Poly (p-phenylene benzobisoxazole) polymer and preparation method thereof
A technology of benzobisoxazoles and poly-p-phenylene, which is applied in the field of poly-p-phenylene benzobisoxazole polymers and its preparation, can solve the problems of low elongation at break and achieve high molecular weight, high Toughness, effect of reducing crystallinity
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Embodiment 1
[0047] In a 200L stainless steel reactor equipped with strong stirring, 92.8Kg of polyphosphoric acid (concentration of 84%) was firstly added, and high-purity nitrogen was introduced to replace the air, and then 20Kg of 4,6-diaminoisophthalene was added under nitrogen protection. Phenol hydrochloride, sealed reactor. Stir and evacuate slowly, heat the reaction material in the reactor to 60°C, hold for 12 hours, then slowly heat up to 100°C and continue the reaction for 36 hours, until the gas is neutral when detected by pH test paper at the vacuum outlet.
[0048] The vacuum of the reactor was removed, and 14.0Kg of terephthalic acid, 1.4Kg of adipic acid and 56.0Kg of phosphorus pentoxide were successively added under nitrogen protection, and the reactor was sealed. The reaction system was heated to 120°C for 12 hours, 140°C for 12 hours, then heated to 160°C for 12 hours, and finally continued at 180°C for 12 hours to complete the polymerization reaction. [η] of the polyme...
Embodiment 2
[0050] In a 200L stainless steel reactor equipped with strong stirring, 80.0Kg of polyphosphoric acid (concentration of 82%) was firstly added, and high-purity nitrogen was introduced to replace the air, and then 20Kg of 4,6-diaminoresorcinol was added under nitrogen protection. Hydrochloride, sealed reactor. Stir and evacuated slowly, heat the reaction material in the reactor to 60°C, hold for 8 hours, then slowly heat up to 95°C and continue the reaction for 36 hours, until the gas is neutral when detected by pH test paper at the vacuum outlet.
[0051] The vacuum of the reactor was removed, and 14.8Kg of terephthalic acid, 554g of succinic acid and 56.0Kg of phosphorus pentoxide were sequentially added under nitrogen protection, and the reactor was sealed. The reaction system was heated to 120°C for 8 hours, 140°C for 12 hours, then heated to 160°C for 12 hours, and finally continued at 180°C for 6 hours to complete the polymerization reaction. [η] of the polymer = 33 dL / g...
Embodiment 3
[0053] In a 200L stainless steel reactor equipped with strong stirring, 72.4Kg of polyphosphoric acid (concentration of 80%) was firstly added, and high-purity nitrogen was introduced to replace the air, and then 20Kg of 4,6-diaminoresorcinol was added under nitrogen protection. Hydrochloride, sealed reactor. Stir and slowly evacuated, the reaction material in the reactor was heated to 60°C, kept for 24 hours, and then slowly raised to 100°C to continue the reaction for 24 hours, until the gas was detected as neutral by pH test paper at the vacuum outlet.
[0054] The vacuum of the reactor was removed, and 15.1Kg of terephthalic acid, 485g of 1,4-cyclohexanedicarboxylic acid and 54.5Kg of phosphorus pentoxide were sequentially added under nitrogen protection, and the reactor was sealed. The reaction system was heated to 120°C for 6 hours, 140°C for 8 hours, then heated to 160°C for 12 hours, and finally continued at 180°C for 12 hours to complete the polymerization reaction. ...
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