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High-performance fiber and preparation method thereof

A technology of fiber modification, applied in the field of high-performance fiber and its preparation, can solve the problems of reducing the thermal performance and deficiency of fiber, and achieve the effect of enhancing the compression resistance and the force between fiber molecules

Active Publication Date: 2017-02-22
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, although the strength of the force between the polar groups is higher than that of the van der Waals force, it is still insufficient for the application of PBO fibers.
Moreover, the introduction of hydroxyl groups will also greatly reduce the thermal properties of the fibers, which is unfavorable for the application of fibers at high temperatures.

Method used

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  • High-performance fiber and preparation method thereof
  • High-performance fiber and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] (1) In a three-necked flask equipped with a condensation and stirring device, add 0.5mol of dimethyl 2-hydroxyterephthalate and 1.1mol of paraformaldehyde, then add 80ml of solvent dimethylformamide, and heat to 70 ℃, after the reagents are fully mixed and dissolved, add 0.5 mol of aniline, raise the temperature to 100 ℃, and react for 10 hours. The system is precipitated, washed and dried to obtain dimethyl terephthalate containing oxazine side groups. Under stirring, add 100 ml of methanol solution containing 1 mol of potassium hydroxide, heat to reflux for 7 hours, add dilute hydrochloric acid to acidify, and dry to obtain terephthalic acid containing oxazine side groups.

[0049] (2) In the reaction kettle equipped with nitrogen protection and stirring device, add 0.2mol of 4,6-diaminoresorcinol hydrochloride, 0.16mol of terephthalic acid, 0.04mol of p- Phthalic acid, 100g polyphosphoric acid (P 2 o 5 Concentration is 83wt%), 80g P 2 o 5 . Wherein, the molar r...

Embodiment 2

[0057] The molar ratio of terephthalic acid to terephthalic acid containing oxazine side groups in Example 1 was changed to n:m=95:5. That is, 31.54g (0.18mol) of terephthalic acid and 2.99g (0.02mol) of terephthalic acid containing oxazine side groups. Other steps are the same as in Example 1.

[0058] The molecular structure of modified PBO in the present embodiment is:

[0059]

[0060] The tensile strength of the modified PBO fiber obtained in this example is 5.2 GPa, the thermal decomposition temperature in air is 575° C., and the compressive strength is 0.9 GPa.

Embodiment 3

[0062] The aniline in Example 2 is changed to p-cyanoaniline, and the feeding amount is changed accordingly. Other operating steps are the same as those in Example 1.

[0063] The molecular structure of modified PBO in the present embodiment is:

[0064]

[0065] The tensile strength of the modified PBO fiber obtained in this example is 5.1 GPa, the thermal decomposition temperature in air is 571° C., and the compressive strength is 1.3 GPa.

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Abstract

The invention relates to a modified poly(p-phenylenebenzobisoxazole) (PBO) fiber and a preparation method thereof. According to the fiber, the main problem of poor pressure resistance of the PBO fiber is solved. The preparation method comprises the steps of reacting by virtue of 2-hydroxyl dimethyl terephthalate, an amine source and paraformaldehyde as raw materials so as to prepare terephthalic acid containing an oxazine side group, reacting by virtue of o-amino-phenol hydrochloride, terephthalic acid and terephthalic acid containing the oxazine side group as raw materials so as to prepare modified PBO containing the oxazine side group, carrying out dry-jet wet spinning method to an obtain original benzoxazine grafted modified PBO fiber, and carrying out thermal treatment and benzoxazine open loop crosslinking on the original benzoxazine grafted modified PBO fiber, so as to obtain the modified PBO fiber. The preparation method has the advantages that by introducing an oxazine structure to the side groups of PBO molecular chains, the tensile property of the fiber is hardly influenced; and oxazine is subjected to open loop crosslinking during the thermal treatment of the fiber, and the PBO molecular chains are chemically crosslinked, so that the pressure resistance of the fiber can be substantially improved.

Description

[0001] 【Technical field】 [0002] The invention relates to a high-performance fiber and a preparation method thereof, in particular to a benzoxazine graft-modified poly-p-phenylenebenzobisoxazole (PBO) fiber and a preparation method thereof. [0003] 【Background technique】 [0004] Poly-p-phenylenebenzobisoxazole (PBO) is a rigid rod-shaped molecule containing an oxazole ring structure, which is usually composed of 4,6-diaminoresorcinol hydrochloride (DAR) and terephthalic acid. The raw material is polycondensed in polyphosphoric acid (PPA). Using dry-jet wet spinning technology, high-performance PBO fibers can be obtained after spinning, coagulation, stretching, washing, drying, heat treatment and other processes. PBO fiber is currently the material with the highest tensile strength and tensile modulus among organic synthetic fibers, and it has good heat resistance, and its decomposition temperature under nitrogen is as high as 600°C. In addition, it has excellent chemical s...

Claims

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Application Information

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IPC IPC(8): C08G73/06D01F6/78
CPCC08G73/06D01F6/78
Inventor 刘小云张如红程鹏辉黄国瑞丁艳玲庄启昕
Owner EAST CHINA UNIV OF SCI & TECH
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