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Preparation method of transparent self-toughening dicyandiamide/epoxy resin-based composite material

An epoxy resin matrix and epoxy resin technology, which is applied in the field of preparation of transparent self-toughening dicyandiamide/epoxy resin based composite materials, can solve the problem of high brittleness, large heat release, opacity, etc. of the cured product of resin and curing agent. problem, to achieve the effect of transparency, low reaction heat, and good toughness of the cured product

Inactive Publication Date: 2017-09-08
AVIC BASIC TECH RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Purpose of the present invention: the present invention provides an epoxy / dicyandiamide curing epoxy system for the problems of large heat release, heat concentration, phase separation of resin and curing agent, and high brittleness and opacity of the cured product. Amine resin composition and preparation method thereof,

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Put 100 parts by mass of bisphenol A liquid epoxy resin DER331, 6 parts by mass of dicyandiamide, and 2 parts by mass of 4,4-bis(N,N-dimethyl)urea diphenylmethane in 100 Dry at ℃ for 3h to remove the moisture and volatiles; add epoxy resin, curing agent, and accelerator to absolute ethanol to dissolve under stirring conditions, heat to 65℃, react for 3h, use rotary evaporation to reduce pressure Under the conditions, the solvent was removed at (50±10)°C to obtain a transparent self-toughened dicyandiamide / epoxy resin system 1.

[0037] The reaction heat and peak heat flow of system 1 were measured by DSC. The heating rate was 10°C / min. The test temperature was from room temperature to 250°C. The reaction heat of system 1 was measured to be 245J / g and the peak heat flow was 1.8W / g, respectively. Universal urea-catalyzed dicyandiamide cures 62% and 53% of the epoxy system, with low reaction heat. Pour the prepared system 1 into a resin casting mold, remove air bubbles under...

Embodiment 2

[0040] 80 parts by mass of bisphenol A liquid epoxy resin DER331, 20 parts by mass of bisphenol A solid epoxy resin DER662, 4 parts by mass of curing agent dicyandiamide, 3 parts by mass of accelerator 4 ,4-Di(N,N-dimethyl)urea diphenylmethane was dried at 102℃ for 4h to remove the moisture and volatiles; under stirring conditions, add epoxy resin, curing agent and accelerator to the solvent Dissolve in medium, heat to 65°C, react for 2.5h, and use rotary evaporation to remove ethylene glycol methyl ether at 50-80°C under reduced pressure to obtain a transparent self-toughening dicyandiamide / epoxy resin system 2.

[0041] The reaction heat and peak heat flow of system 2 were measured by DSC. The heating rate was 10°C / min. The test temperature was from room temperature to 250°C. The measured reaction heat of system 2 was 194J / g and the peak heat flow was 1.4W / g, respectively. General-purpose urea-catalyzed dicyandiamide cures 49% and 41% of the epoxy system, with low reaction heat...

Embodiment 3

[0044] 40 parts by mass of bisphenol A liquid epoxy resin DER331, 40 parts by mass of glycidylamine liquid epoxy resin AG80, 20 parts by mass of bisphenol A solid epoxy resin CYD017, 5 parts by mass The curing agent dicyandiamide, 1 part by mass of the accelerator 3-(4-chlorophenyl)-1,1-dimethylurea were dried at 90°C for 4h to remove the moisture and volatiles. Under stirring conditions, add epoxy resin, curing agent and accelerator to the solvent to dissolve, heat to 70℃, react for 3h, use rotary evaporation to remove dimethyl sulfoxide at 60~90℃ under reduced pressure , A transparent self-toughening dicyandiamide / epoxy resin system 3 is obtained.

[0045] The reaction heat and peak heat flow of system 3 were measured by DSC, the heating rate was 10°C / min, the test temperature was from room temperature to 250°C, the reaction heat of system 3 was measured to be 217J / g, and the peak heat flow was 1.6W / g, respectively General-purpose urea-catalyzed dicyandiamide cures 55% and 47%...

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Abstract

The invention belongs to the technical field of application of high performance epoxy resin and particularly relates to a preparation method of a transparent self-toughening dicyandiamide / epoxy resin-based composite material, in particular to a preparation method of a transparent self-toughening epoxy resin composition with low heat release, a heavy-thickness prepreg unidirectional tape and a composite material. The composition comprises the following raw materials in parts by weight: 60-100 parts of liquid epoxy resin, 0-40 parts of solid epoxy resin, 1.0-12 parts of a dicyandiamide curing agent and 0.5-6 parts of an accelerant. The epoxy resin is prepared by adopting a solution reaction manner; compared with a general dicyandiamide / epoxy resin system, a system in the invention has the advantages that the peak heat flux is decreased by 48% or higher, the heat release is decreased by 38% or higher, and the reaction heat is low; moreover, a resin casting body has 3.5% or more of breaking elongation, 80MPa or higher of tensile strength and 24kJ / m<2> of higher impact strength and has good toughness without adding a toughening agent; 130-DEG C medium temperature curing can be realized, and a cured product is transparent.

Description

Technical field [0001] The invention belongs to the technical field of high-performance epoxy resin application, and specifically relates to a preparation method of a transparent self-toughening dicyandiamide / epoxy resin based composite material. Specifically, it relates to a preparation method of a transparent epoxy resin composition with low exotherm, self-toughening, and a large-thickness prepreg unidirectional tape and composite material. Background technique [0002] Epoxy resin is a kind of thermosetting resin with good mechanical properties, electrical properties, corrosion resistance and manufacturability. It is widely used in various fields such as coatings, electrical insulating materials, adhesives and composite materials. Epoxy resins are epoxy oligomers containing more than two epoxy groups in one molecule, which react with a curing agent to form a three-dimensional crosslinked network of thermosetting materials. There are many types of curing agents for epoxy resin...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08L63/00C08G59/50C08J5/24C08K7/14C08K7/06C08K3/04
CPCC08G59/5006C08J5/24C08J2363/00C08K7/14C08L63/00C08L2201/10C08L2205/025C08K7/06C08K3/04
Inventor 李亚锋洪旭辉
Owner AVIC BASIC TECH RES INST
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