Long carbon chain semi-aromatic polyamide-imide and synthesis method thereof
A polyamide-imide and semi-aromatic technology, applied in the field of long carbon chain semi-aromatic polyamide-imide (PAI11) and its synthesis, to achieve simple and easy polymerization process, simple preparation process, and good heat resistance Effect
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Embodiment 1
[0034] Hexamethylenediamine, 11-aminoundecanoic acid, and 1,2,4,5-pyromellitic acid after vacuum drying are 1.276kg, 2.01kg, and 2.50kg in mass ratio (molar ratio is 1.1:1:1) Add respectively in the stirring type polymerization reactor, then add 5.786g sodium hypophosphite, lead nitrogen 2min after vacuumizing 10min, so circulate 6 times, make reactant exist in the environment under nitrogen protection, control the system pressure in the reactor as 0.2MPa. Seal the reactor and heat it to 160°C, the stirring speed is 200r / min, control the system pressure in the reactor to 1.1MPa, keep the temperature and keep the pressure and stir for 1 hour, slowly release the gas to normal pressure, then heat the reactor to 300°C, stir The speed was 50 r / min, and after constant temperature, the vacuum was continued for 8 hours, and the vacuum degree in the reactor was kept at 80 Pa, and the reaction was completed. According to the actual situation, the material was filled with nitrogen and d...
Embodiment 2
[0038] Hexamethylenediamine, 11-aminoundecanoic acid, and 1,2,4,5-pyromellitic acid after vacuum drying are 1.276kg, 4.02kg, and 2.50kg in mass ratio (molar ratio is 1.1:2:1) Add respectively in the stirring type polymerization reactor, add 7.796g sodium hypophosphite then, lead nitrogen 2min after vacuumizing 10min, so circulate 6 times, make the reactant exist in the environment under nitrogen protection, control the system pressure in the reactor as 0.2MPa. Seal the reactor and heat it to 160°C, with a stirring speed of 200r / min, control the system pressure in the reactor to 1.1MPa, keep warm and keep the pressure and stir for 1 hour, then slowly release the gas to normal pressure, then heat the reactor to 290°C, stir The speed was 50 r / min, and after constant temperature, the vacuum was continued for 8 hours, and the vacuum degree in the reactor was kept at 80 Pa, and the reaction was completed. According to the actual situation, the material was filled with nitrogen and ...
Embodiment 3
[0042] Hexamethylenediamine, 11-aminoundecanoic acid, and 1,2,4,5-pyromellitic dianhydride after vacuum drying are 1.276kg, 2.01kg, 2.18kg in mass ratio (the molar ratio is 1.1:1: 1) Add 5.466g of sodium hypophosphite to the stirring polymerization reactor respectively, vacuumize for 10 minutes and then pass nitrogen for 2 minutes, and cycle like this for 6 times, so that the reactants exist in the environment under the protection of nitrogen, and control the system pressure in the reactor is 0.2MPa. Seal the reactor and heat it to 170°C. After the stirring speed is 200r / min, control the system pressure in the reactor to 1.1MPa, stir and keep the pressure for 1 hour, slowly release the gas to normal pressure, and then heat the reactor to 300°C. The stirring speed was 50r / min, and after constant temperature, the vacuum was continued for 8 hours, and the vacuum degree in the reactor was kept at 80Pa, and the reaction was completed. According to the actual situation, the materia...
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