Organic phosphorus co-polymerized flame retardant polyamide composition and preparation method thereof
A technology of polyamide composition and flame-retardant polyamide, which is applied in the manufacture of fire-resistant and flame-retardant filaments, single-component polyamide artificial filaments, and rayon manufacture, etc.
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[0066] The preparation method of the organophosphorus-based flame-retardant copolymerized polyamide of the present invention specifically includes: (1) preparing the flame-retardant copolymerized polyamide by the following steps:
[0067] (A) Reaction of organophosphorus flame retardant monomers with diamines, preferably with an excess of amino groups, to generate a salt solution;
[0068] (B) reacting the reaction product of step (A) with diacid and diamine or dibasic amide salt in the presence of inorganic nanomaterials to produce organophosphorus copolymerized flame-retardant polyamide;
[0069] (B') reacting the reaction product of step (A) with diacid and diamine or dibasic amide salt to produce organophosphorus copolymerized flame-retardant polyamide, and then blending the copolymerized flame-retardant polyamide with inorganic nanomaterials.
[0070] In step (A), preferably, the diamine monomer is slightly excessive, so that the pH of the salt solution is 7-9. The react...
Embodiment 1
[0088] Stir and react the flame retardant monomer and hexamethylenediamine in an aqueous solution at a molar ratio of 1:1.2 at 40°C for 0.5h, adjust the pH of the solution to 7.2, and dry to form a salt. Mix 50% nylon 66 salt (hexamethylene adipamide salt) solution with the salt obtained above accounting for 6.0% of the mass of nylon 66 salt (excluding the solvent, the same below), accounting for 4wt% of the mass of nano-montmorillonite, each accounting for The catalyst sodium hypophosphite with a ratio of 1wt‰ and the antioxidant p-phenylenediamine were added to the reactor, vacuumed and filled with nitrogen for 5 times, and finally the internal pressure of the reactor was kept at 0.2MPa. Heat the reactor, keep stirring at a high speed, and when the temperature of the reactor reaches 220°C and the pressure is 1.8 MPa, keep the temperature and pressure constant for 1.5 hours. Then the temperature was raised to 250°C, and the pressure was released to normal pressure within 1 ho...
Embodiment 2
[0091] Stir the flame retardant monomer and hexamethylenediamine in an aqueous solution at 50°C for 1 hour at a molar ratio of 1:1.3, and adjust the pH of the solution to 7.8. Adipic acid and hexamethylenediamine are configured according to the molar ratio of 1:1.2, and the above-mentioned salt solution (calculated as salt) accounting for 7% of its weight, and nano-talc accounting for 4wt% of its weight, each accounting for 1‰ The catalyst toluenesulfonic acid, the antioxidant 2,6-di-tert-butyl-4-methylphenol, and 35% deionized water were added to the reactor, vacuumed, nitrogen filled 3 times, and finally kept the reaction The pressure inside the kettle is 0.3MPa. Heat the reactor, keep stirring at a high speed, and when the temperature of the reactor reaches 215°C and the pressure is 1.7 MPa, keep the temperature and pressure constant for 1.6 hours. Then the temperature was raised to 240°C, and the pressure was released to normal pressure within 1.5 hours. Vacuumize to -0....
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