A kind of polyphosphoramide fiber and its solution method preparation method
A technology of polyphosphoramide and fiber solution, which is applied in the field of polyphosphoramide fiber and its solution method preparation, can solve the problems of low rheological temperature, difficult dyeing and finishing, low efficiency, etc., achieve good flame retardant effect, simple preparation process, easy-to-operate effect
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Embodiment 1
[0025] Put 105 mol dimethyl methylphosphonate, 100 mol 4,4'-diaminophenylphenyl phosphine oxide, and 1 mol triethylamine into a polymerization kettle and mix well, react at 381°C for 10 hours, and vacuum pump at 80°C after the reaction After extracting for 2 hours, cool to room temperature after extraction to obtain a light yellow solid, which is a polyphosphoramide resin with a degree of polymerization of 1620. Dissolve the polyphosphoramide resin in N,N-dimethylformamide solvent, stir, filter, and defoam to obtain a spinning solution with a concentration of 14%; after the spinning solution is extruded by a spinning machine, it is passed through A coagulation bath composed of 15% water, 55% ethanol, and 30% methanol is formed. The temperature of the coagulation bath is 40°C, the passage time is 0.5 seconds, and the speed is 80m / min; continue to pass through the water bath with a temperature of 35°C for washing and oiling , obtain 0.83 denier polyphosphoramide fiber filaments,...
Embodiment 2
[0030] Put 100mol of dimethyl methylphosphonate, 100mol of 4,4'-diaminophenylphosphine oxide, and 1.5mol of triphenyl phosphate into a polymerization kettle and mix evenly, react at 379°C for 12h, and vacuum pump at 80°C after the reaction After extraction for 2 hours, cool to room temperature after the extraction to obtain a light yellow solid, which is a polyphosphoramide resin with a degree of polymerization of 1970. Dissolve the polyphosphoramide resin in N, N-dimethylformamide solvent, stir, filter, and defoam to obtain a spinning solution with a concentration of 12%; after the spinning solution is extruded by a spinning machine, the The coagulation bath composed of 17% water, 51% ethanol, and 32% methanol is formed. The temperature of the coagulation bath is 45°C, the passage time is 0.6 seconds, and the speed is 67m / min; continue to pass through the water bath with a temperature of 35°C for washing and oiling , to obtain 1.26 denier polyphosphoramide fiber filament semi...
Embodiment 3
[0035] Put 125 mol dimethyl methylphosphonate, 100 mol 4,4'-diaminophenylphenyl phosphine oxide, and 1.5 mol ferric chloride into a polymerization kettle and mix evenly, react at 386°C for 8 hours, and after the reaction is completed, 80°C Vacuum extraction for 1.5 h, and cooling to room temperature after the extraction was completed, to obtain a light yellow solid, which is a polyphosphoramide resin with a degree of polymerization of 630. Dissolve the polyphosphoramide resin in N, N-dimethylformamide solvent, stir, filter, and defoam to obtain a spinning solution with a concentration of 18%; after the spinning solution is extruded by a spinning machine, it is passed through The coagulation bath composed of 15% water, 60% ethanol, and 25% methanol is formed. The temperature of the coagulation bath is 30°C, the passing time is 0.8 seconds, and the speed is 50m / min; continue to pass through the water bath with a temperature of 35°C for washing and oiling , obtain 2.0 denier poly...
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