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High-toughness halogen-free cyanate ester resin composite material and preparation method thereof

A resin composite material and cyanate resin technology are applied in the field of high toughness halogen-free cyanate resin composite material and its preparation, and achieve the effects of good flame retardant performance, not easy to foam, and good stability

Active Publication Date: 2020-08-14
YANGZHOU TECHIA MATERIAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, at present, the mechanical properties and processing properties of halogen-free cyanate resin composites need to be improved, and the thermal stability, high chemical stability, and flame retardancy need to be further improved.

Method used

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  • High-toughness halogen-free cyanate ester resin composite material and preparation method thereof
  • High-toughness halogen-free cyanate ester resin composite material and preparation method thereof
  • High-toughness halogen-free cyanate ester resin composite material and preparation method thereof

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Effect test

Embodiment 1

[0030] A high-toughness halogen-free cyanate resin composite material, prepared from modified cyanate resin, carbon nanotubes, and surfactants, wherein the carbon nanotubes are uniformly dispersed in the cyanate resin, wherein the modified cyanate The mass ratio of the resin in the composite material is 99.4%, and the mass ratio of the surfactant to the carbon nanotube is 0.5:1; Carbon nanotubes are mixed according to the mass ratio of 1.4:1. The surfactant is a mixture of octylphenol polyoxyethylene ether and high-carbon fatty alcohol polyoxyethylene ether in a mass ratio of 1:1.

[0031] The preparation method of modified cyanate ester resin is as follows:

[0032] S1. Add 149g (1mol) of 5-amino-m-benzaldehyde, 518.4g (2.4mol) of DOPO, 84g (2.8mol) of paraformaldehyde and 2384g of N, N-dimethylformamide in the three-necked flask, and heat up to 157 ℃, reflux and stir the reaction for 11 hours, let it stand until the solid precipitates, filter under reduced pressure, wash t...

Embodiment 2

[0039] A high-toughness halogen-free cyanate resin composite material, prepared from modified cyanate resin, carbon nanotubes, and surfactants, wherein the carbon nanotubes are uniformly dispersed in the cyanate resin, wherein the modified cyanate The mass ratio of the resin in the composite material is 99.4%, and the mass ratio of the surfactant to the carbon nanotube is 0.52:1; Carbon nanotubes are mixed according to the mass ratio of 1.5:1. The surfactant is octylphenol polyoxyethylene ether.

[0040] The preparation method of modified cyanate ester resin is as follows:

[0041] S1. Add 149g (1mol) of 5-amino-m-benzaldehyde, 496.8g (2.3mol) of DOPO, 93g (3.1mol) of paraformaldehyde and 2682g of N,N-dimethylformamide to a three-necked flask, and heat up to 158 ℃, reflux and stir the reaction for 11.5 hours, let it stand until the solid precipitates, filter under reduced pressure, wash the filter cake 3 times with ethyl acetate, concentrate under reduced pressure and recrys...

Embodiment 3

[0048] A high-toughness halogen-free cyanate resin composite material, prepared from modified cyanate resin, carbon nanotubes, and surfactants, wherein the carbon nanotubes are uniformly dispersed in the cyanate resin, wherein the modified cyanate The mass ratio of the resin in the composite material is 99.2%, and the mass ratio of the surfactant to the carbon nanotube is 0.6:1; Carbon nanotubes are mixed according to the mass ratio of 1.5:1. The surfactant is high-carbon fatty alcohol polyoxyethylene ether.

[0049] The preparation method of modified cyanate ester resin is as follows:

[0050] S1. Add 149g (1mol) of 5-amino-m-benzaldehyde, 518.4g (2.4mol) of DOPO, 81g (2.7mol) of paraformaldehyde and 2086g of N,N-dimethylformamide to a three-necked flask, and heat up to 160 ℃, reflux and stir the reaction for 12 hours, let stand until the solid precipitates, filter under reduced pressure, wash the filter cake 3 times with ethyl acetate, concentrate under reduced pressure an...

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Abstract

The invention discloses a high-toughness halogen-free cyanate ester resin composite material and a preparation method thereof. According to the composite material, after modified cyanate ester resin is mixed with carbon nanotubes, surfactants and deionized water, high-speed uniform stirring and ultrasonic dispersion are performed, during which a layer of the surfactants is combined on the surfacesof the single-walled carbon nanotubes and the multi-walled carbon nanotubes, so that the dispersion state of the carbon nanotubes is favorably maintained; the surfactants are all non-ionic type surfactants so that the composite material maintains good solubility in water or an organic solvent, has good stability, is not easily influenced by strong electrolyte inorganic salts, acids and alkalis, is not easy to foam in the curing process, improves the compatibility of the carbon nanotubes and the modified cyanate ester resin, and improves the mechanical properties and processability of the composite material; at high temperature, side phosphorus groups in the DOPO structure are dehydrated and carbonized, oxygen is isolated, and smoke and halogen hydride toxic and harmful substances cannot be generated.

Description

technical field [0001] The invention relates to the technical field of halogen-free cyanate resin, in particular to a high-toughness halogen-free cyanate resin composite material and a preparation method thereof. Background technique [0002] In order to achieve the flame retardancy of the commonly used bisphenol A cyanate resin, halogen is usually added to the resin, but the halogen-containing flame retardant materials will produce a lot of smoke and toxic corrosive hydrogen halide gas during the flame retardancy process , causing pollution and harm, and the toughness of the existing bisphenol A cyanate resin material is not enough, the toughening method is usually to add a toughening agent, carbon nanotubes are widely used in Toughening additives for cyanate resins. In the prior art, carbon nanotubes are usually directly mixed with cyanate resin. Although the toughness can be enhanced, due to the inability to polymerize between the two, the carbon nanotubes are not unifor...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08L79/04C08L71/02C08K3/04
CPCC08L79/04C08L2201/22C08L2201/02C08L71/02C08K3/041
Inventor 季静静吕嘉木张科明熊莉
Owner YANGZHOU TECHIA MATERIAL CO LTD
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