A high-efficiency furan ring-containing bio-based flame retardant and its synthesis method and application
A furan ring and bio-based technology, which is applied in the field of high-efficiency furan ring-containing bio-based flame retardants and their synthesis, can solve the problems of high toxicity, low flame retardant efficiency, and environmental hazards, achieve less side reactions, improve crystallization performance, The effect of high purity
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Embodiment 1
[0051] 1) In a 250mL three-necked round-bottomed flask equipped with magnetic stirring, disperse 0.30mol of methylfurylamine and 0.40mol of triethylamine into 100ml of acetonitrile solution and stir evenly;
[0052] 2) Add 0.10mol of phosphorus oxychloride to 50mL of acetonitrile solution and stir evenly;
[0053] 3) Slowly drop the acetonitrile solution containing phosphorus oxychloride into the acetonitrile solution containing furanmethylamine and triethylamine in an ice-water bath and nitrogen atmosphere with a constant pressure dropping funnel, and the dropping time is controlled within 2 hours. After the dropwise addition, react at room temperature for 2 h, then raise the temperature to 50° C. and continue to react for 6 h.
[0054] 4) After the reaction, remove the white precipitate by filtration, remove the solvent by rotary evaporation, add ethyl acetate for dissolution, wash 5 times with deionized water, and remove the ethyl acetate by rotary evaporation to obtain a y...
Embodiment 2
[0059] In an ice-water bath and a nitrogen atmosphere, add 0.30 mol of methylfuranamine and 0.60 mol of triethylamine in chloroform to a 250 mL three-necked round-bottomed flask equipped with magnetic stirring. After stirring evenly, use a constant pressure dropping funnel to The chloroform solution of 0.50mol phosphorus oxychloride was slowly dropped into the flask, and the dropping time was controlled at 0.5h. After the dropwise addition, react at room temperature for 4 h, then raise the temperature to 80° C. and continue to react for 4 h. After the reaction was completed, it was washed with deionized water for 5 times, and the solvent was removed by rotary evaporation to obtain a light yellow solid product, the structural formula of which was shown in Formula 1.
Embodiment 3
[0061] In an ice-water bath and a nitrogen atmosphere, add 0.30 mol of furan methanol and 0.30 mol of pyridine in a 1,4-dioxane solution into a 250 mL three-neck round bottom flask equipped with magnetic stirring. The 1,4-dioxane solution of phosphorus oxychloride (0.1mol) was slowly dropped into the flask through the funnel, and the dropping time was controlled at 1.5h. After the dropwise addition, react at room temperature for 2 h, then raise the temperature to 50° C. and continue to react for 6 h.
[0062] After the reaction, the white precipitate was removed by filtration, the solvent was removed by rotary evaporation, washed 5 times with deionized water, and vacuum-dried to obtain the dark brown target product, whose structural formula is shown in formula 2:
[0063]
[0064] The compound prepared above can prove that the structure shown in the above formula has been obtained by proton nuclear magnetic spectrum, phosphorous nuclear spectrum and infrared spectrum. The ...
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