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Method for preparing poly(p-phenylene terephthalamide) (PPTA) resin

A technology of poly-p-phenylene terephthalamide and terephthaloyl chloride, which is applied in the field of preparation of p-phenylenediamine resin, can solve the problems of severe toxicity, strong smell, and unfriendly operating conditions, and reduce the Degradation, simple preparation method, and the effect of avoiding adverse effects

Inactive Publication Date: 2012-07-11
DONGHUA UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method adds a pyridine acid-absorbing agent in the final polymerization stage, which has a strong smell and is highly toxic, and the operating conditions are not friendly.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] (1) Feed high-purity nitrogen (purity greater than 99.999%) into a 100L jacketed stainless steel reactor with a flow rate of 2L / min, add 50kg of anhydrous N-methylpyrrolidone (NMP), and add 2.63Kg to activate at high temperature After the anhydrous calcium chloride is completely dissolved, 2.05Kg of p-phenylenediamine is added, and after it is fully dissolved, it is cooled to -15°C. Slowly add 3.28Kg of terephthaloyl chloride powder into the system, and adopt a jacket cooling method to keep the system temperature at about -10°C. After the addition is completed, react for 18 minutes to obtain a prepolymer.

[0026] (2) Add the prepolymer at -10°C with a diameter of 0.5Kg / min In a twin-screw reaction extruder with a length neck ratio of 50 and a rotational speed of 180rpm, add 0.58Kg of terephthaloyl chloride powder at the same time, adjust the airflow rate to 2L / min, and control the temperature of the screw reactor to 70°C. After 15 minutes, The light yellow powder pol...

Embodiment 2

[0029] (1) Feed high-purity nitrogen (purity greater than 99.999%) into a 100L jacketed stainless steel reactor with a flow rate of 5L / min, add 50kg of anhydrous N-methylpyrrolidone (NMP), and add 2.63Kg to activate at high temperature After the anhydrous calcium chloride is completely dissolved, 2.05Kg of p-phenylenediamine is added, and after it is fully dissolved, it is cooled to -15°C. Slowly add 3.28Kg of terephthaloyl chloride powder into the system, and adopt a jacket cooling method to keep the system temperature at about -10°C, adjust the system pressure to 0.25MPa, and react for 18 minutes after the addition to obtain a prepolymer.

[0030] (2) Add the prepolymer at -10°C with a diameter of 0.5Kg / min In a twin-screw reaction extruder with a length neck ratio of 50 and a rotational speed of 180rpm, add 0.58Kg of terephthaloyl chloride powder at the same time, adjust the airflow rate to 5L / min, and control the temperature of the screw reactor to 70°C. After 15 minutes,...

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Abstract

The invention relates to a method for preparing poly(p-phenylene terephthalamide) (PPTA) resin. The method comprises the following steps of: (1) introducing inert gas, adding p-phenylenediamine into cosolvent-containing N-methyl pyrrolidone (NMP) to obtain mixed liquid, adding 50 to 85 percent of the total amount of terephthaloyl chloride after the p-phenylenediamine is completely dissolved, and performing pre-polycondensation to obtain prepolymer; and (2) adding the prepolymer and the rest terephthaloyl chloride into a double-screw extruder simultaneously, introducing inert gas, performing final polycondensation reaction, and extruding after the reaction is completely performed; and standing the extruded polymer, washing, dehydrating, and drying. An acid-acceptor is not required to be added during preparation, environment-friendly production is performed, and a few impurities are introduced; and the PPTA resin has small average particle size, large specific surface area, high molecular weight, low ash content and high logarithmic viscosity number, and is easy to clean.

Description

technical field [0001] The invention belongs to the field of preparation of p-phenylenediamine resin, in particular to a preparation method of poly-p-phenylenediamine terephthalamide resin. Background technique [0002] Poly-p-phenylene terephthalamide resin is the raw material for preparing high-strength, high-modulus, high-temperature-resistant special fiber aramid 1414 and aramid pulp with high wear resistance and high dispersibility. The strength is 5 to 6 times that of steel wire, the specific modulus is 2 to 3 times that of steel wire, para-aramid fiber that can withstand high temperatures of 350 ° C, and aramid pulp that is an ideal substitute for asbestos. It is made of insulating paper with high temperature resistance and friction resistance, so it is widely used in aerospace, transportation and communication, chemical and other departments. [0003] There are many patent reports on the preparation method of poly-p-phenylene terephthaloyl chloride. CN101550231A pro...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G69/32C08G69/28
Inventor 余木火张蕊叶盛滕翠青马禹孔海娟焦玉聪周建军田银彩尤伟刘振全王征辉
Owner DONGHUA UNIV
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