A kind of flame-retardant bismaleimide resin and preparation method thereof
A bismaleimide and resin technology is applied in the fields of biomass-based phosphate ester flame retardant modified bismaleimide resin, flame retardant bismaleimide resin and preparation thereof, and can solve the problem of High volatility, no technical solutions reported in literature, unsatisfactory compatibility, etc., to achieve excellent flame retardant performance, easy industrial production, and low cost.
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Embodiment 1
[0029] 1) Preparation of biomass-based phosphate
[0030] See attached figure 1 , It is the synthesis reaction formula of the biomass-based phosphate ester of the present invention, the reaction is a phosphorylation reaction; in this example, the specific method is: 36.0g sodium hydroxide and 10mL water at 1±0.5℃ Mix to obtain paste A. Under stirring conditions, add dropwise a solution of eugenol (147.8 g) in dichloromethane (300 mL) to paste A to prepare sodium eugenol suspension B. Then, at 0°C, a solution of phosphorus oxychloride (46.0 g) in dichloromethane (200 mL) was slowly added dropwise to the sodium eugenol suspension B, the addition was completed in 2 hours, and the reaction was continued for 2 hours. After the reaction is over, add 120 g of 20% sodium hydroxide aqueous solution to the reaction flask to remove unreacted eugenol and generated sodium chloride. The organic layer was separated by extraction, washed with saturated brine until neutral, and dried over anhydr...
Embodiment 2
[0038] 1) Preparation of biomass-based phosphate
[0039] Mix 42.0g of sodium hydroxide with 13mL of water at 1±0.5℃ to obtain paste A. Under stirring conditions, add eugenol (172.4g) and methylene chloride (400mL) to paste A dropwise Sodium eugenol suspension colloid B was prepared. Then, at 20°C, a solution of phosphorus oxychloride (46.0 g) in dichloromethane (250 mL) was slowly added dropwise to the sodium eugenol suspension B. The addition was completed in 3 hours, and the reaction was continued for 3 hours. After the reaction, add 200g of 10% sodium hydroxide aqueous solution to the reaction flask to remove unreacted eugenol and generated sodium chloride. The organic layer was separated by extraction, washed with saturated brine until neutral, and dried over anhydrous sodium sulfate. Rotate the solvent to obtain a light yellow liquid, which is a biomass-based phosphate flame retardant.
[0040] 2) Preparation of flame-retardant bismaleimide resin
[0041] At 20℃, 50.0g N, N...
Embodiment 3
[0043] 1) Preparation of biomass-based phosphate
[0044] Mix 48.0 g of sodium hydroxide and 15 mL of water in an ice water bath at 0~5℃ to obtain paste A. Under stirring conditions, add eugenol (197.0 g) in methylene chloride ( 500mL) solution to prepare sodium eugenol suspension colloid B. Then, at 30°C, a solution of phosphorus oxychloride (46.0 g) in dichloromethane (300 mL) was slowly added dropwise to the sodium eugenol suspension B. The addition was completed in 4 hours, and the reaction was continued for 4 hours. After the reaction is completed, 300g of 5% sodium hydroxide aqueous solution is added to the reaction flask to remove unreacted eugenol and generated sodium chloride. The organic layer was separated by extraction, washed with saturated brine until neutral, and dried over anhydrous sodium sulfate. Rotate the solvent to obtain a light yellow liquid, which is a biomass-based phosphate flame retardant.
[0045] 2) Preparation of flame-retardant bismaleimide resin
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