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Complex salt and method for preparing high-molecular-weight poly-p-phenylenepyridino-bisiminazole (PIPD) from same

A high molecular weight, phenylene pyridine technology, applied in the preparation of carboxylates, organic chemistry, etc., can solve the problems of low polymer molecular weight, low reaction efficiency, easy oxidation of TD salt, etc., and achieve high polymer molecular weight, simple operation, The effect of short reaction times

Active Publication Date: 2014-09-24
NANJING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0012] The purpose of the present invention is to solve the problems that the TD salt prepared by the TD salt method is easy to oxidize, the reaction efficiency is low, and the molecular weight of the polymer is low.

Method used

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  • Complex salt and method for preparing high-molecular-weight poly-p-phenylenepyridino-bisiminazole (PIPD) from same
  • Complex salt and method for preparing high-molecular-weight poly-p-phenylenepyridino-bisiminazole (PIPD) from same
  • Complex salt and method for preparing high-molecular-weight poly-p-phenylenepyridino-bisiminazole (PIPD) from same

Examples

Experimental program
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Effect test

Embodiment 1

[0037] A kind of preparation method of high molecular weight poly-p-phenylenepyridobisimidazole adopts following steps to prepare:

[0038] 1. Under a nitrogen atmosphere, add 19.8g (0.1mol) of 2,5-dihydroxyterephthalic acid into deoxygenated water and stir evenly, then add 0.3L (0.5mol / L) of sodium hydroxide solution and heat to Stir at 50-90°C to continue the reaction; make 13.325g (0.05mol) of 2,3,5,6-tetraaminopyridine hydrochloride into an aqueous solution, add 0.14g of stannous chloride, pour it into the reactor, and accelerate the stirring. Adjust the pH of the system to neutral, react in an ice bath for 0.5h, precipitate a yellow precipitate, filter the precipitate under a nitrogen atmosphere, wash the filter cake with deoxygenated water, freeze, and then place it in a freeze dryer to dry to obtain TD 2 Salt.

[0039] 2. Under the protection of nitrogen, add 125.2g of polyphosphoric acid with a mass percentage of 80% and 28.3g of phosphorus pentoxide to the reactor, s...

Embodiment 2

[0043] The specific method is the same as that in Example 1, except that in step 2, the reaction was carried out at 140° C. for 4 hours to obtain a poly-p-phenylenepyridobisimidazole polymer, and the measured relative viscosity was 13.41.

Embodiment 3

[0045] The specific method is the same as that in Example 1, except that in step 2, the reaction is carried out at 140° C. for 5 hours to obtain poly-p-phenylenepyridobisimidazole polymer, and the measured relative viscosity is 14.26.

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Abstract

The invention discloses a complex salt and a method for preparing high-molecular-weight poly-p-phenylenepyridino-bisiminazole (PIPD) from the same. The method solves the problems of low molecular weight, wide molecular weight distribution and low raw material utilization ratio in the PIPD prepared by the existing polymerization method. The method comprises the following steps: reacting raw materials 2,3,5,6-tetraaminopyridine (TAP) hydrochloride and excessive 2,5-dihydroxyterephthalic acid (DHTA) to obtain a stable complex salt (TD2 salt for short), and polymerizing in a polyphosphoric acid (PPA) system to obtain the PIPD polymer. The method solves the problem of high oxidation tendency of the obtained TD salt prepared from equal mole ratio of monomers by changing the raw material proportioning of the complex salt; and the method avoids waste of the raw materials due to the nonuniform stirring in the early reaction stage by changing the phosphorus pentoxide addition mode.

Description

technical field [0001] The invention belongs to the technical field of high-performance fiber preparation, and in particular relates to a complex salt and a method for preparing high-molecular-weight poly-p-phenylenepyridobisimidazole. Background technique [0002] PIPD is the abbreviation of polyphenylenepyridine bis-imidazole. It is a new type of high-performance fiber developed by Akzo Nobelcompany in the Netherlands. It is the product of molecular design by material scientists based on the relationship between structure and performance. The purpose is to solve the shortcomings of PBO and other fibers with low compression performance and poor bonding performance. [0003] PIPD has very excellent mechanical properties. Due to the special hydrogen bond network structure between the molecules along the radial direction of the fiber, PIPD fibers not only have excellent tensile properties similar to PBO fibers, but also show better compression resistance than PBO fibers. perf...

Claims

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Application Information

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IPC IPC(8): C07D213/73C07C65/05C07C51/41C08G73/06
CPCC07D213/73C08G73/0688
Inventor 邢晓东胡傲刘祖亮杜杨左彦胡小萍
Owner NANJING UNIV OF SCI & TECH
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