Nitrogen-doped aramid-based enhanced multistage hole carbon fiber preparation method

A technology of nitrogen doping and carbon fiber, which is applied in the fields of fiber chemical characteristics, rayon manufacturing, textiles and paper making, etc. It can solve the problems of unsatisfactory mechanical strength and achieve the goal of improving electromagnetic wave adsorption performance, strong controllability and improving mechanical strength. Effect

Inactive Publication Date: 2018-08-14
DONGGUAN LIANZHOU INTPROP OPERATION MANAGEMENT CO LTD
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  • Application Information

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Problems solved by technology

Chinese patent CN 10276278A discloses a method for preparing porous carbon nanofibers containing metal oxides, porous carbon nanofibers prepared by this method, and carbon nanofiber products containing it. The carbon nanofiber precursor solution containing metal alkoxide is passed through After electrospinning, place it in a hot air circulation furnace for treatment, and heat and carbonize in an inert or vacuum atmosphere to obtain metal oxide porous carbon fibers. The preparation method is simple and the cost is low. The metal oxide porous carbon fibers prepared by this method have Large specific surface area and good electrical conductivity, good pore size distribution, can be used for electromagnetic wave shielding materials, but the mechanical strength is not ideal, so how to improve the mechanical properties of porous carbon fibers is very necessary

Method used

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  • Nitrogen-doped aramid-based enhanced multistage hole carbon fiber preparation method

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Experimental program
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Effect test

Embodiment 1

[0024] (1) Add ferric citrate to Kevlar's aramid pulp and mix it evenly to form a spinning solution, where the content of metal citrate in the spinning solution is 1wt%, and the spinning solution is transferred to the static In the injector of the spinning device, the spinning voltage is 20kV, the inner diameter of the spinneret is 0.5mm, the flow rate of the spinning solution is 0.1mL / h, the spinning distance is 10cm, the collecting roller speed is 5m / min, and the spinneret is transverse. The moving speed is 10cm / min, and the aramid fiber containing metal citrate is formed by electrostatic spinning.

[0025] (2) Put the as-spun aramid fiber containing citrate metal salt in an oxygen atmosphere, perform pre-oxidation treatment at 220°C for 5 minutes, and place it in an atmosphere containing 50% ammonia gas, and carbonize it at 1000°C for 10 minutes , To obtain nitrogen-doped aramid-based porous carbon fiber.

[0026] (3) According to the solid-liquid ratio of 1g:25mL, the nitrogen...

Embodiment 2

[0028] (1) Add nickel citrate, copper citrate and zinc citrate with a mass ratio of 1:1:1 to Kevlar’s ​​aramid pulp, and mix them evenly to form a spinning solution. Among them, the spinning solution The content of metal citrate is 10wt%. The spinning solution is transferred to the syringe of the electrospinning device. The spinning voltage is 30kV, the spinneret inner diameter is 0.8mm, and the spinning solution flow rate is 0.6mL / h. The silk distance is 15cm, the speed of the collecting roller is 8m / min, the spinneret's lateral movement speed is 25cm / min, and the aramid fiber containing citrate metal salt is prepared by electrostatic spinning.

[0029] (2) Put the as-spun aramid fiber containing citrate metal salt in an oxygen atmosphere, perform a pre-oxidation treatment at 300°C for 10 minutes, place it in an atmosphere containing 80% ammonia, and carbonize it at 1500°C for 30 minutes , To obtain nitrogen-doped aramid-based porous carbon fiber.

[0030] (3) According to the so...

Embodiment 3

[0032] (1) Add aluminum citrate, sodium citrate and potassium citrate with a mass ratio of 1:1:1 to Kevlar's aramid pulp, and mix them evenly to form a spinning solution. Among them, the spinning solution The content of citrate metal salt is 5wt%, and the spinning solution is transferred to the syringe of the electrostatic spinning device. The spinning voltage is 25kV, the spinneret inner diameter is 0.6mm, and the spinning solution flow rate is 0.3mL / h. The silk distance is 12cm, the speed of the collecting roller is 6m / min, the spinneret's lateral movement speed is 15cm / min, and the aramid fiber containing citrate metal salt is prepared by electrostatic spinning.

[0033] (2) Put the as-spun aramid fiber containing citrate metal salt in an oxygen atmosphere, perform a pre-oxidation treatment at 2500°C for 6 minutes, place it in an atmosphere containing 60% ammonia, and carbonize it at 1400°C for 20 minutes , To obtain nitrogen-doped aramid-based porous carbon fiber.

[0034] (3)...

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Abstract

The invention provides a nitrogen-doped aramid-based enhanced multistage hole carbon fiber preparation method. The preparation method comprises the following steps: adding metal salt of citric acid inaramid pulp, uniformly mixing the materials to prepare spinning liquid, and performing static spinning to prepare aramid as-spun fiber containing the metal salt of citric acid; placing the aramid as-spun fiber containing the metal salt of citric acid in oxygen atmosphere, performing pre-oxidation treatment, placing the material in ammonia gas-containing atmosphere for carbonization treatment to obtain the nitrogen-doped aramid-based porous carbon fiber; dipping the nitrogen-doped aramid-based porous carbon fiber in the diluted aramid pulp, taking the material out, and drying the material to obtain the nitrogen-doped aramid-based enhanced multistage hole carbon fiber. The porous carbon material takes the aramid pulp and the metal salt of citric acid as carbon source, the as-spun fiber is prepared through static spinning, the nitrogen-doped aramid-based porous carbon fiber is prepared through pre-oxidation and carbonization treatment, and then is enhanced by the aramid pulp to obtain the product, the product has multiple holes, and the electromagnetic adsorptivity is strong.

Description

Technical field [0001] The invention belongs to the technical field of textile materials, and in particular relates to a method for preparing nitrogen-doped aramid-based reinforced multi-level porous carbon fiber. Background technique [0002] Absorbing material refers to a type of material that attenuates or eliminates electromagnetic interference generated by the external environment through absorption, interference and scattering. It uses the effects of dielectric oscillation, eddy current and magnetostriction of the absorber to convert the electromagnetic energy of the external environment The heat is consumed. According to the molding process, the absorbing materials can be divided into two categories: coating type and structure type. The coating type absorbing material is made of absorbing agent and solvent and coated on the surface of the target. The manufacturing process is simple and convenient. However, the density is large, not uniform enough, the frequency of absorbi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D01F9/30D01F1/10
CPCD01F1/10D01F9/30
Inventor 陈东进
Owner DONGGUAN LIANZHOU INTPROP OPERATION MANAGEMENT CO LTD
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