A kind of halogen-free intumescent flame-retardant polycarbonate composite material and preparation method thereof
A technology of flame-retardant polycarbonate and intumescent flame retardant, which is applied in the field of polymer material preparation, can solve the problems of stress cracking, lower polycarbonate hydrolysis stability, heat distortion temperature, and high price, and achieve improved flame-retardant performance Effect
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Embodiment 1
[0037] Example 1: Preparation of halogen-free intumescent flame-retardant polycarbonate composite material
[0038] (1) Preparation of nitrogen-phosphorus flame retardant:
[0039] Add 28.9g of trimethyl phosphite and 8g of self-made dimethylolurea into a 250mL reaction flask, stir mechanically and raise the temperature to 100°C, and keep it warm for 2h. Add the remaining 53.82g of trimethyl phosphite into the constant pressure dropping funnel, and control the dropping rate at 1d / 5s. At the same time, add the remaining 12g of dimethylolurea in batches, and the temperature is still controlled at 100°C. After the feeding was completed, the temperature was raised to 140° C. after 30 minutes of heat preservation, and the reaction solution was transparent for 4 hours of heat preservation, and the heating was stopped. Distill under reduced pressure at 137°C and 0.5mmHg vacuum to obtain oligomers of N,N'-dimethylphosphorylurea with a yield of 95%, which is used as a nitrogen-phospho...
Embodiment 2
[0042] Example 2: Preparation of halogen-free intumescent flame-retardant polycarbonate composite material
[0043] (1) Preparation of nitrogen-phosphorus flame retardant:
[0044] Add 3.0g of paraformaldehyde and 10mL of isopropanol into a 250mL reaction flask equipped with mechanical stirring, adjust the pH to 10 with 1% sodium hydroxide solution, stir mechanically and raise the temperature to 70°C, and keep it warm for 40min to obtain paraformaldehyde the depolymerization solution. Add 12.6g of melamine in batches, and at the same time add 91.7mL of triphenyl phosphite dropwise, after the addition is complete. Incubate at 70°C for 3h. Then the temperature was raised to 165°C, and the generated phenol was distilled off, and the holding time was determined by the amount of generated phenol. After the reaction was completed, by-products were distilled off under reduced pressure to obtain 2,4,6-triaminomethylphosphonic acid diphenyl ester-1,3,5-triazine with a yield of 87%, ...
Embodiment 3
[0047] Example 3: Preparation of halogen-free intumescent flame-retardant polycarbonate composite material
[0048] (1) Preparation of nitrogen-phosphorus flame retardant:
[0049] Add 143.8g of triethyl phosphite into a 500mL four-necked flask equipped with a stirrer, a thermometer, and a bubbler, and add 28.3g of cyanuric chloride in batches within 2 hours. After the addition is complete. Slowly raise the temperature to 100°C and keep it warm for 7h. Filter, wash the filter cake with petroleum ether, and recrystallize with ethanol to obtain 2,4,6-diethyl triphosphate-1,3,5-triazine with a yield of 90%, which is used as a nitrogen-phosphorus flame retardant.
[0050] (2) Using zinc borate as a synergist; ABS grafted maleic anhydride (ABS-g-MAH) as a compatibilizer; tetrakis[(2,4-di-tert-butylphenol)-4,4' Phenyl]diphosphite and 2,4,6-tris(2'-hydroxyl-4'-n-butoxyphenyl)-1,3,5-triazine are mixed in a mass ratio of 1:1.5 as auxiliary agent; 100g polycarbonate, 90g step (1) pre...
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