Method for preparing poly(p-phenylene terephthalamide)
A technology for poly-p-phenylene terephthalamide and terephthaloyl chloride is applied in the field of preparing poly-p-phenylene terephthalamide polymers, and can solve the problem of removal, strong exothermic removal, and reaction heat removal. and other problems, to achieve the effect of uniform temperature, uniform local temperature, and increased molecular weight
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Embodiment 1
[0025] When equipped with a strong stirring device, N 2 In the 140L reactor at the inlet and outlet, feed the dry high-purity N first. 2 The air in the reactor was replaced. in N 2 Under protection, add 30L solvent and 1000g co-solvent successively, stir and dissolve at 50°C and cool to room temperature, wherein the solvent is N-methylpyrrolidone (NMP), and the co-solvent is calcium chloride, while stirring, add p-phenylenediamine ( PPD) powder 1580g, stirring and dissolving at room temperature. When the system is cooled to -10°C, add 1.5L of pyridine as an additive, 1485g of terephthaloyl chloride (TPC) and 3L of liquid nitrogen, and increase the stirring speed at the same time, 200rpm can be selected, and then add 1485g of TPC after reacting for 10 to 20 minutes. Phthaloyl chloride (TPC) and 3L liquid nitrogen, after the system appears gel, continue to stir rapidly for 20 minutes, the stirring speed can be 400rpm, and the gel block is beaten into powder.
[0026] The pol...
Embodiment 2
[0029] In addition to the complete dissolution of the co-solvent powder in the solvent, the method of adding liquid nitrogen to the system is used to rapidly cool the solvent / co-solvent system to 10-25°C, and the mass ratio of the amount of liquid nitrogen added to the amount of solvent added is 1:20 Outside, all the other are identical with embodiment 1.
Embodiment 3
[0031] When equipped with a strong stirring device, N 2 In the 140L reactor at the inlet and outlet, feed the dry high-purity N first. 2 The air in the reactor was replaced. in N 2 Under protection, add 30L solvent and 1500g co-solvent in turn, stir and dissolve at 50°C and cool to room temperature. The co-solvent powder is dissolved in the solvent overshoot, and the system maintains a slight positive pressure. The solvent is dimethylacetamide, and the co-solvent is chlorine. Lithium oxide. While stirring, 1296 g of p-phenylenediamine (PPD) powder was added, and stirred and dissolved at room temperature. When the system is cooled to 0°C, add 2L of α-picoline as an additive, 1218g of terephthaloyl chloride (TPC) and 2.5L of liquid nitrogen, and increase the stirring speed at the same time. Add 1218g of terephthaloyl chloride (TPC) and 2.5L of liquid nitrogen, and continue to stir rapidly for 20 minutes after the system gels. The stirring speed can be selected as 700rpm, and...
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