Preparation method of phosphorus-containing flame-retardant polymethyl methacrylate resin
A technology of polymethyl methacrylate and polymethacrylic acid is applied in the fields of polymer chemistry and polymers, phosphorus-containing flame retardant resins and their preparation, and can solve problems such as flammability and thermal stability.
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[0013] The preparation steps of phosphorus-containing flame-retardant polymethacrylic resin are:
[0014] In a reaction vessel equipped with a stirrer, a thermometer and a glass tube, add the formula amount of methyl methacrylate, tris((6-oxo-6H-dibenzo[c,e][1,2]oxophosphorus Heterohexacyclo-6-yl) methyl) phosphate and initiator benzoyl peroxide. Stir at 85.2°C for about 52 minutes. The system becomes viscous. Then pour the prepolymer into the mold and cool to about 40°C. The temperature is kept for 6 hours, and then the temperature is increased to 80°C for 12 hours to obtain a flame-retardant polymethacrylic resin.
[0015] According to the above-mentioned preparation method of phosphorus-containing flame-retardant polymethyl methacrylate resin, in terms of mass percentage, three ((6-oxo-6H-dibenzo[c,e][1,2] oxygen The formula of phosphahexyl-6-yl) methyl) phosphate is:
[0016] 6-(Hydroxymethyl)-6H-dibenzo[c,e][1,2]oxahexacyclo-6-oxide 9.87%~11.22%, phosphorus oxychloride 10.11%~...
Embodiment 1
[0043] In a reactor equipped with a stirrer, a thermometer, and a reflux condenser, 56.76 kg of xylene and 35.64 kg of DOPO are added and heated with stirring. DOPO is completely dissolved when the temperature is 85°C. Keep the same temperature, add 4.95kg paraformaldehyde in batches within 2h. After the feeding was completed, the temperature was raised to 120°C, the system refluxed, and the system turned from clear to turbid. Then keep the temperature for 6h and discharge. Wash the precipitate with a large amount of xylene while it is hot and filter with suction. Then place it at 120°C for 48h. A white powder HDOPO is obtained.
Embodiment 2
[0045] Add 5.57kg HDOPO and 32.48g dichloromethane solution to a reactor equipped with a thermometer and a gas pipe, and stir for 30min at 25°C. The temperature of the system was lowered to -8°C, 2.49g of triethylamine was added, stirred and kept for 30 minutes. Then began to drop a mixed solution of 5.78 kg of phosphorus oxychloride and 9.28 kg of methylene chloride. After the dripping is completed, keep the temperature at a low temperature for 2 hours, then heat to 25°C and stir for 6 hours. Discharge, evaporate the solvent and triethylamine in the system. The product was recrystallized to obtain the pure product TOPMP.
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