Allylation hyperbranched polyphenyl ether modified bismaleimide resin and preparation method thereof
A technology of bismaleimide and allylation, which is applied in the field of allylated hyperbranched polyphenylene ether modified bismaleimide resin and its preparation, can solve the unfavorable large-scale industrialization and product Low yield and other problems, to achieve the effect of excellent manufacturability, rich raw materials, outstanding toughness
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Embodiment 1
[0020] (1) Preparation of hyperbranched polyphenylene ether
[0021] Under a nitrogen atmosphere, 2.41g (6.82mmol) of 4-bromo-4', 4"-dihydroxytriphenylmethane, 1.08g (7.81mmol) of anhydrous K 2 CO 3 and 25.0ml of toluene were added to 98ml of dimethyl sulfoxide (DMSO) sequentially, and after heating up and reflux for 3 hours, the reaction system was cooled to 45°C, 13.5mg (0.14mmol) of catalyst CuCl was added, and the temperature was raised to 170°C and kept at a constant temperature Reaction for 40 hours. After the mixture was cooled to room temperature, it was acidified with hydrochloric acid, and after stirring for 0.5 hours, it was dropped into a mixed solution of methanol and water (volume ratio 1:8) to precipitate, filtered, and vacuum-dried at 60°C. The crude product was dissolved in a small amount of tetrahydrofuran (THF), filtered, and the filtrate was precipitated with cyclohexane, filtered again, washed with cyclohexane, and dried in vacuum at 90° C. to obtain hyp...
Embodiment 2
[0032] Preparation of Allylated Hyperbranched Polyphenylene Ether
[0033]Under an argon atmosphere, at normal temperature, the hyperbranched polyphenylene ether, 10g of potassium hydroxide, 100g of dimethylformamide (DMF) and 1g of tetrabutyl bromide prepared in the first step (1) of the 100g embodiment Ammonium was put into a three-necked flask. Raise the temperature to 70°C and stir for 1 hour. After cooling down to 40°C, start to add 10g of 3-bromopropene dropwise, and finish dropping in 0.5 hours; then raise the temperature to 60°C, heat-preserve and reflux for 3 hours, then raise the temperature to 70°C, and heat-preserve and reflux for 2 hours. After the reaction was completed, it was cooled to room temperature, stirred and dropped into a mixed solution of methanol and water (volume ratio 1:3), and filtered. After the filter cake was vacuum dried at 50°C, it was dissolved in tetrahydrofuran, dropped into cyclohexane while stirring, filtered, and the filter cake was va...
Embodiment 3
[0037] Preparation of Allylated Hyperbranched Polyphenylene Ether
[0038] Under a nitrogen atmosphere, at normal temperature, the hyperbranched polyphenylene ether, 1.5g sodium hydroxide, 150g dimethylacetamide (DMAc) and 2g benzyltriethyl chloride prepared in step (1) of 100g embodiment Ammonium chloride was put into a three-necked flask. Raise the temperature to 60°C and stir for 0.5 hours. After cooling down to 50° C., 20 g of 3-chloropropene was added dropwise, and the dropwise was completed within 2.5 hours. Then the temperature was raised to 60° C., kept at reflux for 2 hours, then raised to 80° C., kept at reflux for 2 hours. After the reaction was completed, it was cooled to room temperature, stirred and dropped into a mixed solution of methanol and water (volume ratio 1:2), and filtered. After the filter cake was vacuum dried at 60°C, it was dissolved in tetrahydrofuran, dropped into cyclohexane while stirring, filtered, and the filter cake was vacuum dried at 80°...
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