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Ultrahigh-frequency and low-dielectric carboxylated graphene reinforced poly(benzoxazine-urethane) nanocomposite resin and preparation method thereof

A technology of carboxylated graphene and benzoxazine, which is applied in the field of carboxylated graphene-reinforced poly-nanocomposite resin and its preparation, can solve the problem that the dielectric properties cannot meet ultra-high frequency, the resin-matrix interaction is weak, and the dispersion of inorganic particles Poor compatibility and other problems, to achieve the effect of improving processing technology, enhancing compatibility, and good moisture resistance

Active Publication Date: 2020-03-17
淮北绿洲新材料有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] However, there are still problems such as poor dispersion of inorganic particles, weak interaction with the resin matrix, and poor compatibility in the research of micro-nano material-reinforced benzoxazine resins, especially the dielectric properties of benzoxazine nanocomposite resins still cannot meet the requirements of ultra-high Frequency (3-30GHz) requirements (k<3.0, f<0.005), still can not meet the needs of high-frequency and high-speed development of electronic information

Method used

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  • Ultrahigh-frequency and low-dielectric carboxylated graphene reinforced poly(benzoxazine-urethane) nanocomposite resin and preparation method thereof
  • Ultrahigh-frequency and low-dielectric carboxylated graphene reinforced poly(benzoxazine-urethane) nanocomposite resin and preparation method thereof
  • Ultrahigh-frequency and low-dielectric carboxylated graphene reinforced poly(benzoxazine-urethane) nanocomposite resin and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0096] Preparation of epoxy type bisphenol:

[0097] Under the protection of nitrogen, according to the solvent-free method, the molar ratio of bisphenol A novolac epoxy resin to dihydric phenol is 1:5 and added to the four-necked flask, followed by the addition of tetrabutyl bromide with a mass fraction of 1% of the reaction material. Ammonium was used as a catalyst, vigorously stirred at 180°C for 4 hours, and then dried in a vacuum oven. After grinding, a brown powder was obtained, which was epoxy bisphenol. Wherein, the epoxy equivalent of the bisphenol A novolac epoxy resin is 50, and the molecular weight is 1000. The structural formula of dihydric phenol is as follows:

[0098] The infrared spectrum of epoxy type bisphenol is as follows figure 1 shown, of which 3410cm -1 Corresponding to the characteristic absorption peak of the stretching vibration of the hydroxyl group;

[0099]

[0100] Hydroxyl ether bond [-O-CH 2 -CH(OH)-CH 2 -] The stretching vibration cha...

Embodiment 2

[0102] Preparation of epoxy type bisphenol:

[0103] Under the protection of nitrogen, according to the solvent-free method, the molar ratio of bisphenol S epoxy resin and dihydric phenol is 5:1 and is added in the four-necked flask, and then the tetrabutylammonium bromide whose mass fraction is 0.1% of the reaction mass is added As a catalyst, stir vigorously at 120°C for 24 hours, then dry in a vacuum oven, and grind to obtain a light yellow powder, which is epoxy bisphenol. Wherein, the epoxy equivalent of bisphenol S epoxy resin is 500, and the molecular weight is 10000. The structural formula of dihydric phenol is as follows:

Embodiment 3

[0105]

[0106] Preparation of epoxy type main chain benzoxazine resin:

[0107] Under nitrogen protection, in mole % ratio, the epoxy type bisphenol, 1,3-diamino-2-propanol and paraformaldehyde prepared in Example 1 are in a molar ratio of 1:1:4, at 80°C as a toluene solvent React for 48 hours to obtain epoxy-type main chain benzoxazine prepolymer solution, let it stand overnight, filter after recrystallization, dry in a blast oven, and grind the product to obtain a yellow powder, which is epoxy bisphenol-1,3- Diamino-2-propanol type main chain benzoxazine prepolymer.

[0108] Dissolve the epoxy bisphenol-1,3-diamino-2-propanol type main chain benzoxazine prepolymer prepared above in the solvent, vacuumize and degas for 4 hours to remove air bubbles, and then cure the reaction at 200°C After 4h, the main chain type benzoxazine resin was obtained.

[0109] figure 2 (Left one) is the photo of the obtained resin sample after curing in this embodiment, as can be seen from ...

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Abstract

The invention relates to an ultrahigh-frequency and low-dielectric carboxylated graphene reinforced poly(benzoxazine-urethane) nanocomposite resin and a preparation method thereof. The introduction ofcarboxylated graphene effectively reduces the curing temperature of a matrix resin, and the mechanical properties and the thermal properties of the resin are effectively improved through the chemicalbonding effect between nano-particles and the matrix resin. The nanocomposite resin particularly has low dielectric constant and dielectric loss at an ultrahigh frequency, and can be used in the fields of high-frequency and high-speed circuit board substrates, microwave and millimeter wave communication, vehicle-mounted radar and other composite materials.

Description

technical field [0001] The invention relates to the technical field of polymer materials, in particular to a class of carboxylated graphene-reinforced poly(benzoxazine-urethane) nanocomposite resins and a preparation method thereof. Background technique [0002] As a new type of thermosetting phenolic resin, benzoxazine resin has attracted much attention due to its excellent performance. Among them, the main chain type benzoxazine resin not only has the advantages of low moisture absorption, excellent dielectric properties, and good heat resistance, but also overcomes the brittleness and low crosslinking density of traditional benzoxazine resins. The shortcomings of both thermosetting resins and thermoplastic resins, these are the main chain type benzoxazine resin to become the basic material of electronic communication - the matrix resin of the copper clad laminate provides the conditions. However, there are still some problems in the application of the main chain type ben...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G18/54C08G14/073C08G14/12C08L75/04C08L61/34C08K9/04C08K3/04
CPCC08G18/54C08G14/06C08G14/12C08K9/04C08K3/042C08L2201/08C08L75/04C08L61/34
Inventor 曾鸣殷蝶陈江炳
Owner 淮北绿洲新材料有限责任公司