Synthesis method and application of poly(p-phenylene terephthamide)
A technology of poly-p-phenylene terephthalamide and its synthesis method, which is applied in the field of polymer synthesis to achieve the effects of continuous production, stable product quality, and simple process flow
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[0015] A method for synthesizing poly-p-phenylene terephthalamide provided in the embodiment of the present invention is specifically a method for synthesizing high-quality poly-p-phenylene terephthalamide resin. The method specifically includes the following steps:
[0016] N-methylpyrrolidone (NMP) and calcium chloride (CaCl 2 ) aqueous solution as the raw material, under the protection of protective gas (preferably nitrogen), add p-phenylenediamine (PPD) melt at 15°C-20°C, stir and dissolve, then lower the temperature to obtain p-phenylenediamine (PPD) solution;
[0017] The p-phenylenediamine (PPD) solution and the terephthaloyl chloride (TPC) melt are mixed in a closed mixer and then polycondensed in a single-stage twin-screw extruder. The reaction product is washed with water and dried to obtain a light yellow color. The poly-p-phenylene terephthalamide resin powder is the poly-p-phenylene terephthalamide.
[0018] As another preferred embodiment of the present inventi...
Embodiment 1
[0041] A synthetic method for poly-p-phenylene terephthalamide, mainly comprising the following steps:
[0042] 1) Preparation of NMP / CaCl 2 Mixed solvent: Stir and mix 3000kg of NMP and 500kg of calcium chloride aqueous solution with a concentration of 38.0wt% in a stainless steel stirring tank with a jacket, steam the jacket, heat the mixed solution to 90°C-95°C, and then Put the mixed solution into the vacuum distillation tower to distill and remove water. The vacuum degree is -99.0kPa, and the temperature at the top of the tower is 95°C. The index of the mixed solvent is: the moisture content is 50ppm, CaCl 2 The content is 5.5wt%, the solid impurity content is 0.5ppm, the chloroform content is 20ppm, the iron ion content is 0.2ppm, and the color of the mixed solvent is light yellow. After filtering through a 25 μm filter, use a refrigerant to cool the above mixed solvent to 10°C for later use.
[0043] 2) Preparation of PPD solution: Add the PPD melt at 150°C to the NMP...
Embodiment 2
[0046] A synthetic method for poly-p-phenylene terephthalamide, mainly comprising the following steps:
[0047] 1) Preparation of NMP / CaCl 2 Mixed solvent: Stir and mix 2800kg of NMP and 500kg of calcium chloride aqueous solution with a concentration of 38.0wt% in a stainless steel stirring tank with a jacket, steam the jacket, heat the mixed solution to 90°C-95°C, and then Put the mixed solution into a vacuum distillation tower to distill and remove water, the vacuum degree is -99.0kPa, and the temperature at the top of the tower is 96°C. The index of the mixed solvent is: the moisture content is 60ppm, the CaCl 2 The content is 7.0wt%, the solid impurity content is 0.4ppm, the chloroform content is 25ppm, the iron ion content is 0.1ppm, and the color of the mixed solvent is light yellow. After filtering through a 20 μm filter, use a refrigerant to cool the above mixed solvent to 10°C for later use.
[0048] 2) Preparation of PPD solution: Add the PPD melt at 150°C to the N...
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