Phthalonitrile modified benzoxazine and epoxy resin composite material, preparation and application
A technology of phthalonitrile and epoxy resin, which is applied in the direction of organic chemistry, can solve the problems of insufficient thermal stability, high brittleness of cured products, high curing reaction temperature, etc., and achieve high yield, shortened synthesis cycle, and preparation method easy effect
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[0040] Example 1
[0041] A 500 mL flask equipped with a magnetic stirrer was added with 9.91 g (0.05 mol) 4,4'-diaminodiphenylmethane, 6.00 g (0.20 mol) paraformaldehyde and 250 mL chloroform. The mixture was stirred in an ice bath for 30 minutes, and 22.83 g (0.10 mol) of bisphenol A was added, and then gradually heated to 60° C. to reflux and kept at reflux for 12 hours. After the reaction was cooled to room temperature, anhydrous sodium sulfate was added, dried for 12 hours, and then filtered. The filtrate was rotary evaporated to remove the solvent. The residue was dissolved in 250mL of dried DMF. After the dissolution was completed, 17.31g (0.10mol) of 4-nitrate was added sequentially. After adding phthalonitrile and 27.64 g (0.20 mol) of anhydrous potassium carbonate, the mixture was stirred and reacted at room temperature for 24 hours. After the completion of the reaction, the reaction mixture was poured into a large amount of water to precipitate, the precipitate was co...
Example Embodiment
[0043] Example 2
[0044] A 500 mL flask equipped with a magnetic stirrer was charged with 9.91 g (0.05 mol) 4,4'-diaminodiphenylmethane, 6.00 g (0.20 mol) paraformaldehyde and 250 mL dioxane. The mixture was stirred in an ice bath for 30 minutes, 22.83 g (0.10 mol) of bisphenol A was added, and then the temperature was gradually raised to 100° C. to reflux and kept at reflux for 8 hours. After the reaction was cooled to room temperature, anhydrous sodium sulfate was added, dried for 12 hours, and then filtered. The filtrate was rotary evaporated to remove the solvent. The residue was dissolved in 250mL of dried DMF. After the dissolution was completed, 17.31g (0.10mol) of 4-nitrate was added sequentially. After adding phthalonitrile and 27.64g (0.20mol) anhydrous potassium carbonate, the reaction was stirred at 60°C for 6 hours. After the completion of the reaction, the reaction mixture was poured into a large amount of water to precipitate, the precipitate was collected by fil...
Example Embodiment
[0045] Example 3
[0046] A 500 mL flask equipped with a magnetic stirrer was charged with 9.91 g (0.05 mol) 4,4'-diaminodiphenylmethane, 6.00 g (0.20 mol) paraformaldehyde and 250 mL dimethyl sulfoxide. The mixture was stirred in an ice bath for 30 minutes, 22.83g (0.10mol) of bisphenol A was added, and then the temperature was gradually raised to 120°C for 6 hours. After the reaction was cooled to room temperature, anhydrous sodium sulfate was added, dried for 12 hours and filtered to obtain a DMSO solution of the product, and then 17.31g (0.10mol) 4-nitrophthalonitrile and 43.25g (0.20mol) were sequentially added to it. After adding anhydrous tripotassium phosphate, stir and react at room temperature for 24 hours. After the completion of the reaction, the reaction mixture was poured into a large amount of water to precipitate, the precipitate was collected by filtration and washed with water and ethanol several times to remove impurities. The compound of general formula 1 wa...
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