Preparation of high viscosity Poly(p-phenyleneterephthalamide) resin

A technology of poly-p-phenylene terephthalamide and terephthaloyl chloride, which is applied in the field of polymer chemistry, can solve the problems of high local temperature, high heat generation, and gel generation, and achieve the effect of precise dosage

Active Publication Date: 2008-12-24
SINOPEC YIZHENG CHEM FIBER
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The purpose of the present invention is to solve the phenomenon of poly-p-phenylene terephthalamide resin reaction, which generates too much heat, is difficult to transfer heat in time, local temperature is too high, and produces gel. A small amount of terephthaloyl chloride, and the method for preparing high-viscosity poly-p-phenylene terephthalamide resin with most of terephthaloyl chloride and p-phenylenediamine mixed solution

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Add 18Kg of anhydrous N-methylpyrrolidone (NMP) in a 50L jacketed stainless steel reactor, add 1.68Kg of anhydrous calcium chloride activated by high temperature, and after the dissolution is completed, add 1.04Kg of p-phenylenediamine to make it Fully dissolved, dubbed a solution, cooled to -15 ℃. Add 1.67Kg of terephthaloyl chloride powder to the system, and adopt the jacket cooling method to keep the system temperature at about -10°C. After the addition, react for 15 minutes to obtain a prepolymer. The prepolymer is 0.149Kg / min, and the pyridine is 0.004 Kg / min, 6.3Kg NMP low-temperature mixed solution (-15°C) dissolved with 0.3Kg terephthaloyl chloride is added at a speed of 0.042Kg / min with a liquid metering pump and simultaneously added with a diameter of ∮35, an aspect ratio of 56, and a speed of In the 120rpm twin-screw reaction extruder, the temperature of the screw reactor is controlled at 80°C, and the light yellow corn flour-like polymer can be extruded in a...

Embodiment 2

[0032]Add 18Kg of anhydrous N-methylpyrrolidone (NMP) in a 50L jacketed stainless steel reaction kettle, add 1.68Kg of anhydrous calcium chloride activated by high temperature, and after the dissolution is completed, add 1.17Kg of p-phenylenediamine to make it Fully dissolved, dubbed a solution, cooled to -15 ℃. Add 1.98Kg 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, react for 15 minutes to obtain a prepolymer. The prepolymer is 0.152Kg / min, and the pyridine is 0.004 Kg / min, 6.23Kg NMP mixed solution (-20°C) dissolved with 0.23Kg terephthaloyl chloride was added at the speed of 0.048Kg / min with a liquid metering pump and the diameter was ∮35, the aspect ratio was 56, and the speed was 120rpm In the twin-screw reaction extruder, the temperature of the screw reactor is controlled at 80°C, and the light yellow corn flour-like polymer can be extruded in about 10 minutes, soake...

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Abstract

The invention discloses a method for preparing poly p-phenylene terephtha-lamide resin with high viscosity. Firstly, para-phenylene diamine is fully dissolved and added into a prereactor, then paraphthaloyl chloride is added into the prereactor for prepolycondensation, then a prepolymer is added into a double screw extruder, a pyridine acid absorbent and a remained paraphthaloyl chloride low-temperature solution are respectively and synchronously added for a final polycondensation reaction through a liquid metering pump, and the extrusion is performed; and a polymer is kept stand, washed, dehydrated and dried. The inherent viscosity of the poly p-phenylene terephtha-lamide resin prepared by the method is between 6.5 and 9.5dl/g, the resin has good spinnability, and the spun fiber has good color and luster, high strength, and stable performance.

Description

technical field [0001] The invention belongs to the field of macromolecule chemistry, and in particular relates to a method for preparing high-viscosity poly-p-phenylene terephthalamide resin by means of liquid feeding. 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 wear resistance and high dispersibility. It can be made into aramid fibers whose specific strength is 5-6 times that of steel wire, and whose specific modulus is 2-3 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. , Is widely used in aerospace, transportation, chemical industry. [0003] There are many patent reports on the preparation method of poly-p-phenylene terephthalamide. CN90105870.X p...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G69/32C08G69/28
Inventor 朱福和陈昂李海明邓飞
Owner SINOPEC YIZHENG CHEM FIBER
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