PPTA containing 2,4 di (4-amino phenyl)-2,3-diaza naphthalene-1-one and preparation process thereof

A manufacturing method, the technology of poly-p-phenylene terephthalamide, which is applied in the polymerization of para-polyarylamide and the synthesis of high polymers, can solve the problems of insoluble and infusible PPTA resin, resistance to strong acid corrosion, and processing difficulties and other problems, to achieve the effect of good solubility, good electrical insulation performance, and simple synthesis process

Inactive Publication Date: 2009-11-04
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] However, PPTA resin is insoluble and infusible, liquid crystal spinning must be carried out in concentrated sulfuric acid, the process is complicated, the equipment requires resistance to strong acid corrosion, and processing is relatively difficult

Method used

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  • PPTA containing 2,4 di (4-amino phenyl)-2,3-diaza naphthalene-1-one and preparation process thereof
  • PPTA containing 2,4 di (4-amino phenyl)-2,3-diaza naphthalene-1-one and preparation process thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Add 100ml NMP to a 250ml three-necked flask, N 2 protection, stirring, adding a certain amount of CaCl 2 , slowly warming up to 70°C, after completely dissolving, cooling to room temperature, adding 3.078 grams of p-phenylenediamine and 0.492 grams of 2,4-bis(4-aminophenyl)-2,3-naphthyridine-1-one , when all the materials are dissolved, cool to -5°C, add 6.090 grams of terephthaloyl chloride, accelerate stirring until rod climbing occurs, react for 30 minutes, add 2.22 grams of Ca(OH) 2 Neutralize for 20 minutes to obtain a co-polycondensation PPTA solution. The prepared solution was thoroughly washed with water and dried to obtain a new type of PPTA resin, whose characteristic viscosity measured in 98% concentrated sulfuric acid was 3.2. The PPTA can be dissolved into NMP, or solution-spun.

Embodiment 2

[0017] Add 100ml NMP to a 250ml three-necked flask, N 2 protection, stirring, adding a certain amount of CaCl 2 , slowly heat up to 70°C, dissolve, cool to room temperature, add 3.888 grams of p-phenylenediamine, wait until the material is completely dissolved, cool to -5°C, add 8.12 grams of terephthaloyl chloride, react for 10 minutes, and synthesize a certain degree of polymerization For oligomers, add 1.312 grams of 2,4-bis(4-aminophenyl)-2,3-naphthyridine-1-one, after dissolving, add 1 gram of terephthaloyl dichloride, and accelerate stirring until pole climbing occurs Phenomenon, react for 30 minutes, add 2.96 grams of Ca(OH) 2 Neutralize for 20 minutes to obtain a PPTA co-condensation solution. The prepared solution is thoroughly washed with water and dried to obtain a novel PPTA resin whose characteristic viscosity is 2.8 as measured in 98% concentrated sulfuric acid. The PPTA can be dissolved into NMP, or solution-spun.

[0018] The structure of the polymer is con...

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Abstract

The invention discloses a PPTA containing 2,4-bis(4-aminophenyl)-2,3-naphthyridine-1-one and a manufacturing method thereof, comprising the following steps: under the protection of an inert gas, Add solvent to the polymerization reactor, stir, add alkali metal halides to the polymerization system for solubilization, and then add 2,4-bis(4-aminophenyl)-2,3-phthalazin-1-one and p-phenylenediamine; after dissolving, add terephthaloyl chloride with an equimolar concentration of 0.3-0.4mol / l, accelerate stirring, keep the reaction temperature at -10-80°C, and react for 30-120 minutes. Calcium hydroxide in an equimolar amount of phthaloyl chloride is neutralized to obtain a co-polycondensation PPTA solution. The synthesis process is simple and easy, the cost is low, and it is easy to purify, and can be widely used in aerospace, high-performance composite materials, high-temperature resistant films and the preparation of corresponding fabrics.

Description

technical field [0001] The invention belongs to the field of polymer material science and technology, and relates to the synthesis of polymers, in particular to para-position polymers containing 2,4-bis(4-aminophenyl)-2,3-naphthyridine-1-one structure. Polymerization of arylamides (PPTA). Background technique [0002] Para-aramid fiber, that is, poly (para-phenyleneterephthalamide), PPTA for short, is also called aramid fiber 1414 in my country. Due to the high symmetry, regularity and rigid structure of the molecular chain, PPTA has excellent mechanical properties such as high strength and high modulus, low density, high dimensional stability, high temperature resistance, and good affinity with rubber. [0003] However, PPTA resin is insoluble and infusible, and liquid crystal spinning must be carried out in concentrated sulfuric acid. The process is complicated, and the equipment is required to be resistant to strong acid corrosion, so the processing is relatively difficu...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G69/14C08K3/16
Inventor 李丛杰李国伟刘兆峰胡盼盼
Owner DONGHUA UNIV
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