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Method for preparing HMW (High Molecular Weight) p-aramid polymer through ternary co-condensation

A para-aramid fiber and high molecular weight technology, which is applied in the field of ternary copolycondensation to prepare high molecular weight para-aramid fiber polymer to achieve the effects of increasing molecular weight, avoiding side reactions and improving collision probability

Inactive Publication Date: 2018-08-03
THE NORTHWEST RES INST OF CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the PPTA polymer produced by this method is still a solid precipitate, which needs to be dissolved before spinning into fibers

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] This embodiment includes the following steps:

[0023] Step 1. Heat 150mL of NMP to 60°C, then add 3g of CaCl 2 Dissolved, formulated as NMP-CaCl 2 solvent system;

[0024] Step 2, the NMP-CaCl prepared in step 1 2 The solvent system was cooled to -5°C, then fed with nitrogen, and then added 5.25g of 3,4'-diaminodiphenyl ether and 2.835g of p-phenylenediamine under the protection of nitrogen to obtain p-phenylenediamine-NMP-CaCl 2 solution system;

[0025] Step 3, to p-phenylenediamine-NMP-CaCl obtained in step 2 2 Add 10.658g of terephthaloyl chloride to the solution system to obtain the raw material solution system, and carry out the first step of co-polycondensation reaction; the time of the first step of co-polycondensation reaction is 30min;

[0026] Step 4. When colloids appear in the solution of the first step co-condensation reaction in step 3, the reaction temperature is raised to 70° C. to carry out the second step co-condensation reaction to obtain a par...

Embodiment 2

[0028] This embodiment includes the following steps:

[0029] Step 1. Heat 150mL of NMP to 60°C, then add 2.5g of CaCl 2 Dissolved, formulated as NMP-CaCl 2 solvent system;

[0030] Step 2, the NMP-CaCl prepared in step 1 2 The solvent system was cooled to -8°C, then fed with nitrogen, and then added 5.25g of 3,4'-diaminodiphenyl ether and 2.835g of p-phenylenediamine under the protection of nitrogen to obtain p-phenylenediamine-NMP-CaCl 2 solution system;

[0031] Step 3, to p-phenylenediamine-NMP-CaCl obtained in step 2 2 Add 10.658g of terephthaloyl chloride to the solution system to obtain the raw material solution system, and carry out the first step of co-polycondensation reaction; the time of the first step of co-polycondensation reaction is 35min;

[0032] Step 4. When colloids appear in the solution of the first step of co-condensation reaction in step 3, the reaction temperature is raised to 73° C. to carry out the second step of co-condensation reaction to obta...

Embodiment 3

[0034] This embodiment includes the following steps:

[0035] Step 1. Heat 150mL of NMP to 60°C, then add 3g of CaCl 2 Dissolved, formulated as NMP-CaCl 2 solvent system;

[0036] Step 2, the NMP-CaCl prepared in step 1 2 The solvent system was cooled to -10°C, then fed with nitrogen, and then added 6.0g of 3,4'-diaminodiphenyl ether and 3.24g of p-phenylenediamine under the protection of nitrogen to obtain p-phenylenediamine-NMP-CaCl2 solution system;

[0037] Step 3, to p-phenylenediamine-NMP-CaCl obtained in step 2 2 Add 12.18g of terephthaloyl chloride to the solution system to obtain the raw material solution system, and carry out the first step of co-polycondensation reaction; the time of the first step of co-polycondensation reaction is 40min;

[0038] Step 4. When colloids appear in the solution of the first step co-condensation reaction in step 3, the reaction temperature is raised to 75° C. to carry out the second step co-polycondensation reaction to obtain a par...

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Abstract

The invention discloses a method for preparing HMW (High Molecular Weight) p-aramid polymer through ternary co-condensation. The method comprises the following steps: 1, preparing an NMP (N-Methyl Pyrrolidone)-CaCl2 solvent system; 2, cooling the NMP-CaCl2 solvent system, and adding 3,4'-diaminodiphenyl ether and p-phenylenediamine under the protection of nitrogen, thus obtaining a p-phenylenediamine-NMP-CaCl2 solution system; 3, adding p-phthaloyl chloride in the p-phenylenediamine-NMP-CaCl2 solution system, thus obtaining a raw material solution system; carrying out first-step copolycondensation; 4, after colloid appears in a solution of the first-step copolycondensation, rising the reaction temperature, and carrying out second-step copolycondensation, thus obtaining the p-aramid polymer. According to the method disclosed by the invention, a two-step copolycondensation reaction method which is carried out at a high temperature after a low temperature is adopted, ordered proceeding ofreaction is ensured, increment of side effects is avoided, and the intrinsic viscosity of the obtained p-aramid polymer in a dissolved state is 1.95 to 2.13 dL / g.

Description

technical field [0001] The invention belongs to the technical field of aramid fiber preparation, and in particular relates to a method for preparing high-molecular-weight p-aramid polymer through ternary co-condensation polymerization. Background technique [0002] Poly-p-phenylene terephthalamide (PPTA) fiber, also known as para-aramid, is an aromatic polyamide fiber made from aromatic compounds through polycondensation and spinning. It has excellent mechanical properties, stable With chemical properties and ideal mechanical properties, it is widely used in fields such as textiles, aerospace and national defense. [0003] The molecular chain of PPTA is composed of benzene ring and strong polar amide bond. It has high rigidity and strong hydrogen bonding between molecular chains. The molecular chains are tightly packed and highly crystallized, resulting in a high melting point of PPTA, and it is stable in general organic solvents. insoluble. At present, the preparation pro...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G69/32D01F6/80
CPCC08G69/32D01F6/805
Inventor 张华东吴晓妮张玮张晓利张力赵杨锋陈黎辛昭马少波王罡
Owner THE NORTHWEST RES INST OF CHEM IND
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