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High-temperature resistant and high-toughness epoxy matrix resin as well as preparation method and application thereof

A technology of epoxy matrix and epoxy resin, which is applied in the field of epoxy matrix resin with high heat resistance and high toughness and its preparation and application, and can solve the problem of poor process performance of matrix resin, poor modification effect, heat resistance of resin system Reduced performance and other issues, to achieve the effect of excellent comprehensive performance

Inactive Publication Date: 2009-12-09
INST OF CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among these modification methods, a single modification method often has certain limitations. For example, when rubber elastomer modifies epoxy resin, it can effectively improve the toughness of the epoxy resin system, but it will reduce the heat resistance and rigidity of the system.
In the research of Lu Jiankun and Yi Xiaosu (Chinese patent CN1376737), it is pointed out that rubber / clay composite toughening epoxy resin is used, the addition of rubber improves the toughness of epoxy resin, and clay makes up for the rigidity drop caused by rubber modification, but Decreased heat resistance of resin systems
Hyperbranched polymer modified epoxy resin is a newly developed modification method, which is characterized in that it can improve the toughness of epoxy resin without affecting its viscosity, modulus and heat resistance, but hyperbranched polymer The modification effect of the epoxy resin system with high crosslink density is not good, and this problem was pointed out in the research of Russell J Varley (Polymer International, 2004, 53:78)
When thermoplastic resin modifies epoxy resin, the addition of thermoplastic resin has a great influence on the viscosity of the resin system, which makes the process performance of the matrix resin worse

Method used

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  • High-temperature resistant and high-toughness epoxy matrix resin as well as preparation method and application thereof
  • High-temperature resistant and high-toughness epoxy matrix resin as well as preparation method and application thereof
  • High-temperature resistant and high-toughness epoxy matrix resin as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0052] With 80g TGDDM (compound shown in formula (I), wherein R 1 for H, R 2 Mix H), 20g 1,2-epoxycyclohexane 4,5-diglycidyl dicarboxylate and 15g thermoplastic resin PSF (polymer shown in formula (V), n=1), heat to 150°C and stir To form transparent solution, be cooled to 100 ℃ then, then add 15g DDS (compound shown in formula (II) in described transparent solution, wherein R 1 for H, R 2 for H, R 3 for SO 2 ), 25g 1,4,4-6FAPB (compound shown in formula (III), wherein R 1 for CF 3 , R 2 for ) and 0.5g boron trifluoride-monoethylamine, mixed evenly and then poured and solidified. The curing program was 1 hour at 130°C, 2 hours at 180°C, and 2 hours at 200°C to obtain a cured epoxy matrix resin. DMA method (dynamic thermomechanical analysis) to measure glass transition temperature, using three-point bending loading mode, spline size (18±0.5mm)×(5±0.2mm)×(1.5±0.2mm), frequency 1Hz, heating rate 5 °C / min, the measured glass transition temperature of the epoxy matrix re...

Embodiment 2

[0054] With 70g TGDDM (compound shown in formula (I), wherein R 1 for H, R 2 For H), 30g p-aminophenol epoxy resin and 20g thermoplastic resin PEI (polymer shown in formula (VII), n=10) are mixed, heated to 160 ℃ and stirred to form transparent solution, then cooled to 80 ℃, then Add 20gTMDDM (compound shown in formula (I) in described transparent solution, wherein R 1 for CH 3 , R 2 for CH 3 , R 3 for CH 2 ), 15g DDS (compound shown in formula (II), wherein R 1 for H, R 2 for H, R 3 for SO 2 ) and 1.5g boron trifluoride-monoethylamine, mixed evenly and poured and solidified. The curing program is 130° C. for 2 hours, 170° C. for 3 hours, and 200° C. for 2 hours to obtain a cured epoxy matrix resin. DMA method (dynamic thermomechanical analysis) to measure glass transition temperature, using three-point bending loading mode, spline size (18±0.5mm)×(5±0.2mm)×(1.5±0.2mm), frequency 1Hz, heating rate 5 °C / min, the measured glass transition temperature of the epoxy mat...

Embodiment 3

[0056] With 95g DCTGDDM (compound shown in formula (I), wherein R 1 for Cl, R 2 For H), 5g of bisphenol A epoxy resin and 25g of thermoplastic resin PEK (polymer shown in formula (IV), n=60) are mixed, heated to 110 ° C and stirred until a transparent solution is formed, then cooled to 60 ° C, added 25gDDM (the compound shown in formula (II), wherein R 1 for H, R 2 for H, R 3 for CH 2 ), 20g 1,4,4-APB (compound shown in formula (III), wherein R 1 for H, R 2 for ) and 1.5g ethanedithiol, mixed uniformly and then poured and solidified. The curing program is 130° C. for 2 hours, 150° C. for 4 hours, and 180° C. for 4 hours to obtain a cured epoxy matrix resin. DMA method (dynamic thermomechanical analysis) to measure glass transition temperature, using three-point bending loading mode, spline size (18±0.5mm)×(5±0.2mm)×(1.5±0.2mm), frequency 1Hz, heating rate 5 °C / min, the measured glass transition temperature of the epoxy matrix resin is 210 °C, according to the nationa...

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Abstract

The invention discloses high-temperature resistant and high-toughness epoxy matrix resin as well as a preparation method and an application thereof. The epoxy matrix resin is prepared from the following components by weight portion: 100 portions of epoxy resin, 20-60 portions of curing agent, 0.5-5.0 portions of curing accelerator and 5-50 portions of thermoplastic resin. The epoxy matrix resin has the glass-transition temperature of 210-235 DEG C, the tensile strength of 80-86MPa, the elongation at break of 3.0-3.3% and the tensile elastic module of 3.2-3.5GPa. The epoxy matrix resin can meet the requirement of carbon fiber solvent for preimpregnation process and hot-melt preimpregnation process, and after being cured by a proper process, the epoxy matrix resin has excellent comprehensive performance and particularly high-temperature resistance and high toughness, thereby being used for preparing high-performance composite material used in the aerospace field and meeting the requirement of the high technology field represented by the aerospace field.

Description

technical field [0001] The invention relates to an epoxy matrix resin with high heat resistance and high toughness, a preparation method and application thereof. Background technique [0002] Epoxy resin has the advantages of good heat resistance, mechanical properties and manufacturability, and has been widely used in many fields. It is currently one of the most commonly used matrix resins for carbon fiber composite materials. Carbon / epoxy composites have the unique advantages of high specific strength and specific modulus, good designability, good fatigue resistance, good structural dimensional stability, and easy large-area integral molding, and have been widely used in the aerospace field. However, the epoxy resin has the disadvantage of insufficient toughness after curing, and cannot effectively exert the performance of carbon fiber. When the carbon fiber composite material is under load, the composite material is often destroyed due to the premature failure of the epox...

Claims

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Application Information

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IPC IPC(8): C08L63/00C08K5/41C08K5/18C08K5/42C08K5/13C08K5/17C08K5/37C08K13/04C08K7/06
Inventor 杨士勇陈伟明陶志强
Owner INST OF CHEM CHINESE ACAD OF SCI
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