Preparation method and application of halogen-free intumescent flame retardant with crosslinking structure
A technology of intumescent flame retardants and intumescent flame retardants, which is applied in the field of preparation of halogen-free intumescent flame retardants, can solve the problems of poor compatibility, decreased flame retardant performance, easy migration and precipitation, etc., and achieves the best temperature resistance And water resistance, stable flame retardant performance, simple preparation process
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[0029] A preparation method of a halogen-free intumescent flame retardant, comprising the following steps:
[0030] 1) Add phosphorus pentoxide and diammonium hydrogen phosphate into the kneader at a molar ratio of 1:1.0-1.1, preheat the material to 100-300°C, and preheat at 20-25m 3 / h flow into ammonia for 30-40min; then 8-15m 3 The flow rate of / h continues to feed ammonia gas for 4-8h;
[0031] 2) Stop feeding ammonia gas, and keep the temperature at 200-300°C for 0.5-2h;
[0032] 3) Add the triazine compound into the kneader to react with the product obtained in the previous step, control the reaction temperature in the kneader to 150-250°C, the reaction time is 1-4h, the quality of the triazine compound: pentoxide The total mass of diphosphorus and diammonium hydrogen phosphate=15-45:100;
[0033] 4) Put the formaldehyde solution into the kneader to cause a cross-linking reaction with the product obtained in the previous step. Control the reaction temperature in the k...
Embodiment 1
[0044] 1) Transport 141.95kg of crystalline H-type phosphorus pentoxide and 138.66kg of diammonium hydrogen phosphate to the kneader by twin-screw, preheat the materials to 220°C, and feed 22m 3 / h of ammonia gas, through ammonia for 32min; then with 10m 3 The flow rate of / h continuously feeds ammonia gas for 4h;
[0045] 2) Stop feeding ammonia gas, and keep the temperature at 260°C for 1 hour to partially deaminate the product obtained in the previous step;
[0046] 3) Add 70.15kg of triazine compound into the kneader, and the triazine compound reacts with the product obtained in the previous step. Control the reaction temperature in the kneader to 180°C, and the reaction time is 1.5h;
[0047]4) Add 14.03kg of 37% (mass concentration, the concentration of formaldehyde in the following examples is the mass concentration) formaldehyde solution into the kneader, the formaldehyde solution and the product obtained in the previous step undergo a cross-linking reaction, and the ...
Embodiment 2
[0052] 1) Transport 141.95kg of crystalline H-type phosphorus pentoxide and 132.06kg of diammonium hydrogen phosphate to the kneader by twin-screw, preheat the materials to 250°C, and feed 20m 3 / h of ammonia gas, pass through ammonia for 35 minutes; then use 12m 3 The flow rate of / h is continuously fed with ammonia gas for 6h;
[0053] 2) Stop the ammonia gas flow, and keep the temperature at 250°C for 1.5 hours to partially deaminate the product obtained in the previous step;
[0054] 3) Add 54.80kg of triazine compound into the kneader, the triazine compound reacts with the product obtained in the previous step, control the reaction temperature in the kneader to 200°C, and the reaction time is 3h;
[0055] 4) Add 26.30kg of 37% formaldehyde solution into the kneader, the formaldehyde solution and the product obtained in the previous step undergo a crosslinking reaction, control the reaction temperature in the kneader to 150°C, and the reaction time is 2h;
[0056] 5) at ...
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