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Preparation method for poly(2,5-dihydroxyl-1,4-phenylene pyridobisimidazole)

A technology of phenylene pyridine and hydroxyterephthalic acid, which is applied in the direction of one-component synthetic polymer rayon, textile and papermaking, fiber chemical characteristics, etc. and other problems, to achieve the effect of reducing the preparation cost, being easy to operate, and improving the method

Active Publication Date: 2013-07-31
NANJING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method aims at the difficulty that the amino group is easily oxidized during the polymerization process and cannot maintain the equimolar ratio reaction in the whole process, and solves the problems of low molecular weight and harsh polymerization conditions obtained by the existing method

Method used

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  • Preparation method for poly(2,5-dihydroxyl-1,4-phenylene pyridobisimidazole)
  • Preparation method for poly(2,5-dihydroxyl-1,4-phenylene pyridobisimidazole)

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] (1) Under the protection of nitrogen, add 5.2g DHTA to the TD salt reactor, add 50ml nitrogen deoxygenated water, stir and disperse evenly; make 3.15g NaOH into 10~30% aqueous solution and add it to DHTA, add 0.026g SnCl 2 , heated to 50°C under stirring; 7.0gTAP·3HCl·H 2 O (i.e. the salt of TAP

[0030] acid salt) to make an 18~20% aqueous solution, and add the TAP aqueous solution to the DHTA sodium salt, react at 50°C for 30 minutes, adjust the pH value to neutral with deoxyacetic acid, and precipitate a large amount of yellow precipitate. Filtered under water and washed three times with deoxygenated water and deoxyethanol respectively, blown dry with nitrogen, then transferred the obtained TD salt into a vacuum oven, and dried at 50°C and 50mbar for 24h to obtain TD salt.

[0031] (2) Add 19.2g polyphosphoric acid (PPA), 8.9g phosphorus pentoxide (P 2 o 5 ), 0.007g tin powder, 7.0gTD salt. Stir slowly to gradually disperse into the solvent. After stirring evenly...

Embodiment 2

[0033] Same as Example 1, change the reaction temperature in step (1) to 60°C, add 0.035g TAP hydrochloride, the relative viscosity of the polymer measured at 25°C and 0.25g / dl methanesulfonic acid is 22.8.

Embodiment 3

[0035] Same as Example 1, change the reaction temperature in step (1) to 60°C, add 0.070g TAP hydrochloride to obtain poly(2,5-dihydroxy-1,4-phenylenepyridodiimidazole), at 25°C, The relative viscosity measured at 0.25g / dl methanesulfonic acid is 24.2.

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Abstract

The invention relates to a preparation method for poly(2,5-dihydroxyl-1,4-phenylene pyridobisimidazole). The preparation method is realized by the following synthetic method: 2,3,5,6-tetraminopyridine (TAP) hydrochloride and 2,5-dihydroxyl-terephthalic acid (DHTA) are used as raw materials to carry out salificaton by an acid-base neutralization reaction so as to obtain 2,3,5,6-tetraminopyridine-2,5-dihydroxyl-terephthalate composite salt (TD salt); then high molecular weight PIPD fibers are prepared by temperature programmed solution polymerization in a polyphosphoric acid (PPA) system. The method solves the problems of low molecular weight and harsh polymerization conditions of a conventional method, aiming at the difficulties that amino groups are easily oxidized and equimolar ratio reaction can be kept in a whole process. The TD salt obtained by the process for synthesizing the 2,5-dihydroxyl-terephthalc acid-2,3,5,6-tetraminopyridine (TD) composite salt is stable in quality and easy to store; the polymerization reaction combines the advantages of a direct method and a TD salt method, so that the PIPD polymer with higher molecular weight is obtained without changing polymerization environment and polymerization equipment.

Description

technical field [0001] The invention belongs to the field of polymer material preparation, in particular to a method for preparing a novel rigid rod-shaped high-performance fiber poly(2,5-dihydroxy-1,4-phenylenepyridodiimidazole) (PIPD, trade name M5) . Background technique [0002] The chemical structural formula of poly(2,5-dihydroxy-1,4-phenylenepyridodiimidazole) is as follows: [0003] [0004] Akzo Nobel Institute has developed a new type of rigid rod polymer poly(2,5-dihydroxy-1,4-phenylenepyridodiimidazole) (PIPD), the polymer fiber has high strength, high modulus, Excellent compression and twisting performance, in addition to very good heat resistance, flame retardancy, dielectric, bonding and other properties, it is a high-performance fiber with superior comprehensive properties. [0005] Two kinds of methods for preparing PIPD are proposed in US 5674969 and EP 0696297B1: the first is 2,5-dihydroxyterephthalic acid (abbreviated as DHTA) and 2,3,5,6-tetraaminop...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/06D01F6/74
Inventor 刑晓东刘祖亮杜杨范海涛胡傲
Owner NANJING UNIV OF SCI & TECH
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