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A kind of preparation method of poly-p-phenylene benzobisoxazole fiber

A technology of benzobisoxazole and polyparaphenylene, applied in fiber treatment, fiber chemical characteristics, dry spinning method, etc., can solve the problems of poor processing performance, difficult synthesis of PBO spinning system, good spinnability, etc. Achieve the effect of strong dissolving ability, recyclable solvent and good spinnability

Active Publication Date: 2021-07-27
SHANDONG NON METALLIC MATERIAL RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the new method of preparing PBO fibers by two-step dry spinning process provided by the present invention, the precursor PHA has strong solubility in common polar solvents such as DMAC and NMP, and has good spinnability, which solves the problem of traditional one-step PBO spinning system synthesis Difficult, poor processability issues

Method used

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  • A kind of preparation method of poly-p-phenylene benzobisoxazole fiber
  • A kind of preparation method of poly-p-phenylene benzobisoxazole fiber

Examples

Experimental program
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Effect test

Embodiment 1

[0037] A preparation method of poly-p-phenylene benzobisoxazole fiber, comprising the steps of:

[0038] (1) Add 2L of solvent DMAC to a polymerization kettle with nitrogen gas, add 179.4g of 4,6-diaminoresorcinol, stir for 30min, add 6.6g of catalyst isoquinoline, and add part of terephthaloyl dichloride 121.1g , add 1.65g of stannous chloride, stir for 30min, then add remaining 30.2g of terephthaloyl chloride, stir and react at 0°C for 24 hours to obtain the precursor PHA spinning solution;

[0039] (2) After the above PHA solution is filtered and degassed, it is extruded through a spinneret and then dry-spun. The hot air temperature in the spinning tunnel is 250°C, and the spinning air volume is 8m 3 / min, the line speed of the first roll is 500m / min, to obtain PHA as-spun fibers. The solvent volatilized during the fiber forming process is taken out by the hot air and then enters the solvent recovery device, where it is separated by multi-stage tray vacuum distillation to...

Embodiment 2

[0044] A preparation method of poly-p-phenylene benzobisoxazole fiber, comprising the steps of:

[0045] (1) In a nitrogen-filled polymerization kettle, add 2L solvent NMP, add 223.1g of 4,6-diaminoresorcinol, stir for 60min, add catalyst pyridine 0.41g, add part of terephthaloyl dichloride 150.4g, add 0.71g of stannous chloride, stirred for 30min, then added the remaining 37.6g of terephthaloyl chloride, stirred and reacted at 20°C for 24 hours, and the precursor PHA spinning solution was obtained;

[0046] (2) After the above PHA solution is filtered and degassed, it is extruded through a spinneret and then dry-spun. The hot air temperature in the spinning tunnel is 200°C, and the spinning air volume is 30m 3 / min, the line speed of the first roll is 800m / min, to get PHA as-spun fibers. The solvent volatilized during the fiber forming process is taken out by the hot air and then enters the solvent recovery device, where it is separated by multi-stage tray vacuum distillati...

Embodiment 3

[0051] A preparation method of poly-p-phenylene benzobisoxazole fiber, comprising the steps of:

[0052] (1) Add 2L of solvent DMAC to a polymerization kettle with nitrogen gas, add 338.8g of 4,6-diaminoresorcinol, stir for 50min, add 0.62g of catalyst isoquinoline, and add part of terephthaloyl dichloride 228.6g , add 12.4g of stannous chloride, stir for 30min, then add remaining 57.1g of terephthaloyl chloride, stir and react at 10°C for 24 hours to obtain the precursor PHA spinning solution;

[0053] (2) After the above PHA solution is filtered and degassed, it is extruded through a spinneret and then dry-spun. The hot air temperature in the spinning tunnel is 150°C, and the spinning air volume is 15m 3 / min, the line speed of the first roll is 1000m / min, to get PHA as-spun fibers. The solvent volatilized during the fiber forming process is taken out by the hot air and then enters the solvent recovery device, where it is separated by multi-stage tray vacuum distillation t...

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Abstract

The present invention belongs to the field of macromolecular materials, and in particular relates to a kind of polyhydroxyamide (PHA) as a precursor polymer, adopting dry spinning process to prepare PHA as-spun fibers, and then obtaining poly-p-phenylenebenzodiene through thermal cyclization A new approach to oxazole (PBO) fibers. In the new method of preparing PBO fibers by two-step dry spinning process provided by the present invention, the precursor PHA has strong solubility in common polar solvents such as DMAC and NMP, and has good spinnability, which solves the problem of traditional one-step PBO spinning system synthesis Difficult and poor processability. And the precursor PHA spinning system can adopt dry spinning, the spinning speed is greatly improved, the solvent can be recycled and reused, energy saving and environmental protection. In the subsequent PHA thermal cyclization process, the PBO fiber prepared by adopting the cyclization-drawing integration technology can form a better aggregated structure, and the fiber strength modulus is high.

Description

technical field [0001] The invention belongs to the field of polymer materials, and in particular relates to a preparation method of poly-p-phenylenebenzobisoxazole fibers. Background technique [0002] Poly-p-phenylenebenzobisoxazole (PBO) fiber is a high-performance aromatic heterocyclic fiber with high strength, high modulus, high temperature resistance, and high flame retardancy. Its comprehensive performance is the best among organic fibers, and it is known as For the super fiber of the 21st century. PBO fibers can be used in cutting-edge fields such as aerospace, weaponry, high-temperature filtration, and special protection. In the 1960s and 1970s, the Wright-Patteron Laboratory of the U.S. Air Force started the basic research on PBO fibers. In the 1990s, Dow Chemical Company cooperated with Japan Toyobo to develop PBO fibers. Subsequently, Toyobo succeeded in the pilot test and launched commercial products. Zylon. Afterwards, many countries in the world have carrie...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): D01F6/74D01F11/08C08G73/22D01D5/04D01D5/098
CPCC08G73/22D01D5/04D01D5/0985D01F6/74D01F11/08
Inventor 张殿波钟蔚华刘群朱晓琳张鹏虢忠仁陈湘栋张辉宫平曲志敏金子明
Owner SHANDONG NON METALLIC MATERIAL RES INST