Semi-continuous preparation method of poly p-phenylene terephthalamide resin

The technology of poly-p-phenylene terephthalamide and terephthaloyl chloride is applied in the field of semi-continuous preparation of poly-p-phenylene terephthalamide resin, and can solve the problem of high requirements on metering accuracy and feeding equipment. Expensive, difficult to dissipate heat, etc., to achieve the effects of stable performance, good spinnability and good solubility

Inactive Publication Date: 2004-11-17
DONGHUA UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0010] The technical problem to be solved in the present invention is to disclose a method for preparing poly-p-phenylene terephthalamide resin in a semi-continuous manner, so as to overcome the difficulty of heat dissipation in the prior art, the defects of easy local overheating, and the continuous polycondensation In the process, there are unfavorable factors such as expensive feeding equipment and high measurement accuracy requirements

Method used

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  • Semi-continuous preparation method of poly p-phenylene terephthalamide resin

Examples

Experimental program
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Embodiment 1

[0032] In 4 500ml of anhydrous N-methylpyrrolidone (NMP) solution, add 0.30kg of anhydrous calcium chloride to prepare NMP-CaCl 2 Solution, add 0.216kg of p-phenylenediamine (PPDA) at about 15°C, let it fully dissolve, cool to 5°C, add 0.100kg of terephthaloyl chloride (TPC) for pre-condensation, and the pre-condensation polymer produced by the reaction, in Store at a constant temperature below 5°C for later use. Add the precondensed polymer and the remaining 0.306kg of terephthaloyl chloride (TPC) powder into a twin-screw reaction extruder with a diameter of Φ25, an aspect ratio of 40, and a rotational speed of 200rpm, and feed dry liquid ammonia . Control the temperature of the twin-screw reactor at 70°C for about 15 minutes to extrude the polycondensation product in the form of light yellow corn flour, let it stand for 2 hours, remove the solvent, grind it, wash it with water, and dry it to obtain a light yellow polyterephthalmic P-phenylenediamide resin powder, its intri...

Embodiment 2

[0034] In 4500ml of N-methylpyrrolidone (NMP) solution, add 0.30kg of anhydrous calcium chloride to prepare NMP-CaCl2 solution, add 0.203kg of p-phenylenediamine (PPDA) at about 20°C, let it fully dissolve, and cool To 5°C, add 0.22kg of terephthaloyl chloride (TPC) for pre-condensation, and the pre-condensation polymer produced by the reaction is kept at a constant temperature below 5°C for later use. Add the precondensed polymer and the remaining 0.203kg terephthaloyl chloride (TPC) powder into a twin-screw reaction extruder with a diameter of Φ25, an aspect ratio of 40, and a rotational speed of 200rpm to control the temperature of the twin-screw reactor At 50°C, add 0.27kg PVP K30 to the third section of the twin-screw for about 15 minutes to extrude a light yellow corn flour-like polycondensation product, let it stand for 2 hours, remove the solvent, pulverize, wash with water, and dry to obtain light yellow corn flour polycondensation product. Yellow poly-p-phenylene ter...

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Abstract

The invention discloses a semi-continuous preparation method of poly p-phenylene terephthalamide resin which comprises the steps of, proceeding pre-polycondensation to p-phenylene diamine and part of the paraphthaloyl chloride into the dissolvent architecture of solvent and assisting solvent, charging in pre-polymerization member and the remaining paraphthaloyl chloride powder into double bolt extrusion machine, letting in dried liquid ammonia to neutralize the hydrogen chloride gas produced in the reaction, and charging macromolecular addictive polyvinylpyrrolidone into the double bolt extrusion machine to obtain the polymer.

Description

technical field [0001] The present invention relates to the preparation method of poly-p-phenylene terephthalamide resin, in particular to the semi-continuous preparation method of poly-p-phenylene terephthalamide resin with twin-screw extruder as the main reactor . Background technique [0002] Poly(p-phenylene terephthalamide) resin is the raw material for preparing high-strength, high-modulus, high-temperature-resistant special fiber para-aramid and aramid pulp with high friction resistance and high dispersibility. It can be made into aramid fiber whose specific strength is 5 to 6 times that of steel wire, and whose specific modulus is 2 to 3 times that of steel wire, which can withstand high temperatures of 350 ° C. As an ideal substitute for asbestos, it can be made into insulating paper with high temperature resistance and friction resistance. It is widely used in aerospace, transportation and communication, chemical industry and other departments. [0003] Existing ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G69/32
Inventor 尤秀兰周助胜王芳朱福和刘兆峰胡祖明
Owner DONGHUA UNIV
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