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Preparation method of high-modulus poly (p-phenylene benzobisoxazole) fiber

A technology of benzobisoxazole and poly-p-phenylene, which is applied in the field of preparation of high-modulus poly-p-phenylene benzobisoxazole fiber, can solve the problem of low orientation degree of PBO fiber core layer, increase of fiber orientation degree and strength , poor flexibility and other issues, to achieve the effect of compact structure, increased orientation and strength, and favorable movement and closed loop

Pending Publication Date: 2022-03-04
SHANDONG NON METALLIC MATERIAL RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Aiming at the technical problems existing at present, the present invention provides a preparation method of high modulus poly-p-phenylene benzobisoxazole fiber, which introduces carbon nanotubes into the PBO prepolymer solution, and solves the problem of orientation of the PBO fiber core layer. problems of low density and poor flexibility; at the same time, the existence of carbon nanotubes, its plasticizing effect is conducive to the movement and closed loop of molecular chains at high temperatures, and the modulus of primary PBO fibers increases during the heat setting process, while the orientation of the fibers The strength and strength have also increased substantially

Method used

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  • Preparation method of high-modulus poly (p-phenylene benzobisoxazole) fiber

Examples

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Effect test

Embodiment 1

[0029] Add carbon nanotubes in the beaker that fills (volume concentration) 45% sulfuric acid aqueous solution, the addition of carbon nanotubes is 4wt% of 45% sulfuric acid aqueous solution, then beaker is placed in the oil bath of 50 ℃, to the inside of beaker The solution was continuously stirred for 2 hours, and the sulfuric acid solution was removed by centrifugation with a high-speed centrifuge, the centrifuge speed was 7000r / min, and the time was 15min. The remaining carbon nanotubes were repeatedly washed with deionized water until neutral, and then the obtained carbon nanotubes The tubes were dried in a vacuum oven at 80° C. for 9 hours to obtain carboxylated carbon nanotubes. The carbon nanotubes can also be oxidized with bromine water and dilute nitric acid.

[0030] The carboxylated carbon nanotubes in the following examples all adopt the carboxylated carbon nanotubes prepared in Example 1;

Embodiment 2

[0032] A kind of preparation method of high modulus poly-p-phenylene benzobisoxazole fiber, specifically comprises the steps:

[0033] (1) Add 10.048Kg of polyphosphoric acid solvent to a polymerization reactor with nitrogen gas, add 4.98g of carboxylated carbon nanotubes to the polyphosphoric acid solution, stir at 40°C for 3h, and then add 2.18Kg 4,6-diaminoresorcinol hydrochloride (DAR HCl), 3.861Kg phosphorus pentoxide (P 2 o 5 ), vacuumize the reaction kettle, supplement nitrogen three times, start the stirring reaction for 5h, then add 1.699Kg terephthalic acid (TPA), stir, and when the temperature of the system reaches 135°C, the prepolymerization is completed to obtain the PBO prepolymer solution. The intrinsic viscosity of PBO prepolymer solution is 0.78dl / g;

[0034](2) Transport the PBO prepolymer solution to the twin-screw extruder through the pipeline, and fill it with nitrogen for protection. The PBO prepolymer solution is highly polymerized in the twin-screw e...

Embodiment 3

[0039] A kind of preparation method of high modulus poly-p-phenylene benzobisoxazole fiber, specifically comprises the steps:

[0040] (1) Add 10.048Kg of polyphosphoric acid solvent to a polymerization reactor with nitrogen gas, add 9.96g of carboxylated carbon nanotubes to the polyphosphoric acid solution, stir at 40°C for 2 hours, and then add 2.18Kg 4,6-diaminoresorcinol hydrochloride (DAR HCl), 3.861Kg phosphorus pentoxide (P 2 o 5 ), vacuumize the reactor, replenish nitrogen three times, start stirring and reacting for 5 hours, then add 1.699Kg terephthalic acid (TPA), stir, and when the temperature of the system reaches 135°C, the prepolymerization is completed, and the PBO prepolymer solution is inherently viscous The number is 0.66dl / g;

[0041] (2) Transport the PBO prepolymer solution to the twin-screw extruder through the pipeline, and fill it with nitrogen for protection. The PBO prepolymer solution is highly polymerized in the twin-screw extruder to obtain the ...

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Abstract

The invention belongs to the field of high-performance fibers, and particularly relates to a preparation method of a high-modulus poly (p-phenylene benzobisoxazole) fiber, which comprises the following steps: firstly preparing a PBO prepolymer solution, and then polymerizing and spinning to obtain a PBO fiber, the step of preparing the PBO prepolymer solution is as follows: adding a polyphosphoric acid solvent under the condition of nitrogen, and stirring to obtain the PBO fiber. The preparation method comprises the following steps: firstly, oxidizing carbon nanotubes, then adding the oxidized carbon nanotubes into a polyphosphoric acid solution, stirring and dispersing uniformly, then adding phosphorus pentoxide and 4, 6-diamino resorcinol hydrochloride, stirring, then adding terephthalic acid, stirring, heating to 120-150 DEG C, completing prepolymerization to obtain a PBO prepolymer solution, and the solid content of the prepolymer in the PBO prepolymer solution is 13-18%. The tensile breaking strength of the prepared high-modulus PBO fiber is 6.0 to 6.8 GPa, and the tensile modulus of the prepared high-modulus PBO fiber is 280 to 320 GPa.

Description

technical field [0001] The invention belongs to the field of high-performance fibers, and in particular relates to a preparation method of high-modulus poly-p-phenylenebenzobisoxazole fibers. Background technique [0002] Poly-p-phenylenebenzobisoxazole (PBO) fiber is currently the organic reinforcing fiber material with the best comprehensive properties. It is widely used in lightweight composite materials because of its high modulus, high strength and high temperature resistance. , body armor, armor protection and other fields, and also has broad application development prospects in the aerospace field. In the late 1990s, Japan's Toyobo Corporation (Toyobo) announced that it had obtained high-performance PBO fibers with a trade name of Zylon, and applied Zylon to high-tech fields such as aerospace and national defense. my country's research on PBO fiber started late, and foreign countries keep technology secret to my country. Although my country has made some progress in...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D01F6/94D01F1/10
CPCD01F6/94D01F1/10
Inventor 钟蔚华刘宗法朱晓琳刘群孟昭瑞代勇刘薇陈湘栋郭程张殿波
Owner SHANDONG NON METALLIC MATERIAL RES INST
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