A kind of macromolecular nitrogen and phosphorus expansion flame retardant based on cyclotriphosphazene and preparation method thereof
A technology of intumescent flame retardant and cyclotriphosphazene, which is applied in the field of flame retardant synthesis, can solve the problems of limiting the application of halogen-based flame retardants, secondary poisoning, etc., and is conducive to sustainable development and high flame retardant efficiency. , the effect of good application prospects
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Embodiment 1
[0028] Add 9.7g of dicyandiamide to a 500ml four-neck flask equipped with a stirrer, reflux condenser, and inert gas inlet tube, add dimethyl sulfoxide as a solvent to dissolve it, add 10g of pyridine as an acid-binding agent, and pass through helium After heating up to 50°C, 10g of hexachlorocyclotriphosphazene was dissolved in N,N-dimethylformamide and then added dropwise into the four-necked flask with a dropping funnel, and the temperature was controlled at 50°C for 10 hours. Cool to room temperature after the reaction, filter, wash three times with 200ml dimethyl sulfoxide, and dry at 80°C to obtain macromolecular nitrogen and phosphorus intumescent flame retardant. The infrared spectrogram of the macromolecular nitrogen and phosphorus intumescent flame retardant prepared by the present embodiment is as follows: figure 1 shown at 3300cm -1 The double peak split at -1 disappears basically, indicating that the chlorine on the hexachlorocyclotriphosphazene is replaced by a...
Embodiment 2
[0033] Add 14.5g of dicyandiamide into a 500ml four-necked flask equipped with a stirrer, reflux condenser, and inert gas inlet pipe, add toluene as a solvent to dissolve it, add 15g of triethylamine as an acid-binding agent, and let nitrogen flow and heat up After reaching 80°C, dissolve 10g of hexachlorocyclotriphosphazene in toluene and add it dropwise into a four-neck flask with a dropping funnel, control the temperature at 80°C for 9 hours, cool to room temperature after the reaction, and filter with Wash three times with 200ml ethanol and 200ml deionized water, and dry at 80°C to obtain macromolecular nitrogen and phosphorus intumescent flame retardant. The thermal weight loss curve of the macromolecular nitrogen and phosphorus intumescent flame retardant prepared in this embodiment is as follows figure 2 shown. Depend on figure 2 It can be seen that the mass residue of the flame retardant at 700°C is 30.1%, which shows that the flame retardant efficiency is high.
Embodiment 3
[0035] Add 19.3g of dicyandiamide to a 500ml four-necked flask equipped with a stirrer, reflux condenser, and inert gas inlet tube, add N,N-dimethylformamide as a solvent to dissolve it, and then add 15g of imidazole as an acid-binding After passing argon and raising the temperature to 120°C, dissolve 10g of hexachlorocyclotriphosphazene in dimethyl sulfoxide and add it dropwise into the four-necked flask with a dropping funnel, and control the temperature at 120°C for 5 hours. Cool to room temperature after completion, filter, wash three times with 200ml dimethyl sulfoxide and 200ml deionized water, and dry at 80°C to obtain macromolecular nitrogen and phosphorus intumescent flame retardant. Macromolecular nitrogen, phosphorus expansion flame retardant prepared by the present embodiment 31 P NMR spectrum as image 3 shown. 31P NMR (ppm, soil), δ=16.51-19.53 ppm. Apply the obtained macromolecular nitrogen and phosphorus intumescent flame retardant to the silicone rubber fla...
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