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

Inactive Publication Date: 2021-07-06
AFCHINA CORP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the embodiments of the present invention is to provide a synthesis method of poly-p-phenylene terephthalamide, to solve the problem that the existing synthesis method of poly-p-phenylene terephthalamide proposed in the above-mentioned background technology cannot carry out poly-p-phenylene terephthalamide Problems of continuous and stable polymerization of p-phenylene terephthalamide

Method used

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preparation example Construction

[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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Abstract

The invention relates to the technical field of polymer synthesis, and particularly discloses a synthesis method and application of poly(p-phenylene terephthamide). According to the synthetic method of the poly(p-phenylene terephthamide), a p-phenylenediamine solution and a terephthaloyl chloride melt are mixed in a closed manner and then are subjected to a condensation polymerization reaction in a single-order twin-screw extruder to generate the poly(p-phenylene terephthamide), the content of solvent impurities is low, and the influence on the reaction is small. The overall polymerization reaction rate is controlled by adjusting the ratio of the content of calcium chloride to the content of p-phenylenediamine in the p-phenylenediamine solution, so that the high-quality poly-p-phenylene terephthamide resin is produced, the technological process is simple, reaction dead zones are reduced, the product quality is stable, continuous production can be realized, the problem that continuous and stable polymerization of the poly-p-phenylene terephthamide cannot be carried out in an existing poly-p-phenylene terephthamide synthesis method is solved, and the method has a wide market prospect.

Description

technical field [0001] The invention relates to the technical field of polymer synthesis, in particular to a synthesis method and application of poly-p-phenylene terephthalamide. Background technique [0002] Poly-p-phenylene terephthalamide (PPTA) is an all-para-position polymer formed by condensation polymerization of p-phenylenediamine (PPD) and terephthaloyl chloride (TPC). Aromatic amide, with excellent compressive strength and flexural strength, stable thermal shrinkage and creep properties, is widely used in the chemical industry, and can be used to prepare bulletproof products, civil engineering products, anti-cut products, friction sealing materials, and synthetic Para-aramid fiber. [0003] Among them, para-aramid fiber has the advantages of high strength, high modulus, high temperature resistance, etc., and is widely used in national defense, optical cable, protection and other fields. The quality and stability of PPTA resin for para-aramid spinning has an impor...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G69/28C08G69/26
CPCC08G69/28C08G69/26
Inventor 范志平潘宏宇韩郡丰巩文玉
Owner AFCHINA CORP CO LTD
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