Preparation of pentaerythritol diphosphonate melamine salt
The technology of pentaerythritol bisphosphate melamine salt and bisphosphate melamine salt is applied in the fields of intumescent flame retardant preparation and flame retardant preparation, and can solve the problems of needing organic solvents, low synthesis yield and high product cost, and achieves improved Reaction yield, good flame retardancy and good compatibility
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Embodiment 1
[0028] Take 4.3g Na 2 CO 3 , 11.88g of pentaerythritol diphosphate diphosphoryl chloride, 10.08g of melamine, and 80mL of water were added to a three-neck flask with a stirrer, condenser, and thermometer, heated to reflux, stirred for 10 minutes, stopped the reaction, cooled to room temperature, filtered, and washed with water The product was filtered four times until there was no chloride ion in the filtrate, and dried to obtain 18.8 g of a white solid with a yield of 91.8%.
Embodiment 2
[0030] Take 6.0g of triethanolamine, 5.94g of pentaerythritol diphosphate diphosphoryl chloride, 4.91g of melamine, and 40mL of water into a three-necked flask equipped with a stirrer, condenser, and thermometer, heat to 80°C, stir for 30 minutes, stop the reaction, and cool to Filter at room temperature, wash the filtered product with water six times until there is no chloride ion in the filtrate, and dry to obtain 9.0 g of white solid, with a yield of 89.0%.
Embodiment 3
[0032] Take 12mL of ammonia water, 29.7g of pentaerythritol diphosphate diphosphoryl chloride, 25.2g of melamine, and 250mL of water into a three-necked flask equipped with a stirrer, condenser, and thermometer, heat to 60°C, stir for 60 minutes, stop the reaction, and cool to room temperature. Filter, wash with water five times until there is no chloride ion in the filtrate, add the filtered product to 150mL 1wt% sodium dodecylbenzenesulfonate aqueous solution, stir at 50°C for 30min, cool to room temperature, filter, and dry to obtain 46.5g of white solid, product The rate is 90.8%.
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