comprises a first resin, a second resin, a filler, an auxiliary agent and a solvent, wherein the first resin comprises at least one of a resin A or a resin B,
the structural formula of the resin A is shown as a formula (1),
in the formula (1), R1Is CaH2aAnd has no branched chain, a is more than or equal to 5 and less than or equal to 30, and n is more than or equal to 1 and less than or equal to 10;
the structural formula of the resin B is shown as a formula (2),
in the formula (2), m is more than or equal to 10 and less than or equal to 100, and t is more than or equal to 0 and less than or equal to 50;
the structural formula of the second resin is shown as a formula (3),
in the formula (3), x is more than or equal to 0.1 and less than or equal to 10.
In the resin composition of the present invention, the use of the first resin can improve the toughness of the material after curing of the resin composition, but also lowers the glass transition temperature of the material and increases the thermal expansion coefficient. For this reason, in the resin composition of the present invention, a second resin is further used in combination with the first resin to increase the glass transition temperature of the material and to lower the thermal expansion coefficient of the material.
In order to make the material have better toughness and higher glass transition temperature and lower thermal expansion coefficient, in formula (1), a is more than or equal to 5 and less than or equal to 15, n is more than or equal to 1 and less than or equal to 5, in formula (2), m is more than or equal to 10 and less than or equal to 60, t is more than or equal to 0 and less than or equal to 20, and in formula (3), x is more than or equal to 0.3 and less than or equal to 5.
In order to further reduce the thermal expansion coefficient of the material and improve the dimensional stability of the material, in one embodiment, the filler is preferably an inorganic filler comprising at least one of silica, aluminum dioxide, talc, aluminum hydroxide and calcium carbonate, and the particle size of the filler is preferably 2 μm to 20 μm.
Similarly, while improving the toughness of the material, in order to simultaneously achieve the mechanical property, the thermal expansion coefficient and the glass transition temperature of the material, in the resin composition, the mass of the first resin is 5 to 40 parts by weight, the mass of the second resin is 60 to 95 parts by weight, the mass of the filler is 20 to 100 parts by weight, the mass of the auxiliary agent is 0.01 to 22 parts by weight, and the mass of the solvent is 10 to 100 parts by weight. In one embodiment, the filler has a mass 2 to 5 times the mass of the first resin.
The solvent is preferably an organic solvent, and includes at least one of propylene glycol methyl ether (PM), propylene glycol methyl ether acetate (PMA), Methyl Ethyl Ketone (MEK), and Dimethylformamide (DMF).
Therefore, in the resin composition, the first resin, the second resin and the filler are compounded, so that the resin-based composite material prepared from the resin composition is resistant to 90-degree bending without damage, has excellent toughness, and simultaneously has excellent mechanical properties, high glass transition temperature and low thermal expansion coefficient.
In the resin composition of the present invention, the auxiliary includes at least one of a curing agent and an accelerator. Wherein the mass of the curing agent is 1-20 parts by weight, and the mass of the accelerator is 0.01-2 parts by weight.
In one embodiment, the curing agent includes at least one of a latent amine curing agent, a phenolic curing agent, and an anhydride curing agent, and the accelerator includes at least one of dimethylimidazole, undecanoimidazole, diphenylimidazole, or diethyltetramethylimidazole.
In combination with the above resin composition, the present invention also provides a method for preparing a resin-based composite material, comprising:
s1, providing fiber cloth;
s2, forming the resin composition on the fiber cloth and drying to obtain a prepreg;
s3, overlapping at least two prepregs to form a prepreg layer, covering release films on two sides of the prepreg layer, and curing to obtain a prefabricated product;
s4, removing the release film in the prefabricated product to obtain the resin-based composite material, wherein the mass fraction of the fiber cloth in the resin-based composite material is 20-65%.
In the preparation method of the resin-based composite material, the resin composition is adopted, and the mass fraction of the glass fiber cloth in the resin-based composite material is limited, so that the relationship between the toughness and the mechanical property, the thermal expansion coefficient and the glass transition temperature of the resin-based composite material can be better balanced.
In order to balance the toughness of the resin-based composite material with the properties such as the thermal expansion coefficient, in one embodiment, the mass fraction of the fiber cloth in the resin-based composite material is more preferably 30% to 55%.
In order to further improve the 90-degree bending resistance of the resin-based composite materialAnd step S1, the fiber cloth is formed by weaving warp and weft yarns in a transverse and longitudinal mode, wherein the diameter of a single yarn of the warp and weft yarns is 1.5-4 mu m, and the mass of the fiber cloth is 20g/m2-110g/m2Preferably 45g/m2-110g/m2And the thickness is 0.01mm-0.1mm, preferably 0.035mm-0.1 mm.
Further, the breaking elongation of the fiber cloth is preferably 3.5% -7%.
In one embodiment, the fiber cloth is preferably an electronic grade fiber cloth, and more preferably a glass fiber cloth.
In step S2, in order to better bond the resin composition to the fiber cloth, in one embodiment, the fiber cloth is further subjected to a coupling agent treatment and/or an ultrasonic treatment before the resin composition is formed on the fiber cloth and dried.
The resin composition is formed on the fiber cloth by coating, impregnation or the like, and the mass fraction of the fiber cloth in the resin-based composite material is controlled by controlling the mass of the resin composition formed on the fiber cloth.
In one embodiment, the thickness of the prepreg is less than or equal to 0.2 mm.
In step S3, the curing temperature is preferably 120-160 ℃, and the pressure is preferably 20kg/cm2-35kg/cm2The time is preferably 10min to 30 min.
In step S4, the structure of the obtained resin-based composite material is preferably a layered structure, and the thickness is adjusted and controlled by stacking different numbers of prepregs according to the requirements of the application field.
The invention also provides a resin-based composite material by combining the preparation method of the resin-based composite material.
The resin-based composite material disclosed by the invention is small in density, low in cost, easy to form, free of electromagnetic shielding, resistant to 90-degree bending without damage, excellent in toughness, excellent in mechanical property, high in glass transition temperature and low in thermal expansion coefficient. Furthermore, the resin-based composite material can meet the use requirements of fields with higher toughness requirements, such as computer products, communication products, consumer electronics products and the like.
Therefore, the invention also provides the application of the resin-based composite material in electronic products, and further the resin-based composite material is used as a shell reinforcing material of computer, communication and consumer electronic products.
Hereinafter, the resin composition, the resin-based composite material, the preparation method and the application thereof will be further described by the following specific examples.
Example 1
The resin composition of this example included 5 parts by weight of resin a, 95 parts by weight of the second resin, 20 parts by weight of silica filler (particle size of 20 μm), 8 parts by weight of dicyandiamide curing agent, 0.09 parts by weight of dimethylimidazole accelerator, and 30 parts by weight of DMF solvent. Wherein, a is 15, n is 5 in the resin A; and x in the second resin is 5.
And (3) uniformly coating the resin composition on electronic-grade glass fiber cloth, baking the glass fiber cloth at 160 ℃ for 3min, and cooling the glass fiber cloth to room temperature to obtain a prepreg. The electronic-grade glass fiber cloth is formed by weaving warp and weft yarns in a transverse and longitudinal mode, wherein the diameters of single yarns of the warp and weft yarns are 3.5 mu m, and the mass of the glass fiber cloth is 80g/m2The thickness was 0.06mm, and the elongation at break was 4%.
And (3) superposing 7 prepregs to form a prepreg layer, covering release films on two surfaces of the prepreg layer, and putting the prepreg layer into a superposed press for pressing and curing to obtain a prefabricated product. Wherein the curing temperature is 150 deg.C, and the curing pressure is 30kg/cm2The curing time was 20 minutes. And finally, removing the release films on the two sides of the prefabricated product to obtain the resin-based composite material. In the resin-based composite material, the mass fraction of the glass fiber cloth in the resin-based composite material is 55%.
Example 2
The resin composition of this example comprises 40 parts by weight of resin A, 60 parts by weight of the second resin, 20 parts by weight of a talc filler (particle size 15 μm), 80 parts by weight of an aluminum dioxide filler (particle size 2 μm), 2 parts by weight of a dicyandiamide curing agent, 0.6 parts by weight of an undecanimidazole accelerator, and 100 parts by weight of DMF solvent. Wherein, a is 5, n is 10 in the resin A; and x in the second resin is 10.
And (3) uniformly coating the resin composition on electronic-grade glass fiber cloth, baking the glass fiber cloth at 160 ℃ for 3min, and cooling the glass fiber cloth to room temperature to obtain a prepreg. The electronic-grade glass fiber cloth is formed by weaving warp and weft yarns in a transverse and longitudinal mode, wherein the diameters of single yarns of the warp and weft yarns are 4 mu m, and the mass of the glass fiber cloth is 110g/m2The thickness was 0.1mm and the elongation at break was 4%.
And (3) laminating the prepregs to form a prepreg layer, covering release films on two surfaces of the prepreg layer, and putting the prepreg layer into a laminating press for pressing and curing to obtain the prefabricated product. Wherein the curing temperature is 150 deg.C, and the curing pressure is 30kg/cm2The curing time was 20 minutes. And finally, removing the release films on the two sides of the prefabricated product to obtain the resin-based composite material. In the resin-based composite material, the mass fraction of the glass fiber cloth in the resin-based composite material is 20%.
Example 3
The resin composition of this example included 20 parts by weight of resin a, 80 parts by weight of the second resin, 20 parts by weight of a calcium carbonate filler (particle size of 12 μm), 60 parts by weight of a silica filler (particle size of 10 μm)4 parts by weight of a dicyandiamide curing agent, 0.8 parts by weight of a diphenylimidazole accelerator, and 60 parts by weight of an MEK solvent. Wherein, a is 15, n is 1 in the resin A; x in the second resin is 0.1.
And (3) uniformly coating the resin composition on electronic-grade glass fiber cloth, baking the glass fiber cloth at 160 ℃ for 3min, and cooling the glass fiber cloth to room temperature to obtain a prepreg. The electronic-grade glass fiber cloth is formed by weaving warp and weft yarns in a transverse and longitudinal mode, wherein the diameters of single yarns of the warp and weft yarns are 3.5 mu m, and the mass of the glass fiber cloth is 60g/m2The thickness was 0.055mm and the elongation at break was 4%.
And (3) superposing 8 prepregs to form a prepreg layer, covering release films on two surfaces of the prepreg layer, and putting the prepreg layer into a superposed press for pressing and curing to obtain a prefabricated product. Wherein the curing temperature is 150 deg.C, and the curing pressure is 30%kg/cm2The curing time was 20 minutes. And finally, removing the release films on the two sides of the prefabricated product to obtain the resin-based composite material. In the resin-based composite material, the mass fraction of the glass fiber cloth in the resin-based composite material is 45%.
Example 4
The resin composition of this example comprised 5 parts by weight of resin B, 95 parts by weight of the second resin, 25 parts by weight of an aluminum hydroxide filler (particle size 15 μm), 5 parts by weight of a dicyandiamide curing agent, 0.5 parts by weight of a diethyltetramethylimidazole accelerator, and 40 parts by weight of DMF solvent. Wherein m is 100 and t is 0 in the resin B; and x in the second resin is 5.
And (3) uniformly coating the resin composition on electronic-grade glass fiber cloth, baking the glass fiber cloth at 160 ℃ for 3min, and cooling the glass fiber cloth to room temperature to obtain a prepreg. The electronic-grade glass fiber cloth is formed by weaving warp and weft yarns in a transverse and longitudinal mode, wherein the diameters of single yarns of the warp and weft yarns are 1.5 mu m, and the mass of the glass fiber cloth is 20g/m2The thickness was 0.01mm, and the elongation at break was 4%.
And (3) superposing 20 prepregs to form a prepreg layer, covering release films on two surfaces of the prepreg layer, and putting the prepreg layer into a superposed press for pressing and curing to obtain a prefabricated product. Wherein the curing temperature is 150 deg.C, and the curing pressure is 30kg/cm2The curing time was 20 minutes. And finally, removing the release films on the two sides of the prefabricated product to obtain the resin-based composite material. In the resin-based composite material, the mass fraction of the glass fiber cloth in the resin-based composite material is 65%.
Example 5
The resin composition of this example included 40 parts by weight of resin B, 60 parts by weight of the second resin, 15 parts by weight of a talc filler (particle size 15 μm), 75 parts by weight of an aluminum dioxide filler (particle size 5 μm), 2 parts by weight of a dicyandiamide curing agent, 0.5 parts by weight of a diphenylimidazole accelerator, and 80 parts by weight of an MEK solvent. Wherein m is 100 and t is 50 in the resin B; and x in the second resin is 10.
The resin composition is evenly coated on electronic-grade glass fiber cloth and is baked for 3min at 160 ℃,and cooling to room temperature to obtain the prepreg. The electronic-grade glass fiber cloth is formed by weaving warp and weft yarns in a transverse and longitudinal mode, wherein the diameters of single yarns of the warp and weft yarns are 3.5 mu m, and the mass of the glass fiber cloth is 90g/m2The thickness was 0.08mm and the elongation at break was 7%.
And (3) superposing 5 prepregs to form a prepreg layer, covering release films on two surfaces of the prepreg layer, and putting the prepreg layer into a superposed press for pressing and curing to obtain a prefabricated product. Wherein the curing temperature is 150 deg.C, and the curing pressure is 30kg/cm2The curing time was 20 minutes. And finally, removing the release films on the two sides of the prefabricated product to obtain the resin-based composite material. In the resin-based composite material, the mass fraction of the glass fiber cloth in the resin-based composite material is 45%.
Example 6
The resin composition of this example comprised 30 parts by weight of resin B, 70 parts by weight of the second resin, 10 parts by weight of a talc filler (particle size 15 μm), 70 parts by weight of an aluminum dioxide filler (particle size 7 μm), 18 parts by weight of a methylhexahydrophthalic anhydride curing agent, and 60 parts by weight of a PM solvent. Wherein m is 10 and t is 3 in the resin B; x in the second resin is 0.1.
And (3) uniformly coating the resin composition on electronic-grade glass fiber cloth, baking the glass fiber cloth at 160 ℃ for 3min, and cooling the glass fiber cloth to room temperature to obtain a prepreg. The electronic-grade glass fiber cloth is formed by weaving warp and weft yarns in a transverse and longitudinal mode, wherein the diameters of single yarns of the warp and weft yarns are 3.5 mu m, and the mass of the glass fiber cloth is 50g/m2The thickness was 0.045mm and the elongation at break was 3.5%.
And (3) superposing 8 prepregs to form a prepreg layer, covering release films on two surfaces of the prepreg layer, and putting the prepreg layer into a superposed press for pressing and curing to obtain a prefabricated product. Wherein the curing temperature is 150 deg.C, and the curing pressure is 30kg/cm2The curing time was 20 minutes. And finally, removing the release films on the two sides of the prefabricated product to obtain the resin-based composite material. In the resin-based composite material, the mass fraction of the glass fiber cloth in the resin-based composite material is 45%.
Example 7
The resin composition of this example comprised 5 parts by weight of resin A, 5 parts by weight of resin B, 90 parts by weight of the second resin, 40 parts by weight of an aluminum dioxide filler (particle size 7 μm), 20 parts by weight of a phenol novolac, 0.2 parts by weight of a dimethylimidazole accelerator, and 50 parts by weight of a PMA solvent. Wherein, resin A and the second resin are shown in example 1, and resin B is shown in example 4.
And (3) uniformly coating the resin composition on electronic-grade glass fiber cloth, baking the glass fiber cloth at 160 ℃ for 3min, and cooling the glass fiber cloth to room temperature to obtain a prepreg. The electronic-grade glass fiber cloth is formed by weaving warp and weft yarns in a transverse and longitudinal mode, wherein the diameters of single yarns of the warp and weft yarns are 3.5 mu m and 2.5 mu m respectively, and the mass of the glass fiber cloth is 90g/m2The thickness was 0.08mm and the elongation at break was 4%.
And (3) superposing 5 prepregs to form a prepreg layer, covering release films on two surfaces of the prepreg layer, and putting the prepreg layer into a superposed press for pressing and curing to obtain a prefabricated product. Wherein the curing temperature is 150 deg.C, and the curing pressure is 30kg/cm2The curing time was 20 minutes. And finally, removing the release films on the two sides of the prefabricated product to obtain the resin-based composite material. In the resin-based composite material, the mass fraction of the glass fiber cloth in the resin-based composite material is 50%.
Example 8
The resin composition of this example includes 8 parts by weight of resin a, 3 parts by weight of resin B, 89 parts by weight of the second resin, 10 parts by weight of an aluminum hydroxide filler (particle diameter of 18 μm), 40 parts by weight of an aluminum dioxide filler (particle diameter of 10 μm), 12 parts by weight of a methylhexahydrophthalic anhydride curing agent, and 10 parts by weight of a PM solvent. Wherein, resin A and the second resin are shown in example 2, and resin B is shown in example 4.
And (3) uniformly coating the resin composition on electronic-grade glass fiber cloth, baking the glass fiber cloth at 160 ℃ for 3min, and cooling the glass fiber cloth to room temperature to obtain a prepreg. The electronic-grade glass fiber cloth is formed by weaving warp and weft yarns in a transverse and longitudinal mode, wherein the diameters of single yarns of the warp and weft yarns are 3.5 mu m, and the mass of the glass fiber cloth is 90g/m2Is thick and thickThe degree was 0.08mm and the elongation at break was 5%.
And (3) superposing 5 prepregs to form a prepreg layer, covering release films on two surfaces of the prepreg layer, and putting the prepreg layer into a superposed press for pressing and curing to obtain a prefabricated product. Wherein the curing temperature is 150 deg.C, and the curing pressure is 30kg/cm2The curing time was 20 minutes. And finally, removing the release films on the two sides of the prefabricated product to obtain the resin-based composite material. In the resin-based composite material, the mass fraction of the glass fiber cloth in the resin-based composite material is 50%.
Example 9
Example 9 differs from example 1 only in that the glass fiber cloth of example 9 is a conventional glass fiber cloth, the warp and weft yarns have a diameter of 1 μm, and the glass fiber cloth has a mass of 80g/m2The thickness was 0.06mm, and the elongation at break was 2.1%.
Example 10
Example 10 differs from example 1 only in that the glass fiber cloth of example 10 is a conventional glass fiber cloth, the warp and weft yarns have a diameter of 9 μm, and the glass fiber cloth has a mass of 80g/m2The thickness was 0.06mm, and the elongation at break was 8%.
Example 11
Example 11 differs from example 1 only in that the glass cloth of example 11 is a conventional glass cloth, the warp and weft yarns have a diameter of 3.5 μm, and the glass cloth has a mass of 10g/m2The thickness was 0.009mm, and the elongation at break was 4%.
Example 12
Example 12 differs from example 1 only in that the glass fiber cloth of example 12 is a conventional glass fiber cloth, the diameter of the warp and weft is 3.5 μm, and the mass of the glass fiber cloth is 200g/m2The thickness was 0.17mm, and the elongation at break was 4%.
Example 13
Example 13 differs from example 1 in that the filler of the resin composition of example 13 is a silica filler (particle size 30 μm).
Comparative example 1
The comparative example resin composition includes 100 parts by weight of a general bisphenol a type epoxy resin, 20 parts by weight of a silica filler (particle size of 20 μm), 8 parts by weight of a dicyandiamide curing agent, 0.09 parts by weight of a dimethylimidazole accelerator, and 30 parts by weight of a DMF solvent.
And (3) uniformly coating the resin composition on electronic-grade glass fiber cloth, baking the glass fiber cloth at 160 ℃ for 3min, and cooling the glass fiber cloth to room temperature to obtain a prepreg. The electronic-grade glass fiber cloth is formed by weaving warp and weft yarns in a transverse and longitudinal mode, wherein the diameters of single yarns of the warp and weft yarns are 3.5 mu m, and the mass of the glass fiber cloth is 80g/m2The thickness was 0.06mm, and the elongation at break was 4%.
And (3) superposing 7 prepregs to form a prepreg layer, covering release films on two surfaces of the prepreg layer, and putting the prepreg layer into a superposed press for pressing and curing to obtain a prefabricated product. Wherein the curing temperature is 150 deg.C, and the curing pressure is 30kg/cm2The curing time was 20 minutes. And finally, removing the release films on the two sides of the prefabricated product to obtain the resin-based composite material. In the resin-based composite material, the mass fraction of the glass fiber cloth in the resin-based composite material is 55%.
Comparative example 2
The resin composition of this comparative example includes 100 parts by weight of the second resin, 20 parts by weight of a silica filler (particle size of 20 μm), 8 parts by weight of a dicyandiamide curing agent, 0.09 parts by weight of a dimethylimidazole accelerator, and 30 parts by weight of a DMF solvent. Wherein x in the second resin is 5.
And (3) uniformly coating the resin composition on electronic-grade glass fiber cloth, baking the glass fiber cloth at 160 ℃ for 3min, and cooling the glass fiber cloth to room temperature to obtain a prepreg. The electronic-grade glass fiber cloth is formed by weaving warp and weft yarns in a transverse and longitudinal mode, wherein the diameters of single yarns of the warp and weft yarns are 3.5 mu m, and the mass of the glass fiber cloth is 80g/m2The thickness was 0.06mm, and the elongation at break was 4%.
And (3) superposing 7 prepregs to form a prepreg layer, covering release films on two surfaces of the prepreg layer, and putting the prepreg layer into a superposed press for pressing and curing to obtain a prefabricated product. Wherein the curing temperature is 150 ℃ and the curing pressure is 30kgcm2The curing time was 20 minutes. And finally, removing the release films on the two sides of the prefabricated product to obtain the resin-based composite material. In the resin-based composite material, the mass fraction of the glass fiber cloth in the resin-based composite material is 55%.
Comparative example 3
The resin composition of this comparative example includes 100 parts by weight of resin A, 20 parts by weight of silica filler (particle diameter of 20 μm), 8 parts by weight of dicyandiamide curing agent, 0.09 parts by weight of dimethylimidazole accelerator, 30 parts by weight of DMF solvent. Wherein, a is 15 and n is 5 in the resin A.
And (3) uniformly coating the resin composition on electronic-grade glass fiber cloth, baking the glass fiber cloth at 160 ℃ for 3min, and cooling the glass fiber cloth to room temperature to obtain a prepreg. The electronic-grade glass fiber cloth is formed by weaving warp and weft yarns in a transverse and longitudinal mode, wherein the diameters of single yarns of the warp and weft yarns are 3.5 mu m, and the mass of the glass fiber cloth is 80g/m2The thickness was 0.06mm, and the elongation at break was 4%.
And (3) superposing 7 prepregs to form a prepreg layer, covering release films on two surfaces of the prepreg layer, and putting the prepreg layer into a superposed press for pressing and curing to obtain a prefabricated product. Wherein the curing temperature is 150 deg.C, and the curing pressure is 30kg/cm2The curing time was 20 minutes. And finally, removing the release films on the two sides of the prefabricated product to obtain the resin-based composite material. In the resin-based composite material, the mass fraction of the glass fiber cloth in the resin-based composite material is 55%.
Comparative example 4
The resin composition of this example included 5 parts by weight of a general bisphenol a type epoxy resin, 95 parts by weight of a second resin, 20 parts by weight of a silica filler (particle size of 20 μm), 8 parts by weight of a dicyandiamide curing agent, 0.09 parts by weight of a dimethylimidazole accelerator, and 30 parts by weight of a DMF solvent. Wherein x in the second resin is 5.
And (3) uniformly coating the resin composition on electronic-grade glass fiber cloth, baking the glass fiber cloth at 160 ℃ for 3min, and cooling the glass fiber cloth to room temperature to obtain a prepreg. Wherein the electronic grade glass fiber cloth is formed by warp and weft yarns through horizontal and vertical weaving, wherein,the single yarn diameter of the warp and weft yarns is 3.5 mu m, and the mass of the glass fiber cloth is 80g/m2The thickness was 0.06mm, and the elongation at break was 4%.
And (3) superposing 7 prepregs to form a prepreg layer, covering release films on two surfaces of the prepreg layer, and putting the prepreg layer into a superposed press for pressing and curing to obtain a prefabricated product. Wherein the curing temperature is 150 deg.C, and the curing pressure is 30kg/cm2The curing time was 20 minutes. And finally, removing the release films on the two sides of the prefabricated product to obtain the resin-based composite material. In the resin-based composite material, the mass fraction of the glass fiber cloth in the resin-based composite material is 55%.
Comparative example 5
The resin composition of this example comprised 5 parts by weight of resin A, 95 parts by weight of a general bisphenol A type epoxy resin, 20 parts by weight of a silica filler (particle size of 20 μm), 8 parts by weight of a dicyandiamide curing agent, 0.09 parts by weight of a dimethylimidazole accelerator, and 30 parts by weight of a DMF solvent. Wherein, a is 15 and n is 5 in the resin A.
And (3) uniformly coating the resin composition on electronic-grade glass fiber cloth, baking the glass fiber cloth at 160 ℃ for 3min, and cooling the glass fiber cloth to room temperature to obtain a prepreg. The electronic-grade glass fiber cloth is formed by weaving warp and weft yarns in a transverse and longitudinal mode, wherein the diameters of single yarns of the warp and weft yarns are 3.5 mu m, and the mass of the glass fiber cloth is 80g/m2The thickness was 0.06mm, and the elongation at break was 4%.
And (3) superposing 7 prepregs to form a prepreg layer, covering release films on two surfaces of the prepreg layer, and putting the prepreg layer into a superposed press for pressing and curing to obtain a prefabricated product. Wherein the curing temperature is 150 deg.C, and the curing pressure is 30kg/cm2The curing time was 20 minutes. And finally, removing the release films on the two sides of the prefabricated product to obtain the resin-based composite material. In the resin-based composite material, the mass fraction of the glass fiber cloth in the resin-based composite material is 55%.
Comparative example 6
The resin composition of this example comprised 100 parts by weight of resin B, 25 parts by weight of an aluminum hydroxide filler (particle diameter 15 μm), 5 parts by weight of a dicyandiamide curing agent, 0.5 parts by weight of a diethyltetramethylimidazole accelerator, and 40 parts by weight of DMF solvent. Wherein m is 100 and t is 0 in the resin B.
And (3) uniformly coating the resin composition on electronic-grade glass fiber cloth, baking the glass fiber cloth at 160 ℃ for 3min, and cooling the glass fiber cloth to room temperature to obtain a prepreg. The electronic-grade glass fiber cloth is formed by weaving warp and weft yarns in a transverse and longitudinal mode, wherein the diameters of single yarns of the warp and weft yarns are 1.5 mu m, and the mass of the glass fiber cloth is 20g/m2The thickness was 0.01mm, and the elongation at break was 4%.
And (3) superposing 20 prepregs to form a prepreg layer, covering release films on two surfaces of the prepreg layer, and putting the prepreg layer into a superposed press for pressing and curing to obtain a prefabricated product. Wherein the curing temperature is 150 deg.C, and the curing pressure is 30kg/cm2The curing time was 20 minutes. And finally, removing the release films on the two sides of the prefabricated product to obtain the resin-based composite material. In the resin-based composite material, the mass fraction of the glass fiber cloth in the resin-based composite material is 65%.
Comparative example 7
Based on example 1, the mass fraction of the glass fiber cloth in the resin-based composite material was adjusted to 15%.
Comparative example 8
Based on example 1, the mass fraction of the glass fiber cloth in the resin-based composite material was adjusted to 70%.
The resin-based composite materials of examples 1 to 13 and comparative examples 1 to 8 were subjected to the performance test, and the results are shown in Table 1.
Wherein, the bending strength, the glass transition temperature and the thermal expansion coefficient are implemented according to the IPC-TM-650 test standard, and the tensile strength is implemented according to the GB/T1447-2005 test standard.
TABLE 1
From examples 9 to 12, it is known that the warp and weft yarn diameter, the breaking growth rate, the gram weight and the thickness of the glass fiber cloth affect the mechanical property or the bending effect of the composite material.
It is understood from example 13 that the bending effect of the composite material is also affected when the particle size of the filler is too large.
As is clear from comparative examples 3 and 6, when the first resin is used alone, the glass transition temperature of the resin-based composite material is too low and the thermal expansion coefficient is large, which is not satisfactory.
As can be seen from comparative example 2, when the second resin was used alone, the glass transition temperature of the resin-based composite material was high, and the material had a bending angle of only 60 degrees, which was not satisfactory.
From comparative examples 1, 4 and 5, it is clear that the use of bisphenol a epoxy resin molding materials does not simultaneously satisfy the material property requirements in terms of glass transition temperature or bending angle.
It is understood from comparative examples 7 and 8 that the glass fiber cloth cannot be molded when the content is too low, and the bending angle is only 55 ° when the content is too high, and the requirements are not satisfied.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (11)
1. A resin composition comprising a first resin, a second resin, a filler, an auxiliary agent, and a solvent, wherein the first resin comprises at least one of a resin A or a resin B,
the structural formula of the resin A is shown as a formula (1),
in the formula (1), R1Is CaH2aAnd has no branched chain, a is more than or equal to 5 and less than or equal to 30, and n is more than or equal to 1 and less than or equal to 10;
the structural formula of the resin B is shown as a formula (2),
in the formula (2), m is more than or equal to 10 and less than or equal to 100, and t is more than or equal to 0 and less than or equal to 50;
the structural formula of the second resin is shown as a formula (3),
in the formula (3), x is more than or equal to 0.1 and less than or equal to 10.
2. The resin composition according to claim 1, wherein the filler is an inorganic filler, and the particle size of the filler is 2 μm to 20 μm.
3. The resin composition according to any one of claims 1 to 2, wherein the mass of the first resin is 5 to 40 parts by weight, the mass of the second resin is 60 to 95 parts by weight, the mass of the filler is 20 to 100 parts by weight, the mass of the auxiliary is 0.01 to 22 parts by weight, and the mass of the solvent is 10 to 100 parts by weight.
4. The resin composition according to claim 3, wherein the mass of the filler is 2 times to 5 times the mass of the first resin.
5. The resin composition according to claim 4, wherein the auxiliary agent comprises at least one of a curing agent and an accelerator.
6. A method for preparing a resin-based composite material, comprising:
providing a fiber cloth;
forming the resin composition according to any one of claims 1 to 5 on the fiber cloth and drying to obtain a prepreg;
overlapping at least two prepregs to form a prepreg layer, covering release films on two sides of the prepreg layer, and curing to obtain a prefabricated product;
and removing the release film in the prefabricated product to obtain the resin-based composite material, wherein the mass fraction of the fiber cloth in the resin-based composite material is 20-65%.
7. The method for preparing the resin-based composite material according to claim 6, wherein the fiber cloth is formed by warp and weft yarns through weft and warp knitting, and the single yarn diameter of the warp and weft yarns is 1.5 μm to 4 μm.
8. The method for preparing the resin-based composite material according to claim 6 or 7, wherein the fiber cloth has an elongation at break of 3.5% -7%;
and/or the mass of the fiber cloth is 20g/m2-110g/m2The thickness is 0.01mm-0.1 mm.
9. The method for preparing a resin-based composite material according to claim 6, wherein the fiber cloth is further subjected to a coupling agent treatment and/or an ultrasonic treatment before the resin composition according to any one of claims 1 to 7 is formed on the fiber cloth and dried.
10. A resin-based composite material obtainable by a process for the preparation of a resin-based composite material according to any one of claims 6 to 9.
11. Use of the resin-based composite material according to claim 10 in electronic products.
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| CN112724598A (en) * | 2020-12-28 | 2021-04-30 | 广东盈骅新材料科技有限公司 | Resin composition, prepreg and preparation method and application thereof |
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| CA2999423A1 (en) * | 2015-09-30 | 2017-04-06 | Nippon Steel & Sumikin Chemical Co., Ltd. | Curable epoxy resin composition, and fiber-reinforced composite material obtained using same |
| CN107953630A (en) * | 2017-12-21 | 2018-04-24 | 浙江华正新材料股份有限公司 | Heated flexible molding copper-clad plate of one kind and preparation method thereof |
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