CN114031746A - High-temperature-resistant tough resin - Google Patents
High-temperature-resistant tough resin Download PDFInfo
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- CN114031746A CN114031746A CN202111464617.5A CN202111464617A CN114031746A CN 114031746 A CN114031746 A CN 114031746A CN 202111464617 A CN202111464617 A CN 202111464617A CN 114031746 A CN114031746 A CN 114031746A
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- curing agent
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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
- C08G59/20—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 epoxy compounds used
- C08G59/32—Epoxy compounds containing three or more epoxy groups
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- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Epoxy Resins (AREA)
- Reinforced Plastic Materials (AREA)
Abstract
The invention discloses a high-temperature-resistant tough resin which is prepared from the following raw materials in parts by weight: 100 parts of epoxy resin, 10-20 parts of diluent and 15-25 parts of curing agent; the epoxy resin is a mixture of 1, 2-epoxy cyclohexane 4, 5-dicarboxylic acid diglycidyl ester (TDE-85) and p-aminophenol epoxy resin (AFG-90), and the epoxy resin are mixed according to a mass ratio of 1-5: 1; the diluent is a 6360 toughening diluent; the curing agent is an amine curing agent, wherein the amine curing agent is diethyl toluene diamine (DETDA) and DDM (diaminodiphenylmethane), and the amine curing agent is mixed according to the mass ratio of 1-5: 1. The high-temperature-resistant tough resin has good high-temperature resistance, good toughness and process performance, the glass transition temperature reaches 170-185 ℃, the fracture elongation is more than 4.0%, and the high-temperature-resistant tough resin is suitable for a carbon fiber wet winding process.
Description
Technical Field
The invention belongs to the technical field of epoxy resin materials, and relates to a high-temperature-resistant tough resin.
Background
The solid rocket engine shell is a part of the whole structure of the missile, has higher requirements on the performance of shell materials, the resin matrix has to resist the high temperature of more than 170 ℃, and has certain toughness so as to give full play to the characteristics of high strength and high modulus of carbon fibers, improve the strength conversion rate of the fibers, meet the wet winding process requirements of low viscosity, long trial period at room temperature and the like, and ensure that the strength and the rigidity of the engine shell meet the design requirements in the working process.
The temperature resistance of the existing single-component epoxy resin used for the shell of the wet-process winding solid rocket engine is mostly below 130 ℃, and the requirements of the shell of the wet-process winding solid rocket engine on the comprehensive properties such as good process performance, high temperature resistance, high toughness and the like are difficult to meet simultaneously, so the invention provides a formula of the double-component high-temperature-resistant tough epoxy resin.
Disclosure of Invention
Technical problem to be solved
The invention aims to solve the technical problem of providing a high-temperature-resistant tough resin aiming at the problems of the matrix resin of the solid rocket engine shell. The resin has good high temperature resistance, high toughness and high technological performance, and can be used for manufacturing rocket engine shells, high temperature resistant pressure vessels, pipelines and other products.
(II) technical scheme
In order to solve the technical problems, the invention provides a high-temperature-resistant tough resin which is prepared from the following raw materials in parts by weight: 100 parts of epoxy resin, 10-20 parts of diluent and 15-25 parts of curing agent; the epoxy resin is a mixture of TDE-85 and AFG-90, and is mixed according to a mass ratio of 1-5: 1; the diluent is a 6360 toughening diluent; the curing agent is an amine curing agent, wherein the amine curing agent is a curing agent formed by mixing DETDA and DDM according to a mass ratio of 1-5: 1; the glass transition temperature of the high-temperature resistant and tough resin reaches 170-185 ℃, the elongation at break is more than 4.0%, and the resin has good matching property and processing performance with carbon fiber materials.
The high-temperature-resistant tough resin is prepared from the following raw materials, by weight, 100 parts of epoxy resin, 10-20 parts of a diluent and 15-25 parts of a curing agent.
In the high-temperature resistant tough resin, the trifunctional resin is TDE-85 epoxy resin and AFG-90 epoxy resin.
In the high-temperature resistant tough resin, the curing agent is DETDA curing agent and DDM curing agent.
The preparation method of the high temperature resistant tough resin comprises the following steps: stirring DETDA and DDM curing agent at 60 deg.C for 35min to completely dissolve and mix DDM to obtain component A; uniformly mixing the epoxy resin and the diluent at room temperature (25 ℃) to obtain a component B; and then uniformly mixing the component A and the component B at room temperature to obtain the high-temperature-resistant tough resin.
(III) advantageous effects
Compared with the prior art, the high-temperature resistant tough resin provided by the technical scheme has the following advantages:
1. the high-temperature-resistant tough resin has good high-temperature resistance, higher toughness and processing performance, is suitable for a fiber winding process, and has high bonding strength with a carbon fiber interface and high fiber strength conversion rate.
2. The high temperature resistant tough resin can be used for producing products such as engine housings, high temperature resistant pressure vessels, pipelines and the like, and the products prepared by the high temperature resistant tough resin have the characteristics of high rigidity, good impact resistance, high temperature resistance and the like.
Detailed Description
In order to make the objects, contents and advantages of the present invention clearer, the following detailed description of the embodiments of the present invention will be given in conjunction with examples.
Example 1
The high-temperature resistant tough resin of the embodiment is prepared from the following raw materials: 1kg of TDE-85 epoxy resin, 1kg of AFG-90 epoxy resin, 0.2kg of 6360 diluent, 0.15kg of DETDDA and 0.15kg of curing agent.
The preparation method of the high temperature resistant tough resin of the embodiment is that DETDA and DDM curing agent are stirred for 35min at 60 ℃, so that DDM is completely dissolved and uniformly mixed to obtain component A; mixing TDE epoxy resin, AFG90 epoxy resin and 6360 diluent at room temperature (25 ℃) to obtain a component B; and then uniformly mixing the component A and the component B at room temperature to obtain the high-temperature-resistant tough resin.
Example 2
The high-temperature resistant tough resin of the embodiment is prepared from the following raw materials: 3kg of TDE-85 epoxy resin, 1kg of AFG-90 epoxy resin, 0.4kg of 6360 diluent, 0.45kg of DETDDA and 0.35kg of curing agent.
The preparation method of the high temperature resistant tough resin of the embodiment is that DETDA and DDM curing agent are stirred for 35min at 60 ℃, so that DDM is completely dissolved and uniformly mixed to obtain component A; mixing TDE-85 epoxy resin, AFG-90 epoxy resin and 6360 diluent at room temperature (25 ℃) to obtain a component B; and then uniformly mixing the component A and the component B at room temperature to obtain the high-temperature-resistant tough resin.
Example 3
The high-temperature resistant tough resin of the embodiment is prepared from the following raw materials: 5kg of TDE-85 epoxy resin, 1kg of AFG-90 epoxy resin, 0.6kg of 6360 diluent, 0.9kg of DETDDA and 0.3kg of curing agent.
The preparation method of the high temperature resistant tough resin of the embodiment is that DETDA and DDM curing agent are stirred for 35min at 60 ℃, so that DDM is completely dissolved and uniformly mixed to obtain component A; stirring and mixing the TDE-85 epoxy resin, the AFG-90 epoxy resin and the 6360 toughening diluent uniformly at room temperature (25 ℃) to obtain a component B; and then uniformly mixing the component A and the component B at room temperature to obtain the high-temperature-resistant tough resin.
Comparative example 4
The resin of this comparative example was made from the following raw materials: 3kg of TDE-85 epoxy resin, 1kg of AFG-90 epoxy resin and 2.2kg of 70# anhydride curing agent.
The preparation method of the high temperature resistant and tough resin of the embodiment is to mix the TDE-85 epoxy resin, the AFG-90 epoxy resin, and the 70# curing agent uniformly at room temperature to obtain the resin.
The high-temperature resistant toughness resin and the comparative resin are prepared into samples, the curing temperature parameter is 80 ℃/2h +120 ℃/3h +160 ℃/8h, then the tensile property of the resin casting is tested according to GB/T2570-2008, the glass transition temperature of the resin casting is tested by a DSC method, and the resin viscosity is tested by a DNJ-7 type rotational viscometer in the trial preparation process.
TABLE 1 Performance parameters of the high temperature toughness resistant resin samples of examples 1-3 and comparative example 4.
The high-temperature resistant tough resin can be used for manufacturing a solid rocket combustion chamber engine shell, and the specific method comprises the following steps: winding high-temperature-resistant tough resin (the carbon fiber content is 70% -75%) reinforced by T800 carbon fibers on the surface of a core mold, wherein the winding thickness is 4-5 mm, and the curing system is as follows: 80 ℃/2h +120 ℃/3h +160 ℃/8h to obtain the engine shell, wherein the prepared shell has the high temperature of more than 175 ℃, the explosion pressure is more than 20MPa, the axial bearing load is more than 700KN, and the use requirement of the engine shell is met.
The above description is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, several modifications and variations can be made without departing from the technical principle of the present invention, and these modifications and variations should also be regarded as the protection scope of the present invention.
Claims (10)
1. The high-temperature-resistant tough resin is characterized by being prepared from the following raw materials in parts by weight: 100 parts of epoxy resin, 10-20 parts of diluent and 15-25 parts of curing agent; the epoxy resin is a mixture of TDE-85 and AFG-90, and the curing agent is an amine curing agent.
2. The high-temperature-resistant tough resin according to claim 1, wherein the TDE-85 epoxy resin and the AFG-90 epoxy resin are mixed in a mass ratio of 1-5: 1.
3. The high temperature resistant tough resin according to claim 2, wherein the diluent is a 6360 toughening diluent.
4. The resin with high temperature toughness of claim 3, wherein the amine curing agent is a mixture of DETDA and DDM.
5. The high-temperature-resistant tough resin according to claim 4, wherein DETDA and DDM are mixed in a mass ratio of 1-5: 1.
6. The high temperature resistant tough resin according to claim 5, which comprises 1kg of TDE-85 epoxy resin, 1kg of AFG-90 epoxy resin, 0.2kg of 6360 diluent, 0.15kg of DETDDA and 0.15kg of curing agent.
7. The high temperature resistant tough resin according to claim 5, which comprises 3kg of TDE-85 epoxy resin, 1kg of AFG-90 epoxy resin, 0.4kg of 6360 diluent, 0.45kg of DETDDA and 0.35kg of curing agent.
8. The high temperature resistant tough resin according to claim 5, which comprises 5kg of TDE-85 epoxy resin, 1kg of AFG-90 epoxy resin, 0.6kg of 6360 diluent, 0.9kg of DETDDA and 0.3kg of curing agent.
9. The preparation method of the high-temperature-resistant tough resin is characterized by comprising the following steps: firstly, dissolving an amine curing agent to obtain a component A; then mixing the TDE-85 and AFG-90 three-functional epoxy resin with a diluent to obtain a component B; and then uniformly mixing the component A and the component B at room temperature to obtain the high-temperature-resistant tough resin.
10. The method for preparing high temperature resistant tough resin according to claim 9, wherein the amine curing agent is DETDA and DDM curing agent, and stirring is performed at 60 ℃ for 35min to completely dissolve and uniformly mix DDM; the two trifunctional epoxy resins are mixed with a diluent at room temperature of 25 ℃.
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| CN202111464617.5A CN114031746A (en) | 2021-12-03 | 2021-12-03 | High-temperature-resistant tough resin |
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| CN202111464617.5A CN114031746A (en) | 2021-12-03 | 2021-12-03 | High-temperature-resistant tough resin |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116162225A (en) * | 2023-01-09 | 2023-05-26 | 华东理工大学 | Epoxy resin material and preparation method and application thereof |
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| US4255302A (en) * | 1979-11-15 | 1981-03-10 | The United States Of America As Represented By The Secretary Of The Navy | Resin system for filament winding of pressure vessels |
| CN101948611A (en) * | 2010-09-30 | 2011-01-19 | 蓝星(北京)化工机械有限公司 | Winding epoxy resin composition, preparation method thereof and use thereof |
| CN105131255A (en) * | 2015-09-30 | 2015-12-09 | 西安超码复合材料有限公司 | High-temperature-resistant resin |
| CN108048009A (en) * | 2017-12-11 | 2018-05-18 | 王建东 | A kind of bi-component epoxide-resin steel bonding glue |
| CN109852004A (en) * | 2019-01-04 | 2019-06-07 | 恩莱登（北京）工业技术有限公司 | Epoxy resin-base composition, epoxy resin-base and preparation method thereof |
| CN110283300A (en) * | 2019-07-15 | 2019-09-27 | 上海华谊树脂有限公司 | One kind being suitable for molding epoxy composite of composite liquid and preparation method thereof |
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2021
- 2021-12-03 CN CN202111464617.5A patent/CN114031746A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4255302A (en) * | 1979-11-15 | 1981-03-10 | The United States Of America As Represented By The Secretary Of The Navy | Resin system for filament winding of pressure vessels |
| CN101948611A (en) * | 2010-09-30 | 2011-01-19 | 蓝星(北京)化工机械有限公司 | Winding epoxy resin composition, preparation method thereof and use thereof |
| CN105131255A (en) * | 2015-09-30 | 2015-12-09 | 西安超码复合材料有限公司 | High-temperature-resistant resin |
| CN108048009A (en) * | 2017-12-11 | 2018-05-18 | 王建东 | A kind of bi-component epoxide-resin steel bonding glue |
| CN109852004A (en) * | 2019-01-04 | 2019-06-07 | 恩莱登（北京）工业技术有限公司 | Epoxy resin-base composition, epoxy resin-base and preparation method thereof |
| CN110283300A (en) * | 2019-07-15 | 2019-09-27 | 上海华谊树脂有限公司 | One kind being suitable for molding epoxy composite of composite liquid and preparation method thereof |
Non-Patent Citations (2)
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| 舒碧光等: "碳纤维复合壳体用基体环氧树脂研究进展", 宇航材料工艺, no. 3, pages 611 - 612 * |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116162225A (en) * | 2023-01-09 | 2023-05-26 | 华东理工大学 | Epoxy resin material and preparation method and application thereof |
| CN116162225B (en) * | 2023-01-09 | 2024-04-02 | 华东理工大学 | Epoxy resin material and preparation method and application thereof |
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