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Copolyaramide containing phthalazine biphenyl structure and its preparation method

A technology of naphthone biphenyl and copolyaramide is applied in the synthesis field of copolyaramide, which can solve the problems of solution direct spinning and PPTA inability, and achieve the effects of easy purification, good solubility, and simple and feasible synthesis process.

Inactive Publication Date: 2004-07-21
DALIAN UNIV OF TECH +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0013] The purpose of the present invention is to provide a preparation method of polyarylamide containing phthalazinone biphenyl structure based on molecular structure design. The glass transition temperature of the obtained polymer can be as high as 334°C, which can meet the requirements of high temperature resistance The demand for long-term use, and the solubility of the polymer has also been significantly improved, which solves the problem that PPTA cannot be directly spun by solution

Method used

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  • Copolyaramide containing phthalazine biphenyl structure and its preparation method
  • Copolyaramide containing phthalazine biphenyl structure and its preparation method
  • Copolyaramide containing phthalazine biphenyl structure and its preparation method

Examples

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Embodiment 1

[0030] In a three-necked flask equipped with a stirrer, a reflux condenser, a thermometer, and a nitrogen inlet and outlet, under nitrogen protection, 1.5768 grams of 1,2-dihydro-2-(4-aminophenyl)-4-[4 -(4-aminophenoxy)-phenyl]-phthalazin-1-one, 1.1262 grams of 4,4'-diaminodiphenyl ether, 1.014 grams of p-phenylenediamine, a total of 18.75mmol and equivalent Terephthalic acid 3.1149g (18.75mmol), anhydrous lithium chloride 6.48g, triphenyl phosphite (TPP) 15ml, pyridine (PY) 18ml, N-methylpyrrolidone (NMP) 48ml, under nitrogen protection in After reacting at 110°C for 30 minutes, the viscosity of the reaction system increased significantly. After reacting for 6 hours, the reaction mixture was poured into 400ml of ethanol and water (1:1) to settle under vigorous stirring to obtain a white flocculent copolymer, which was filtered and washed thoroughly with hot water, and the polymer was vacuum-dried at 120°C After 24 hours, a pure copolyaramid resin was obtained. Its intrinsic...

Embodiment 2

[0032]In a three-necked flask equipped with a stirrer, a reflux condenser, a thermometer, and a nitrogen inlet and outlet, under the protection of nitrogen, add 0.3 g of lithium chloride and 1.14 ml of pyridine. When the salt is completely dissolved, add 0.6728 g of 1,2-bis Hydrogen-2-(4-aminophenyl)-4-[4-(4-aminophenoxy)-phenyl]-phthalazin-1-one, 0.3204 g 4,4'-diaminodiphenyl Ether, 0.5190 grams of p-phenylenediamine, add 0.8161 grams of terephthaloyl dichloride while stirring, after 10 minutes of reaction, add the remaining 0.8162 grams of terephthaloyl dichloride, accelerate stirring, keep the reaction temperature at 20 °C under normal pressure, and react The reaction stopped after 6 hours. The reaction mixture was poured into 400ml of ethanol and water (1:1) to settle under vigorous stirring to obtain a white flocculent polymer, which was filtered and washed thoroughly with hot water, and the polymer was vacuum-dried at 120°C for 24 hours to obtain pure Copolyaramid resin...

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Abstract

A refractory and soluble copolyarylamide is prepared from the moldifier which is the mixture of a novel diamine and the diamine H2N-Ar-X-Ar-NH2, and poly-p-phenyl diformyl p-pheyldiamine (PPTA) through directly condensation or low-temp solution polymerizing in the solution of the salt of alkali metal or alkali-earth metal. Its advantages are high vitrification temp and inherent viscosity, and better solubility, mechanical performance and thermal stability.

Description

technical field [0001] The invention belongs to the technical field of polymer materials, and relates to the synthesis of polymer compounds, in particular to the synthesis of a copolyarylamide containing a phthalazinone biphenyl structure. Background technique [0002] At present, all-aromatic polyamide resin is an important class of high-performance engineering plastics, among which polyparaphenylene terephthalamide (PPTA) is the most eye-catching one, and it can be made by spinning concentrated sulfuric acid solution. It is one of the organic fibers with the highest strength and the largest modulus. In 1972, DuPont realized its industrial production under the trade name of Kevlar. The commercialized Kevlar grades include Kevlar-29, Kevlar-49, and Kevlar-149. U.S. Patent USP 3673143 reports that PPTA is synthesized by polycondensation, and its basic reaction is: [0003] [0004] It has the advantages of high strength and high modulus, but there are some deficiencies i...

Claims

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Application Information

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IPC IPC(8): C08G69/32
Inventor 蹇锡高张元红刘鹏涛李杨洪定一吕占霞
Owner DALIAN UNIV OF TECH
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