CN113004655A - Preparation method of glass fiber reinforced thermosetting resin prepreg - Google Patents
Preparation method of glass fiber reinforced thermosetting resin prepreg Download PDFInfo
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- CN113004655A CN113004655A CN201911332090.3A CN201911332090A CN113004655A CN 113004655 A CN113004655 A CN 113004655A CN 201911332090 A CN201911332090 A CN 201911332090A CN 113004655 A CN113004655 A CN 113004655A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/24—Impregnating materials with prepolymers which can be polymerised in situ, e.g. manufacture of prepregs
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/04—Reinforcing macromolecular compounds with loose or coherent fibrous material
- C08J5/06—Reinforcing macromolecular compounds with loose or coherent fibrous material using pretreated fibrous materials
- C08J5/08—Reinforcing macromolecular compounds with loose or coherent fibrous material using pretreated fibrous materials glass fibres
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2363/00—Characterised by the use of epoxy resins; Derivatives of epoxy resins
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- 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
- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
- C08K13/06—Pretreated ingredients and ingredients covered by the main groups C08K3/00 - C08K7/00
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- 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
- C08K2201/00—Specific properties of additives
- C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K
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- 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
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- 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
- C08K7/10—Silicon-containing compounds
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- 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
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- 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
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
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Abstract
The invention provides a preparation method of a glass fiber reinforced thermosetting resin prepreg, which comprises the following steps: firstly, treating a nano material by adopting a silane coupling agent, then adding an organic solvent into the treated nano material, and uniformly stirring to obtain a mixture; secondly, adding a filler into the mixture, and performing ultrasonic dispersion treatment; thirdly, adding the mixture subjected to the ultrasonic dispersion treatment into the molten epoxy resin treated by the epoxy-containing silane coupling agent, and uniformly stirring to obtain an impregnation liquid; and fourthly, placing the glass fiber treated by the silane coupling agent into an impregnating solution for impregnation to obtain the glass fiber reinforced thermosetting resin prepreg. The glass fiber reinforced thermosetting resin prepreg prepared by the method has the tensile strength of more than 500MPa and the bending strength of more than 800MPa after molding and curing.
Description
Technical Field
The invention belongs to the technical field of fiber reinforced composite materials, and particularly relates to a preparation method of a glass fiber reinforced thermosetting resin prepreg.
Background
The glass fiber reinforced thermosetting resin is a fiber reinforced composite material which adopts glass fiber as a reinforcing material and thermosetting resin (including epoxy resin, phenolic resin, epoxy resin and the like) as a matrix, and is widely applied to the fields of aviation, aerospace, automobiles, ships, circuit boards, wind power and the like due to the characteristics of small specific gravity, high specific strength and the like.
Epoxy resins are excellent thermosetting resins. Compared with unsaturated polyester resin which is widely applied at present, the modified polyester resin has better mechanical property, electrical insulation property, chemical resistance, heat resistance and adhesive property. The glass fiber reinforced epoxy resin composite material is a composite material with wide application, and has the characteristics of light weight, high strength, large modulus, good corrosion resistance, excellent electrical property and the like. How to further improve the mechanical properties of the glass fiber reinforced epoxy resin composite material is an important direction for the research of the technicians in the field.
Disclosure of Invention
The technical problem to be solved by the present invention is to provide a method for preparing a glass fiber reinforced thermosetting resin prepreg, aiming at the defects in the prior art. The glass fiber reinforced thermosetting resin prepreg prepared by the method has the tensile strength of more than 500MPa and the bending strength of more than 800MPa after molding and curing.
In order to solve the technical problems, the invention adopts the technical scheme that: the preparation method of the glass fiber reinforced thermosetting resin prepreg is characterized by comprising the following steps:
step one, treating a nano material by adopting a silane coupling agent, then adding an organic solvent into the treated nano material, and uniformly stirring to obtain a mixture; the nano material is nano potassium hexatitanate, nano silicate or nano SiO2And nanoscale Al2O3One or more of the above; the organic solvent is acetone, and the mass of the organic solvent is 10-15% of that of the nano material;
step two, adding a filler into the mixture obtained in the step one, and performing ultrasonic dispersion treatment; the filler is micron-sized talcum powder and Si3N4One or more of crystal whisker and SiC crystal whisker;
step three, adding the mixture subjected to the ultrasonic dispersion treatment in the step two into molten epoxy resin treated by the epoxy-containing silane coupling agent, and uniformly stirring to obtain an impregnation liquid; the mass content of the nano material in the impregnation liquid is 1-5%, and the mass content of the filler is 1-3%;
step four, placing the glass fiber treated by the silane coupling agent into the impregnating solution in step three for impregnation to obtain a glass fiber reinforced thermosetting resin prepreg; the volume percentage content of the impregnating solution in the glass fiber reinforced thermosetting resin prepreg is 20-30%.
The preparation method of the glass fiber reinforced thermosetting resin prepreg is characterized in that the stirring speed in the step one is 5000-7000 rpm.
The preparation method of the glass fiber reinforced thermosetting resin prepreg is characterized in that in the step one, the silane coupling agent is KH 560.
The preparation method of the glass fiber reinforced thermosetting resin prepreg is characterized in that in the third step, the epoxy-containing silane coupling agent is KH 560.
The preparation method of the glass fiber reinforced thermosetting resin prepreg is characterized in that the silane coupling agent is KH560 in the fourth step.
Compared with the prior art, the invention has the following advantages:
the invention adopts the epoxy resin treated by the silane coupling agent containing epoxy groups, and adds the nano material and the filler into the resin, thereby obviously improving the mechanical property of the thermosetting resin. The glass fiber reinforced thermosetting resin prepreg prepared by the method has the tensile strength of more than 500MPa and the bending strength of more than 800MPa after molding and curing.
The technical solution of the present invention is further described in detail with reference to the following examples.
Detailed Description
Example 1
The preparation method of the glass fiber reinforced thermosetting resin prepreg of the embodiment comprises the following steps:
step one, treating a nano material by using a silane coupling agent KH560, then adding an organic solvent into the treated nano material, and uniformly stirring to obtain a mixture; the nano material is nano potassium hexatitanate; the organic solvent is acetone, and the mass of the organic solvent is 10% of that of the nano material; the stirring speed is 5000 rpm;
step two, adding a filler into the mixture obtained in the step one, and performing ultrasonic dispersion treatment; the filler is micron-sized talcum powder;
step three, adding the mixture subjected to the ultrasonic dispersion treatment in the step two into molten epoxy resin treated by the epoxy-containing silane coupling agent, and uniformly stirring to obtain an impregnation liquid; the mass content of the nano material in the impregnation liquid is 1%, and the mass content of the filler is 3%; the silane coupling agent containing epoxy groups is KH 560;
step four, placing the glass fiber treated by the silane coupling agent KH560 into the impregnation liquid in step three for impregnation to obtain a glass fiber reinforced thermosetting resin prepreg; the volume percentage content of the impregnating solution in the glass fiber reinforced thermosetting resin prepreg is 20%.
The tensile strength of the glass fiber reinforced thermosetting resin prepreg prepared in the embodiment reaches more than 500MPa after molding and curing, and the bending strength reaches more than 800 MPa.
Example 2
The preparation method of the glass fiber reinforced thermosetting resin prepreg of the embodiment comprises the following steps:
step one, treating a nano material by using a silane coupling agent KH560, then adding an organic solvent into the treated nano material, and uniformly stirring to obtain a mixture; the nano material is nano Al2O3(ii) a The organic solvent is acetone, and the mass of the organic solvent is 15% of that of the nano material; the stirring rate is 7000 rpm;
step two, adding a filler into the mixture obtained in the step one, and performing ultrasonic dispersion treatment; the filler is Si3N4Whisker;
step three, adding the mixture subjected to the ultrasonic dispersion treatment in the step two into molten epoxy resin treated by the epoxy-containing silane coupling agent, and uniformly stirring to obtain an impregnation liquid; the mass content of the nano material in the impregnation liquid is 5%, and the mass content of the filler is 1%; the silane coupling agent containing epoxy groups is KH 560;
step four, placing the glass fiber treated by the silane coupling agent KH560 into the impregnation liquid in step three for impregnation to obtain a glass fiber reinforced thermosetting resin prepreg; the volume percentage content of the impregnating solution in the glass fiber reinforced thermosetting resin prepreg is 30%.
The tensile strength of the glass fiber reinforced thermosetting resin prepreg prepared in the embodiment reaches more than 500MPa after molding and curing, and the bending strength reaches more than 800 MPa.
Example 3
The preparation method of the glass fiber reinforced thermosetting resin prepreg of the embodiment comprises the following steps:
step one, treating a nano material by using a silane coupling agent KH560, then adding an organic solvent into the treated nano material, and uniformly stirring to obtain a mixture; the nano material is nano silicate or nano SiO2And nanoscale Al2O3(the mass ratio is 1:1: 1); the organic solvent is acetone, and the mass of the organic solvent is 12% of that of the nano material; the stirring speed is 6000 rpm;
step two, adding a filler into the mixture obtained in the step one, and performing ultrasonic dispersion treatment; the filler is micron-sized talcum powder and Si3N4Crystal whisker (the mass ratio is 2: 1);
step three, adding the mixture subjected to the ultrasonic dispersion treatment in the step two into molten epoxy resin treated by the epoxy-containing silane coupling agent, and uniformly stirring to obtain an impregnation liquid; the mass content of the nano material in the impregnation liquid is 3%, and the mass content of the filler is 2%; the silane coupling agent containing epoxy groups is KH 560;
step four, placing the glass fiber treated by the silane coupling agent KH560 into the impregnation liquid in step three for impregnation to obtain a glass fiber reinforced thermosetting resin prepreg; the volume percentage content of the impregnating solution in the glass fiber reinforced thermosetting resin prepreg is 30%.
The tensile strength of the glass fiber reinforced thermosetting resin prepreg prepared in the embodiment reaches more than 500MPa after molding and curing, and the bending strength reaches more than 800 MPa.
Example 4
The preparation method of the glass fiber reinforced thermosetting resin prepreg of the embodiment comprises the following steps:
step one, treating a nano material by using a silane coupling agent KH560, then adding an organic solvent into the treated nano material, and uniformly stirring to obtain a mixture; the nano material is nano silicate and nano SiO2(the mass ratio is 3: 1); the organic solvent is acetone, and the mass of the organic solvent is 12% of that of the nano material; the stirring speed is 6000 rpm;
step two, adding a filler into the mixture obtained in the step one, and performing ultrasonic dispersion treatment; the filler is micron-sized talcum powder and Si3N4Crystal whiskers and SiC crystal whiskers (the mass ratio is 2:1: 2);
step three, adding the mixture subjected to the ultrasonic dispersion treatment in the step two into molten epoxy resin treated by the epoxy-containing silane coupling agent, and uniformly stirring to obtain an impregnation liquid; the mass content of the nano material in the impregnation liquid is 4%, and the mass content of the filler is 1%; the silane coupling agent containing epoxy groups is KH 560;
step four, placing the glass fiber treated by the silane coupling agent KH560 into the impregnation liquid in step three for impregnation to obtain a glass fiber reinforced thermosetting resin prepreg; the volume percentage content of the impregnating solution in the glass fiber reinforced thermosetting resin prepreg is 30%.
The tensile strength of the glass fiber reinforced thermosetting resin prepreg prepared in the embodiment reaches more than 500MPa after molding and curing, and the bending strength reaches more than 800 MPa.
Example 5
The preparation method of the glass fiber reinforced thermosetting resin prepreg of the embodiment comprises the following steps:
step one, treating a nano material by using a silane coupling agent KH560, then adding an organic solvent into the treated nano material, and uniformly stirring to obtain a mixture; the nano material is nano potassium hexatitanate, nano silicate or nano SiO2And nanoscale Al2O3(the mass ratio is 2:1:1: 2); the organic solvent is acetone, and the mass of the organic solvent is 12% of that of the nano material; the stirring rate is 7000 rpm;
step two, adding a filler into the mixture obtained in the step one, and performing ultrasonic dispersion treatment; the filler is Si3N4Crystal whiskers and SiC crystal whiskers (the mass ratio is 1: 1);
step three, adding the mixture subjected to the ultrasonic dispersion treatment in the step two into molten epoxy resin treated by the epoxy-containing silane coupling agent, and uniformly stirring to obtain an impregnation liquid; the mass content of the nano material in the impregnation liquid is 2%, and the mass content of the filler is 3%; the silane coupling agent containing epoxy groups is KH 560;
step four, placing the glass fiber treated by the silane coupling agent KH560 into the impregnation liquid in step three for impregnation to obtain a glass fiber reinforced thermosetting resin prepreg; the volume percentage content of the impregnating solution in the glass fiber reinforced thermosetting resin prepreg is 30%.
The tensile strength of the glass fiber reinforced thermosetting resin prepreg prepared in the embodiment reaches more than 500MPa after molding and curing, and the bending strength reaches more than 800 MPa.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and all simple modifications, changes and equivalent structural changes made to the above embodiment according to the technical spirit of the present invention still fall within the protection scope of the technical solution of the present invention.
Claims (5)
1. The preparation method of the glass fiber reinforced thermosetting resin prepreg is characterized by comprising the following steps:
step one, treating a nano material by adopting a silane coupling agent, then adding an organic solvent into the treated nano material, and uniformly stirring to obtain a mixture; the nano material is nano potassium hexatitanate, nano silicate or nano SiO2And nanoscale Al2O3One or more of the above; the organic solvent is acetone, and the mass of the organic solvent is 10-15% of that of the nano material;
step two, adding a filler into the mixture obtained in the step one, and performing ultrasonic dispersion treatment; the filler is micron-sized talcum powder and Si3N4One or more of crystal whisker and SiC crystal whisker;
step three, adding the mixture subjected to the ultrasonic dispersion treatment in the step two into molten epoxy resin treated by the epoxy-containing silane coupling agent, and uniformly stirring to obtain an impregnation liquid; the mass content of the nano material in the impregnation liquid is 1-5%, and the mass content of the filler is 1-3%;
step four, placing the glass fiber treated by the silane coupling agent into the impregnating solution in step three for impregnation to obtain a glass fiber reinforced thermosetting resin prepreg; the volume percentage content of the impregnating solution in the glass fiber reinforced thermosetting resin prepreg is 20-30%.
2. The method according to claim 1, wherein the stirring speed in the first step is 5000-7000 rpm.
3. The method for preparing a glass fiber reinforced thermosetting resin prepreg according to claim 1, wherein the silane coupling agent in the first step is KH 560.
4. The method for preparing a glass fiber reinforced thermosetting resin prepreg according to claim 1, wherein the epoxy-containing silane coupling agent in step three is KH 560.
5. The method for preparing a glass fiber reinforced thermosetting resin prepreg according to claim 1, wherein the silane coupling agent in the fourth step is KH 560.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114262481A (en) * | 2021-12-28 | 2022-04-01 | 广东圆融新材料有限公司 | Polypropylene material with low warpage and low shrinkage performance and preparation method thereof |
| CN114539707A (en) * | 2022-02-24 | 2022-05-27 | 浙江杭欧实业股份有限公司 | Reinforced MPP material, preparation method thereof and prepared cable protection tube |
-
2019
- 2019-12-21 CN CN201911332090.3A patent/CN113004655A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114262481A (en) * | 2021-12-28 | 2022-04-01 | 广东圆融新材料有限公司 | Polypropylene material with low warpage and low shrinkage performance and preparation method thereof |
| CN114539707A (en) * | 2022-02-24 | 2022-05-27 | 浙江杭欧实业股份有限公司 | Reinforced MPP material, preparation method thereof and prepared cable protection tube |
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