Preparation method of high-polymerization-degree melamine polyphosphate
A technology of melamine polyphosphate and high degree of polymerization, which is applied in the field of preparation of melamine polyphosphate, can solve the problems of low flame retardant efficiency, poor compatibility, low thermal stability of melamine polyphosphate, etc., and achieves improved flame retardant effect. , The effect of easy availability of raw materials and large degree of polymerization
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Embodiment 1
[0029] A preparation method of melamine polyphosphate with a high degree of polymerization comprises completely dissolving melamine in deionized water at 50°C, the mass ratio of melamine to deionized water is 1:5, and the dropping concentration is 80wt% industrial phosphoric acid, The dropping time of industrial phosphoric acid is 0.5 hours, wherein the molar ratio of melamine to industrial phosphoric acid is 1:0.5, after the dropping is completed, react at 50°C for 2 hours; then add 0.5% phosphotungsten into the solution dropwise acid, the time to add phosphotungstic acid is 0.2h, and the reaction time is 1 hour at 50°C after the dropwise addition; the final reaction product is cooled, filtered, dried in a blast drying oven at 80°C for 12 hours and crushed to obtain the modified intermediate body; under the protection of nitrogen atmosphere, the modified intermediate is first heated to 200°C and then heated to 380°C at a rate of 0.1°C / min-0.5°C / min for thermal condensation rea...
Embodiment 2
[0031] A preparation method of melamine polyphosphate with a high degree of polymerization comprises completely dissolving melamine in deionized water at 95°C, the mass ratio of melamine to deionized water is 1:50, and the dropping concentration is 90wt% industrial phosphoric acid, The dropping time is 3 hours, and the reaction molar ratio of melamine and industrial phosphoric acid is 1:2. After the dropping is completed, the reaction is carried out at 95°C for 5 hours; then silicotungstic acid with a mass fraction of 5% is added dropwise into the solution , the time to add dropwise silicotungstic acid is 1h, and the reaction time is 3 hours at 95°C after the dropwise addition; the final reaction product is cooled, filtered, dried in a blast drying oven at 150°C for 12 hours and crushed to obtain a modified intermediate; Under the condition of a relative vacuum of -0.08MPa, the temperature of the neutral intermediate is firstly raised to 200°C, and then the temperature is raise...
Embodiment 3
[0033] A preparation method of melamine polyphosphate with a high degree of polymerization, melamine is completely dissolved in deionized water at 60°C, the mass ratio of melamine to deionized water is 1:10, and the concentration of dripping is 81wt% industrial phosphoric acid, The dropping time is 1 hour, wherein the reaction molar ratio of melamine and industrial phosphoric acid is 1:1, and after the dropping is completed, the reaction is carried out at 60°C for 3 hours; then tungstic acid with a mass fraction of 1% is added dropwise to the solution, The time for dropping tungstic acid is 0.3h. After the dropping is completed, the reaction time is 2 hours at 60°C; the final reaction product is cooled, filtered, dried in a blast drying oven at 90°C for 2 hours and crushed to obtain a modified intermediate; The modified intermediate is first heated to 200°C under the protection of nitrogen atmosphere, and then heated to 380°C at a relative vacuum of -0.07MPa at a rate of 0.1°C / ...
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