CN110845829A - Low-temperature curing epoxy resin composition and preparation method of prepreg and composite material thereof - Google Patents
Low-temperature curing epoxy resin composition and preparation method of prepreg and composite material thereof Download PDFInfo
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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
- C08L63/04—Epoxynovolacs
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
- C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
- C08G59/4007—Curing agents not provided for by the groups C08G59/42 - C08G59/66
- C08G59/4014—Nitrogen containing compounds
- C08G59/4021—Ureas; Thioureas; Guanidines; Dicyandiamides
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
- C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
- C08G59/50—Amines
- C08G59/504—Amines containing an atom other than nitrogen belonging to the amine group, carbon and hydrogen
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
- C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
- C08G59/50—Amines
- C08G59/5046—Amines heterocyclic
- C08G59/5053—Amines heterocyclic containing only nitrogen as a heteroatom
- C08G59/5073—Amines heterocyclic containing only nitrogen as a heteroatom having two nitrogen atoms in the ring
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
- C08G59/68—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the catalysts used
- C08G59/686—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the catalysts used containing nitrogen
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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
- C08J2363/00—Characterised by the use of epoxy resins; Derivatives of epoxy resins
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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
- C08J2363/04—Epoxynovolacs
-
- 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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- Manufacturing & Machinery (AREA)
- Reinforced Plastic Materials (AREA)
- Epoxy Resins (AREA)
Abstract
The invention discloses a low-temperature curing epoxy resin composition and a preparation method of a prepreg and a composite material thereof, relating to the technical field of high polymer materials, wherein the epoxy resin composition comprises the following components in parts by weight: 60-80 parts of phenolic epoxy resin, 20-40 parts of bisphenol A epoxy resin, 5-25 parts of toughening agent and 6-15 parts of compound curing agent; the compound curing system is specifically composed of the following components in parts by weight: 3-6 parts of dicyandiamide, 3-5 parts of an organic urea accelerator URAcc 572 and 8-8 parts of an imidazole latent curing agent PN-235, wherein the prepreg prepared from the low-temperature curing epoxy resin composition disclosed by the invention has a long viscous life at 23 +/-2 ℃, and the cured composite material can show excellent mechanical property and heat resistance, can realize low-temperature curing and has a long service time, is suitable for preparing large-size composite material structural members and is beneficial to popularization of the structural members.
Description
Technical Field
The invention relates to the technical field of high polymer materials, in particular to a low-temperature curing epoxy resin composition, and a preparation method of a prepreg and a composite material thereof.
Background
The fiber reinforced composite material has the characteristics of light weight, high strength and high rigidity, so the fiber reinforced composite material has a wide application range from the sports and leisure fields such as fishing rods and golf clubs to the industrial application fields such as automobiles, airplanes, unmanned planes and the like. In the manufacturing process of the composite material product, the prepreg is an intermediate material, the prepreg is generally obtained by infiltrating reinforcing fibers with resin, and the content of the reinforcing fibers can be controlled at a relatively high proportion according to design requirements. The forming process of obtaining the fiber reinforced composite material by the prepreg comprises hand lay-up, autoclave, vacuum bag pressing and compression molding.
The curing temperature of the existing general fiber reinforced resin matrix composite material is 120 ℃ or above, the heat release amount of the epoxy resin is large in the curing process, certain thermal stress exists in the cured product, the performance of the product can be influenced, and the thermal stress of the low-temperature cured epoxy resin is small; on the other hand, some manufacturers of large-sized composite structural members desire to employ low-temperature curing to reduce manufacturing cost, and the use of low-temperature curing for composite metal connectors can reduce the influence of product size due to the heat deformability of the two materials. In addition, the epoxy resin which can be cured at low temperature generally cannot meet the requirement of the paving period of large-sized parts due to high activity and short storage life at room temperature. Therefore, it is necessary to develop an epoxy resin for low-temperature curing prepreg, which has a long tack life at room temperature.
Disclosure of Invention
The invention aims to: the low-temperature curing epoxy resin composition, the prepreg thereof and the preparation method of the composite material are provided, and the problem that the existing low-temperature curing epoxy resin cannot meet the paving period requirement of large-sized parts due to high activity and short room-temperature storage life is solved.
The technical scheme adopted by the invention is as follows:
the low-temperature curing epoxy resin composition comprises the following components in parts by weight: 60-80 parts of phenolic epoxy resin, 20-40 parts of bisphenol A epoxy resin, 5-25 parts of toughening agent and 6-15 parts of compound curing agent;
the compound curing system is specifically composed of the following components in parts by weight: 3-6 parts of dicyandiamide, 572-5 parts of organic urea accelerator and 8-235 parts of imidazole latent curing agent PN-235.
According to the invention, the cured phenolic epoxy resin has high crosslinking density, can provide excellent heat resistance, strength, modulus, water resistance and corrosion resistance, and has a faster reaction rate with the compound curing agent of the invention at 80 ℃; the bisphenol A epoxy resin is mainly used for adjusting the viscosity of a system, so that the resin system can be suitable for preparing a prepreg by a hot melting method and has proper viscosity; the toughening agent is used for improving the toughness and the film forming property of the system;
further, the epoxy resin composition is composed of the following components in parts by weight: 70-80 parts of phenolic epoxy resin, 20-30 parts of bisphenol A epoxy resin, 10-20 parts of toughening agent and 8-15 parts of compound curing agent;
further, the phenolic epoxy resin is specifically one or more of NPPN-631 and NPPN-638S, but is not limited to the above product grades, as long as the product types are the same.
Further, the bisphenol A epoxy resin is specifically one or more of NPEL-127, NPEL-128, NPES-901, NPES-902 and NPES-904, but is not limited to the above product brands, as long as the above product types are acceptable.
Further, the toughening agent is specifically one or more of MX153, MX154, MX217 and MX227, the core-shell rubber toughening agents have good dispersibility, the Tg of the cured resin can be kept not to be reduced by adding the toughening agent, and meanwhile, the toughness of the system can be improved, but common rubber toughening agents such as one or more of carboxyl-terminated butadiene-acrylonitrile rubber, amino-terminated butadiene-acrylonitrile rubber and epoxy-terminated butadiene-acrylonitrile rubber can also be adopted.
A preparation method of a low-temperature curing epoxy resin composition specifically comprises the following steps:
a) under the heating condition of 90-110 ℃, 60-80 parts of novolac epoxy resin and 20-40 parts of bisphenol A epoxy resin are uniformly mixed until completely dissolved;
b) and cooling the mixture to 50-55 ℃, adding 5-25 parts of toughening agent and 6-15 parts of compound curing agent, and uniformly mixing under a vacuum condition to obtain the epoxy resin composition.
A preparation method of a prepreg of a low-temperature curing epoxy resin composition comprises the following specific steps: baking the epoxy resin composition of claim 1 to a fluid state, coating with a coating device to obtain a resin film, and heating and compounding the resin film and a fiber reinforced material sheet to obtain the prepreg, wherein the prepreg is in a flexible state at room temperature and has good spreadability and drapability, and the viscosity can still meet the manufacturing requirements of composite material products after the prepreg is placed at room temperature for 30 days.
Further, the fibrous reinforcement sheet is present in the prepreg in an amount of 60% to 70%, typically at least 68% by mass. However, in industrial and aerospace applications, high performance is required of the material, and thus continuous fiber manufacture is preferred, typically at a level of 30% to 70%, particularly at a level of 50% to 70% by volume.
A preparation method of a composite material of a low-temperature curing epoxy resin composition specifically comprises the following steps:
a prepreg prepared according to claim 7 is placed on a mold and cured according to a curing cycle to obtain a composite of the epoxy resin composition.
Further, the curing period is specifically that the curing temperature is increased from room temperature to 80 ℃ at a temperature increase rate of 2 ℃/min, the temperature is maintained for 120min, then the curing period is cooled to room temperature, and in the curing process, 1 bar-6.5 bar of pressure is required to be added to exhaust gas so as to reduce the formation of pores, and the curing temperature is generally higher than 70 ℃, preferably 80-100 ℃.
In summary, due to the adoption of the technical scheme, the invention has the beneficial effects that:
the prepreg of the low-temperature curing epoxy resin composition provided by the invention has a viscous service life of 30 days at 23 +/-2 ℃; the prepreg of the low-temperature curing epoxy resin composition provided by the invention can be cured for 120min at 80 ℃ to obtain a composite material with excellent mechanical properties.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
Heating the mixed reaction kettle to 90 ℃, adding 70 parts of phenolic epoxy resin NPPN-638S, 70 parts of bisphenol A epoxy resin NPEL-12810 parts and 120 parts of NPES-90120 parts, and stirring until the components are completely dissolved to form a uniform transparent state; cooling to 55 ℃, respectively adding the toughening agent MX-15415 parts and the compound curing agent 10 parts, stirring while vacuumizing, uniformly mixing, and discharging for later use.
And coating the epoxy resin composition on a coating device, compounding the epoxy resin composition with the basalt fiber fabric, and performing hot-pressing impregnation to obtain the low-temperature cured basalt fiber fabric prepreg. The prepreg is placed in a thermostatic chamber at 23 +/-2 ℃, the viscosity change of the prepreg is observed, and the viscosity life of the prepreg can reach 30 days.
According to the requirements of mechanical property (compression property, bending property and interlaminar shear property) test and DMA test sample, respectively preparing a laminated board, adopting vacuum bag press molding, preserving heat for 120min at 80 ℃, cooling, demoulding to obtain a low-temperature cured composite material, and cutting the laminated board into required sample size for testing.
The test results are shown in Table 1.
Example 2
Heating the mixed reaction kettle to 90 ℃, adding 40 parts of phenolic epoxy resin NPPN-63140, NPPN-638S and 130 parts of bisphenol A epoxy resin NPES-90, and stirring until the materials are completely dissolved to form a uniform transparent state; cooling to 55 ℃, respectively adding the toughening agent MX-15415 parts and the compound curing agent 10 parts, stirring while vacuumizing, uniformly mixing, and discharging for later use.
And coating the epoxy resin composition on a coating device, compounding the epoxy resin composition with the basalt fiber fabric, and performing hot-pressing impregnation to obtain the low-temperature cured basalt fiber fabric prepreg. The prepreg is placed in a thermostatic chamber at 23 +/-2 ℃, the viscosity change of the prepreg is observed, and the viscosity life of the prepreg can reach 30 days.
According to the requirements of mechanical property (compression property, bending property and interlaminar shear property) test and DMA test sample, respectively preparing a laminated board, adopting vacuum bag press molding, preserving heat for 120min at 80 ℃, cooling, demoulding to obtain a low-temperature cured composite material, and cutting the laminated board into required sample size for testing.
The test results are shown in Table 1.
Example 3
Heating the mixed reaction kettle to 90 ℃, adding phenolic epoxy resin NPPN-63150 parts, NPPN-638S 30 parts and bisphenol A epoxy resin NPES 90220 parts, and stirring until the materials are completely dissolved to form a uniform transparent state; cooling to 55 ℃, respectively adding the toughening agent MX-15415 parts and the compound curing agent 10 parts, stirring while vacuumizing, uniformly mixing, and discharging for later use.
And coating the epoxy resin composition on a coating device, compounding the epoxy resin composition with the basalt fiber fabric, and performing hot-pressing impregnation to obtain the low-temperature cured basalt fiber fabric prepreg. The prepreg is placed in a thermostatic chamber at 23 +/-2 ℃, the viscosity change of the prepreg is observed, and the viscosity life of the prepreg can reach 30 days.
According to the requirements of mechanical property (compression property, bending property and interlaminar shear property) test and DMA test sample, respectively preparing a laminated board, adopting vacuum bag press molding, preserving heat for 120min at 80 ℃, cooling, demoulding to obtain a low-temperature cured composite material, and cutting the laminated board into required sample size for testing.
The test results are shown in Table 1.
Table 1: epoxy resin composition and composite material performance
In conclusion, the prepreg prepared from the low-temperature curing epoxy resin composition disclosed by the invention has a long viscous life at 23 +/-2 ℃, the cured composite material can show excellent mechanical property and heat resistance, low-temperature curing can be realized, the service life is long, and the prepreg is suitable for preparing large-size composite material structural members and is beneficial to popularization of the structural members.
Although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that various changes in the embodiments and/or modifications of the embodiments and/or portions thereof may be made, and all changes, equivalents, and modifications which fall within the spirit and scope of the invention are therefore intended to be embraced by the appended claims.
Claims (10)
1. The low-temperature curing epoxy resin composition is characterized by comprising the following components in parts by weight: 60-80 parts of phenolic epoxy resin, 20-40 parts of bisphenol A epoxy resin, 5-25 parts of toughening agent and 6-15 parts of compound curing agent;
the compound curing system is specifically composed of the following components in parts by weight: 3-6 parts of dicyandiamide, 572-5 parts of organic urea accelerator and 8-235 parts of imidazole latent curing agent PN-235.
2. The low-temperature curing epoxy resin composition as claimed in claim 1, wherein the epoxy resin composition comprises the following components in parts by weight: 70-80 parts of phenolic epoxy resin, 20-30 parts of bisphenol A epoxy resin, 10-20 parts of toughening agent and 8-15 parts of compound curing agent.
3. The low-temperature-curable epoxy resin composition according to claim 1, wherein the phenolic epoxy resin is one or more selected from the group consisting of NPPN-631 and NPPN-638S.
4. The low-temperature-curable epoxy resin composition according to claim 1, wherein the bisphenol A-type epoxy resin is one or more selected from the group consisting of NPEL-127, NPEL-128, NPES-901, NPES-902 and NPES-904.
5. A low temperature curing epoxy resin composition as claimed in claim 1, wherein said flexibilizer is in particular one or more of MX153, MX154, MX217, MX 227.
6. The preparation method of the low-temperature curing epoxy resin composition is characterized by comprising the following steps:
a) under the heating condition of 90-110 ℃, 60-80 parts of novolac epoxy resin and 20-40 parts of bisphenol A epoxy resin are uniformly mixed until completely dissolved;
b) and cooling the mixture to 50-55 ℃, adding 5-25 parts of toughening agent and 6-15 parts of compound curing agent, and uniformly mixing under a vacuum condition to obtain the epoxy resin composition.
7. A preparation method of a prepreg of a low-temperature curing epoxy resin composition is characterized by comprising the following specific steps: baking the epoxy resin composition of claim 1 to a fluid state, coating with a coating device to obtain a resin film, and heating and compounding the resin film and a fiber reinforced material sheet to obtain the prepreg.
8. The method for preparing the prepreg of the low-temperature curing epoxy resin composition according to claim 7, wherein the mass content of the fiber reinforced material sheet in the prepreg is 60-70%.
9. A method for preparing a composite material of a low-temperature curing epoxy resin composition is characterized by comprising the following steps of spreading the prepreg prepared according to the claim 7 on a mould and curing according to a curing period to obtain the composite material of the epoxy resin composition.
10. The method for preparing a composite material of a low-temperature curing epoxy resin composition according to claim 9, wherein the curing period is specifically that the curing temperature is raised from room temperature to 80 ℃ at a heating rate of 2 ℃/min, the temperature is kept for 120min, then the curing temperature is cooled to room temperature, and a pressure of 1bar to 6.5bar is added during the curing process to exhaust gas so as to reduce the formation of pores.
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Cited By (5)
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| CN111690233A (en) * | 2020-07-22 | 2020-09-22 | 黑龙江省科学院石油化学研究院 | Low-temperature curing high-toughness epoxy resin system and preparation method thereof |
| CN112574530A (en) * | 2020-12-07 | 2021-03-30 | 嘉兴聚新航空材料科技有限公司 | Design and processing technology of basalt fiber propeller |
| CN115044172A (en) * | 2022-06-09 | 2022-09-13 | 台州市黄岩区武汉理工高性能复合材料技术研究院 | Single-component epoxy resin composition for prepreg and preparation method thereof |
| CN116606529A (en) * | 2023-07-19 | 2023-08-18 | 常州天启新新科技有限公司 | Low-temperature cured epoxy resin, preparation method, prepreg, composite material and application |
| CN117384407A (en) * | 2023-10-11 | 2024-01-12 | 常州天启新新科技有限公司 | Low-density marine epoxy resin glass fiber prepreg, preparation method, glass fiber composite material and application |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111690233A (en) * | 2020-07-22 | 2020-09-22 | 黑龙江省科学院石油化学研究院 | Low-temperature curing high-toughness epoxy resin system and preparation method thereof |
| CN111690233B (en) * | 2020-07-22 | 2023-05-23 | 黑龙江省科学院石油化学研究院 | Low-temperature curing high-toughness epoxy resin system and preparation method thereof |
| CN112574530A (en) * | 2020-12-07 | 2021-03-30 | 嘉兴聚新航空材料科技有限公司 | Design and processing technology of basalt fiber propeller |
| CN115044172A (en) * | 2022-06-09 | 2022-09-13 | 台州市黄岩区武汉理工高性能复合材料技术研究院 | Single-component epoxy resin composition for prepreg and preparation method thereof |
| CN116606529A (en) * | 2023-07-19 | 2023-08-18 | 常州天启新新科技有限公司 | Low-temperature cured epoxy resin, preparation method, prepreg, composite material and application |
| CN116606529B (en) * | 2023-07-19 | 2023-09-22 | 常州天启新新科技有限公司 | Low-temperature cured epoxy resin, preparation method, prepreg, composite material and application |
| CN117384407A (en) * | 2023-10-11 | 2024-01-12 | 常州天启新新科技有限公司 | Low-density marine epoxy resin glass fiber prepreg, preparation method, glass fiber composite material and application |
| CN117384407B (en) * | 2023-10-11 | 2024-05-03 | 常州天启新新科技有限公司 | Low-density marine epoxy resin glass fiber prepreg, preparation method, glass fiber composite material and application |
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