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Poly(p-phenylene benzobisoxazole) fiber containing fluorine on surface and preparation method thereof

A benzobisoxazole and poly-p-phenylene technology is applied in the field of poly-p-phenylene benzobisoxazole fiber and its preparation, and can solve the problem of polymer macromolecular chain breakage, high fluorination rate, and corrosion of fluorination equipment and other problems, to achieve the effect of reducing the decline of mechanical strength, improving the shear strength between layers, and improving the interfacial interaction.

Active Publication Date: 2017-04-12
SICHUAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the surface activity and shear bonding strength of the material surface after oxyfluorination treatment are obviously improved, but because there is a certain amount of water in the air, the hydrogen fluoride produced during the fluorination process will combine with water to damage the fluorination equipment. cause severe corrosion
In order to solve these problems, CN101798748B adopts oxygen-free fluorination, although problems such as equipment corrosion can be overcome, because there is no oxygen in the fluorine gas mixture, the inhibitory effect of oxygen on the fluorination reaction rate disappears, thereby causing the fluorination rate to be too high and It is difficult to control the uniformity and repeatability of the chemical composition of the fiber surface
In addition, it has been disclosed in literature that C=N in polymers is easily oxidized by strong oxidants (Liao J H, Li Q F, Rudbeck H C, et al. Oxidative degradation of polybenzimidazole membranes as electrolytes for high temperature proton exchange membrane fuel cells[J].Fuel Cells, 2011,11(6):745-755.)
Since the macromolecular chain of PBO fiber contains a large number of C=N bonds, and fluorine gas is a strong oxidizing agent, both pure fluorination and oxygen fluorination can easily cause the polymer macromolecular chain to break and affect the fiber itself. The mechanical properties of the surface, and the decrease of the mechanical properties of the surface of the fiber itself will cause the interface between it and the composite material prepared by the resin to appear as a weak interface, which is not conducive to the improvement of the performance of the composite material

Method used

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  • Poly(p-phenylene benzobisoxazole) fiber containing fluorine on surface and preparation method thereof
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  • Poly(p-phenylene benzobisoxazole) fiber containing fluorine on surface and preparation method thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] First place the poly-p-phenylene benzobisoxazole fiber body in a closed vacuum reactor, then evacuate, and replace the air in the reactor with nitrogen three times, then fill the vacuum reactor with hydrogen fluoride gas, and treat for 3 Minutes, then fill the vacuum reactor with fluorine / oxygen / nitrogen mixed gas, control the partial pressure of hydrogen fluoride in the reactor to 1KPa, the partial pressure of fluorine to 10KPa, the partial pressure of oxygen to 1KPa, and the partial pressure of nitrogen to 50KPa, and heat up The fluorination treatment was carried out at 25°C for 20 minutes, and finally the poly(p-phenylenebenzobisoxazole) fiber was stored in air atmosphere for at least 1 hour.

[0034] Add the obtained fluorine-containing PBO fiber into the epoxy resin matrix to prepare the corresponding composite material. The relevant properties of the obtained composite material are shown in the attached table.

Embodiment 2

[0036] First place the poly-p-phenylene benzobisoxazole fiber body in a closed vacuum reactor, then evacuate, and replace the air in the reactor with nitrogen three times, then fill the vacuum reactor with hydrogen fluoride gas, and treat for 5 Minutes, then fill the vacuum reactor with fluorine / oxygen / argon mixed gas, control the partial pressure of hydrogen fluoride in the reactor to 4KPa, the partial pressure of fluorine to 60KPa, the partial pressure of oxygen to 6KPa, and the partial pressure of argon to 240KPa, The temperature was raised to 50° C. for fluorination treatment for 5 minutes, and finally the poly(p-phenylenebenzobisoxazole) fiber was stored in air atmosphere for at least 1 hour.

[0037] Add the obtained fluorine-containing PBO fiber into the epoxy resin matrix to prepare the corresponding composite material. The relevant properties of the obtained composite material are shown in the attached table.

Embodiment 3

[0039] First place the poly-p-phenylene benzobisoxazole fiber body in a closed vacuum reactor, then evacuate, and replace the air in the reactor with nitrogen three times, then fill the vacuum reactor with hydrogen fluoride gas for 10 Minutes, then fill the vacuum reactor with fluorine / oxygen / helium mixed gas, control the partial pressure of hydrogen fluoride in the reactor to 0.01KPa, the partial pressure of fluorine to 0.5KPa, the partial pressure of oxygen to 0.05KPa, and the partial pressure of helium to The pressure is 5KPa, and the temperature is raised to 100°C for fluorination treatment for 2 hours, and finally the poly(p-phenylenebenzobisoxazole) fiber is stored in the air atmosphere for at least 1 hour.

[0040] Add the obtained fluorine-containing PBO fiber into the epoxy resin matrix to prepare the corresponding composite material. The relevant properties of the obtained composite material are shown in the attached table.

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Abstract

The invention discloses a polyparaphenylene benzo dioxazole fiber containing fluorine on surface, which is prepared through the following steps: the body of the polyparaphenylene benzo dioxazole fiber is treated by using a hydrogen fluoride gas, then is mixed by using fluorine / oxygen / inert gas, is subjected to fluoridation for 10 seconds to 2 hours at 5-150 DEG C, and finally is stored in air atmosphere for at least one hour. A contact angle between the surface of the obtained fiber and water is 60-90 degrees, the interlaminar shear strength of a composite material prepared from the fiber and epoxy resin is 30-45MPa, the tensile strength of an impregnated filament is 5.0-5.3GPa, and the tensile modulus is 264-280GPa. The polyparaphenylene benzo dioxazole fiber containing fluorine on surface is high in surface activity, interfacial interaction between the fiber and matrix resin is strong, the interlaminar shear strength of the composite material prepared by using the fiber can be improved by 50-125%, the tensile strength of the impregnated filament is improved by 4-10%, and the modulus is improved by 10-16%. According to the invention, the fluorination rate is high, the treatment time is short, the process is simple and controllable, the cost is relatively low, and the fiber has relatively strong application prospect.

Description

technical field [0001] The invention belongs to the technical field of poly-p-phenylene benzobisoxazole (PBO) fiber and its preparation, and in particular relates to a surface fluorine-containing poly-p-phenylene benzobisoxazole (PBO) fiber and a preparation method thereof. Background technique [0002] Compared with aircraft parts manufactured by traditional metal materials and methods, the integrated design and manufacture of fiber-reinforced resin-based composite materials can not only reduce the weight of aircraft parts by 20-30%, but also reduce the use and maintenance costs by 15-25% compared with metal materials. , so it has been widely used in aerospace field. It is understood that the amount of resin-based composite materials used in aircraft has reached more than 50% of its structural weight. [0003] Although fiber-reinforced resin-based composites have been widely used in the aerospace field due to their light weight, their mechanical properties cannot fully mee...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): D06M11/11D06M11/09C08L63/00D06M101/30
Inventor 刘向阳罗龙波吴鹏黄杰阳李保印刘洋
Owner SICHUAN UNIV