Regenerated flame-retardant engineering plastic and preparation method thereof
A technology of engineering plastics and flame retardants, applied in the field of engineering plastics, can solve the problems of poor reproducibility, prone to spontaneous combustion, and no toughness, etc., and achieve the effect of high performance of recycled materials, outstanding cost performance, and environmental protection
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Embodiment 1
[0045] Preparation of flame retardant:
[0046] Step C1, add 0.1mol 2,2'-diphenol and 0.5mol phosphorus oxychloride to a three-necked flask, raise the temperature to 110°C, reflux and stir for 2 hours, remove excess phosphorus oxychloride by rotary evaporation, and obtain intermediate 1 ;
[0047] Step C2, add 0.01mol melamine and 15mL tetrahydrofuran to the three-necked flask, stir to dissolve, add 0.02mol sodium hydride, stir at room temperature for 40min, heat up to 60°C, add 10mL of the tetrahydrofuran solution of intermediate 1, and heat up to 80°C , reacted for 3h, put the product in an ice bath and added saturated ammonium chloride solution to remove excess sodium hydride, rotary steamed to remove tetrahydrofuran, added deionized water to dissolve, extracted with ethyl acetate, combined organic phases, and used anhydrous Drying over sodium sulfate and purifying by column chromatography gave Intermediate 2, wherein the ratio of Intermediate 1 to THF in the tetrahydrofuran...
Embodiment 2
[0051] Preparation of flame retardant:
[0052] Step C1, add 0.2mol 2,2'-diphenol and 1mol phosphorus oxychloride to a three-necked flask, raise the temperature to 110°C, reflux and stir for 2 hours, remove excess phosphorus oxychloride by rotary evaporation, and obtain intermediate 1;
[0053] Step C2, add 0.013mol melamine and 17mL tetrahydrofuran to the three-necked flask, stir to dissolve, add 0.025mol sodium hydride, stir at room temperature for 45min, heat up to 60°C, add 11mL of tetrahydrofuran solution of intermediate 1, and heat up to 80°C , reacted for 3h, put the product in an ice bath and added saturated ammonium chloride solution to remove excess sodium hydride, rotary steamed to remove tetrahydrofuran, added deionized water to dissolve, extracted with ethyl acetate, combined organic phases, and used anhydrous Dried over sodium sulfate, purified by column chromatography to obtain intermediate 2, wherein the ratio of intermediate 1 to tetrahydrofuran in the tetrahy...
Embodiment 3
[0057] Preparation of flame retardant:
[0058] Step C1, add 0.15mol 2,2'-diphenol and 0.75mol phosphorus oxychloride to a three-necked flask, raise the temperature to 110°C, reflux and stir for 2 hours, remove excess phosphorus oxychloride by rotary evaporation, and obtain intermediate 1 ;
[0059] Step C2, add 0.015mol melamine and 20mL tetrahydrofuran to the three-necked flask, stir to dissolve, add 0.03mol sodium hydride, stir at room temperature for 50min, heat up to 60°C, add 12mL of tetrahydrofuran solution of intermediate 1, and heat up to 80°C , reacted for 4h, put the product in an ice bath and add saturated ammonium chloride solution to remove excess sodium hydride, remove tetrahydrofuran by rotary evaporation, add deionized water to dissolve, extract with ethyl acetate, combine organic phases, and use anhydrous Dried over sodium sulfate, purified by column chromatography to obtain intermediate 2, wherein the amount ratio of intermediate 1 and tetrahydrofuran in th...
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