A kind of preparation method of microscopically dispersed zirconium phosphate synergistic flame retardant spandex
A micro-dispersion and uniform technology, which is applied in the field of polyurethane elastic fiber material manufacturing, can solve the problems of uneven dispersion and good spinnability of spinning dope, and achieve the effects of reduced additive amount, good spinnability and high molecular weight
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preparation example Construction
[0028] A preparation method of microscopically dispersed uniform zirconium phosphate synergistic flame-retardant spandex of the present invention comprises the following steps:
[0029] (1) Prepolymerization stage: at 20°C-60°C, add N,N-dimethylacetamide (DMAC) into the reaction kettle, start stirring, add oligomer polyol, and mix evenly by strong mechanical stirring, Then add diisocyanate to prepare a urethane prepolymer terminated with isocyanate (-NCO), and add DMAC solvent to fully dissolve to obtain a prepolymer solution;
[0030](2) Intercalation modified zirconium phosphate: first, disperse ZrP in DMAC solvent, stir for 24h-96h, preferably 72h, to obtain a uniformly dispersed ZrP solution; Alkanolamine, and add the above ZrP solution and protonated alkanolamine to DMAC at 30°C-80°C (preferably 50°C), raise the temperature to 30°C-80°C (preferably 70°C) and stir for 1h-24h (preferably 5h ), adding other amine compounds to obtain a mixed amine solution;
[0031] (3) Cha...
Embodiment 1
[0040] At 35°C, add N,N-dimethylacetamide (DMAC) to the reaction kettle, start stirring, add oligomer polyol, stir for 2 hours, add non-intercalated modified zirconium phosphate, stir at high speed for 3 hours, and then Add diisocyanate, polymerize at 51° C. for 2 hours, and add DMAC to prepare a prepolymer solution.
[0041] Cool the prepolymer solution to 8°C, add protonated alkanolamine and other amine compounds (without ZrP) to carry out chain extension reaction and chain termination reaction.
[0042] Phosphate ester flame retardant solution, antioxidant, matting agent, lubricating reliever, and antistatic agent are added to obtain a polyurethane spinning stock solution; finally, after the polyurethane spinning stock solution is stored and matured, the flame-retardant spandex is obtained through a dry spinning system.
Embodiment 2
[0044] At 30°C, add N,N-dimethylacetamide (DMAC) to the reaction kettle, start stirring, add oligomer polyol, stir for 2 hours, then stir at high speed for 3 hours, add diisocyanate, at 49°C After polymerization for 2 hours, DMAC was added to prepare a prepolymer solution.
[0045] Cool the prepolymer solution to 8°C, add alkanolamine intercalation modified zirconium phosphate and other amine compounds to carry out chain extension reaction and chain termination reaction.
[0046] Phosphate ester flame retardant solution, antioxidant, matting agent, lubricating reliever, and antistatic agent are added to obtain a polyurethane spinning stock solution; finally, after the polyurethane spinning stock solution is stored and matured, the flame-retardant spandex is obtained through a dry spinning system.
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