Preparation of a phosphorus-containing bismaleimide and its application in flame-retardant epoxy resin
A technology of bismaleimide and maleimide, which is applied in the preparation of phosphorus-containing bismaleimide and the application field of flame-retardant epoxy resin, can solve the problem of epoxy resin flame-retardant performance, mechanical Performance and heat resistance are difficult to balance and other problems, to achieve significant flame retardant effect, improved flame retardant performance, improved thermal performance and mechanical properties
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Embodiment 1
[0028] The preparation method of described phosphorus-containing bismaleimide:
[0029] (1) In a 250mL reaction vessel equipped with stirring, add 7.65g of N-(4-hydroxyphenyl)maleimide and 50mL of tetrahydrofuran under ice-cooling, and dissolve them by magnetic stirring; after completely dissolving, add triethyl Amine 5.3g, continue stirring until uniformly mixed. Then, at 5-7° C., 4.5 g of a mixed solution of phenyl dichlorophosphate and tetrahydrofuran was added dropwise into the above-mentioned reaction vessel, and the system gradually produced white precipitates.
[0030] (2) After the solution was added dropwise, the system was reacted at room temperature for 10 h, the white precipitate triethylamine hydrochloride was filtered and then distilled under reduced pressure, purified and dried with ethyl acetate and petroleum ether to obtain a light yellow solid product, the yield was was 91.7%.
Embodiment 2
[0032] The preparation method of described phosphorus-containing bismaleimide:
[0033] (1) In a 250mL reaction vessel equipped with stirring, add 7.65g of N-(4-hydroxyphenyl)maleimide and 50mL of tetrahydrofuran under ice-cooling, and dissolve them by magnetic stirring; after completely dissolving, add triethyl Amine 4.89g, continue stirring until uniformly mixed. Then, at 5-7° C., 4.5 g of a mixed solution of phenyl dichlorophosphate and tetrahydrofuran was added dropwise into the above-mentioned reaction vessel, and the system gradually produced white precipitates.
[0034] (2) After the solution was added dropwise, the system was reacted at room temperature for 12 hours, the white precipitate triethylamine hydrochloride was filtered and then distilled under reduced pressure, purified and dried with ethyl acetate and petroleum ether to obtain a light yellow solid product, the yield was 92.5%.
Embodiment 3
[0041] The preparation method of described phosphorus-containing bismaleimide:
[0042] (1) In a 250mL reaction vessel equipped with stirring, add 7.65g of N-(4-hydroxyphenyl)maleimide and 50mL of tetrahydrofuran under ice-cooling, and dissolve them by magnetic stirring; after completely dissolving, add triethyl Amine 5.35g, continue to stir until evenly mixed. Then, at 5-7° C., 4.5 g of a mixed solution of phenyl dichlorophosphate and tetrahydrofuran was added dropwise into the above-mentioned reaction vessel, and the system gradually produced white precipitates.
[0043] (2) After the solution was added dropwise, the system was reacted at room temperature for 8 hours, the white precipitate triethylamine hydrochloride was filtered and then distilled under reduced pressure, purified and dried with ethyl acetate and petroleum ether to obtain a light yellow solid product, the yield was 95.3%.
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