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
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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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