A kind of preparation method and use of highly flame-retardant phosphorus-containing benzoxazine resin
A technology of benzoxazine and high flame retardancy, which is applied in the field of preparation of benzoxazine resin, can solve problems affecting product appearance, improve heat resistance and flame retardancy, and improve product purity and yield Effect
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Embodiment 1
[0030] Embodiment 1, a kind of highly flame-retardant phosphorus-containing benzoxazine resin, the chemical structural formula of its phosphorus-containing benzoxazine resin is as shown in formula I:
[0031]
[0032] in, is one of the following structures:
[0033]
[0034] The invention also discloses a preparation method of phosphorus-containing benzoxazine resin, which specifically comprises the following steps:
[0035] (1) Preparation of benzoxazine monomers, adding phosphorus-containing bisphenol intermediates, primary amines, aldehydes in a molar ratio of 1:2:4 to the organic solvent in the self-priming exhaust heat exchange reactor in turn compound, and add an amine catalyst, turn on the stirring machine for stirring and mixing, and use a gradient to heat up to 80 ° C ~ 120 ° C, react for 2-8 hours, when the system becomes transparent, pass condensed water to cool down to terminate the reaction; obtain benzene oxazine monomer mixture. Among them, the amine c...
Embodiment 2
[0042] Adopt solution method to prepare benzoxazine resin reaction equation as follows:
[0043]
[0044]The experimental steps are: at room temperature, add 0.1 mol of aniline, 30 mL of toluene and 0.2 mol of paraformaldehyde to a 100 mL three-necked round-bottomed flask equipped with a reflux condenser and a thermometer, and add 0.05 mol of phosphorus-containing bisphenol under full stirring. After the intermediate A, the temperature was raised to 80°C and the reaction was performed for 4 hours. After cooling to room temperature, the reactant was washed three times with water, and the solvent and residual moisture were removed by distillation under reduced pressure to obtain about 26.5 g of the target benzoxazine resin BZ-1 with a yield of 85%. The obtained composition is subjected to 31P NMR test, and the obtained results are as follows figure 1 shown; the DSC test results are as follows figure 2 shown; the results obtained by the TGA test are as follows image 3 sho...
Embodiment 3
[0046] Adopt solution method to prepare benzoxazine resin reaction equation as follows:
[0047]
[0048] The experimental steps are: at room temperature, add 0.1 mol of methylamine, 30 mL of dioxane and 0.2 mol of paraformaldehyde to a 100 mL three-necked round-bottomed flask equipped with a reflux condenser and a thermometer, and add 0.05 mol of paraformaldehyde under full stirring. After the phosphorus-containing bisphenol intermediate A, the temperature was raised to 60° C. to react for 8 hours. After cooling to room temperature, the reactant was washed three times with water, and the solvent and residual water were distilled off under reduced pressure to obtain about 19.4 g of the target benzoxazine resin BZ-2 with a yield of 78%.
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