A kind of preparation method of modified phosphorus nitrogen type flame retardant
A flame retardant and modification technology, which is applied in the field of preparation of modified phosphorus-nitrogen flame retardants, can solve the problem of unsatisfactory improvement of polycarbonate flame retardancy, achieve a significant increase in LOI, and improve flame retardancy Effect
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Embodiment 1
[0019] (1) Synthesis reaction:
[0020] In a 1000L reactor, add 100Kg phosphoric acid, 50Kg ethylene glycol, 110Kg melamine, 3Kg methyl isobutyl carbinol; esterify at 120°C for 3 hours, and react at 110°C for 1 hour, then cool and wash , to get intermediate products.
[0021] (2) Modification treatment
[0022] In the 5000L reactor, add 100Kg intermediate product, 15Kg vinyl acetate, 0.5Kg dimethylsilyl (cyclopentadiene) (9-fluorenyl) zirconium dichloride, 0.5Kg dicyclopentadiene, 2000Kg toluene, 3Kg hydroxymethylcellulose, 1Kg azobisisoheptanonitrile, react at 85°C for 8h to obtain the product. Product number M-1.
Embodiment 2
[0024] (1) Synthesis reaction:
[0025] In a 1000L reactor, add 100Kg of phosphoric acid, 30Kg of ethylene glycol, 70Kg of melamine, and 1Kg of methyl isobutyl carbinol; at 100°C for 1 hour of esterification, at 100°C for 0.5 hour of salt formation, and then cool. Washing yields an intermediate product.
[0026] (2) Modification treatment
[0027] In the 5000L reactor, add 100Kg intermediate product, 5Kg vinyl acetate, 0.1Kg dimethylsilyl (cyclopentadiene) (9-fluorenyl) zirconium dichloride, 0.1Kg dicyclopentadiene, 1000Kg toluene, 1Kg hydroxymethylcellulose, 0.5Kg azobisisoheptanonitrile, react at 80°C for 5h to obtain the product. Product number M-2.
Embodiment 3
[0029] (1) Synthesis reaction:
[0030] In a 1000L reactor, add 100Kg phosphoric acid, 70Kg ethylene glycol, 110Kg melamine, 5Kg methyl isobutyl carbinol; esterify at 130°C for 4 hours, and react at 120°C for 2 hours, then cool and wash get intermediate products.
[0031] (2) Modification treatment
[0032] In a 5000L reactor, add 100Kg intermediate product, 20Kg vinyl acetate, 1Kg dimethylsilyl (cyclopentadiene) (9-fluorenyl) zirconium dichloride, 1Kg dicyclopentadiene, 3000Kg toluene, 4Kg hydroxyl Methyl cellulose and 2Kg azobisisoheptanonitrile were reacted at 95°C for 12 hours to obtain the product. Product number M-3.
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