A kind of preparation method of mca flame retardant polyamide material
A technology of flame-retardant polyamide and polyamide monomer, which is applied in the field of preparation of MCA flame-retardant polyamide materials, can solve the problems of unsatisfactory nano-dispersion effect, little improvement of flame-retardant efficiency, and unimproved droplet problem. Achieve the effects of excellent flame retardancy and mechanical properties, low cost, and simplified preparation process
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Embodiment 1
[0027] Take equimolar adipic acid and melamine, stir and react at 80° C. for 4 hours, centrifuge, filter and dry to obtain melamine adipate. Take equimolar hexamethylenediamine and cyanuric acid, stir and react at 60°C for 3 hours, centrifuge, filter and dry to obtain hexamethylenediamine cyanurate salt. In parts by weight, in the polymerization kettle, drop 70.32 parts of caprolactam, 10.88 parts of melamine adipate, 9.8 parts of hexamethylenediamine cyanurate, 1 part of SiO 2 , 1 Fe 2 o 3 , 7 parts of water, heated up, melted and stirred, and reacted for 6 hours at 235°C to 253°C and a pressure of 0.5MPa. The small molecules are removed by depressurization, decompression and vacuum pumping, and the material is discharged into pellets and extracted to obtain MCA flame-retardant polyamide 6 resin. The dried flame-retardant PA6 resin was solid-state polycondensed at 200°C for 36 hours to increase the molecular weight, and the vertical burning performance of the sample reache...
Embodiment 2
[0029] Take equimolar adipic acid and melamine, stir and react at 90° C. for 2 h, filter and dry to obtain melamine adipate. Take equimolar hexamethylenediamine and cyanuric acid, stir and react at 70°C for 2.5 hours, centrifuge, filter and dry to obtain hexamethylenediamine cyanurate salt. In parts by weight, in the polymerization kettle, drop 5.44 parts of melamine adipate, 4.9 parts of hexamethylenediamine cyanurate, 0.5 parts of SiO 2 and 0.5 parts TiO 2 , take 84.66 parts of hexamethylenediamine adipate salt solution and put it in the kettle, heat up, melt and stir, and pour N 2 Exclude the air, heat up to 225°C in a sealed environment, and the pressure reaches 1.80Mpa, continue heating after holding the heat for 1 hour, and slowly lower the pressure at the same time, the temperature is 270°C, and when the pressure is normal pressure, hold the heat for 1 hour again and then evacuate to -0.05MPa After 1.5 hours of post-condensation, extrusion, material cutting, drying, a...
Embodiment 3
[0031] Take equimolar isophthalic acid and melamine, stir and react at 90°C for 2.5h, filter and dry to obtain melamine isophthalate. Take equimolar m-phenylenediamine and cyanuric acid, stir and react at 60°C for 3 hours, centrifuge, filter and dry to obtain m-phenylenediamine cyanurate salt. In parts by weight, in the polymerization kettle, 76.05 parts of caprolactam, 10.23 parts of melamine isophthalate, 8.30 parts of m-phenylenediamine cyanurate, 0.78 parts of SiO 2 , 0.64 Fe 2 o 3 And 4 parts of water, heat up, melt and stir, and react for 9 hours at 250°C and pressure of 0.9MPa. Small molecules are removed by pressure relief, decompression and vacuum pumping, and the material is discharged and pelletized to obtain MCA flame-retardant polyamide 6 resin. The dried flame-retardant PA6 resin was solid-state polycondensed at 200°C for 36 hours to increase the molecular weight. The sample had excellent flame-retardant properties and good mechanical properties.
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