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A kind of ultra-fine size metal-pan-based carbon fiber and preparation method thereof

A technology based on carbon fiber and carbon fiber, applied in the field of ultra-fine size metal-PAN based carbon fiber and its preparation, can solve the problems of poor dispersion, difficulty in preparing metal particle size, affecting catalytic performance, etc.

Active Publication Date: 2021-07-06
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The patent (CN111005047A) discloses a method for preparing a uniform electroplated copper layer on carbon fibers. The preparation process uses electroplating technology to uniformly load micron-sized copper particles on the surface of carbon fibers, but the uniformity within the control range is poor and dense. high degree
Patent (CN110970628A) discloses a nano-carbon fiber and metal composite electrode and its application. The composite material is obtained by electrospinning in one step. Although the obtained metal nanoparticles are small in size (20nm), the particle dispersion is poor and cannot be controlled.
Therefore, the current problem in the preparation of metal / carbon fiber hybrid materials is that it is difficult to prepare metal / carbon fiber hybrid materials with small metal particle size, uniform size and uniform dispersion.
However, in the above studies, in order to increase the adsorption capacity of metal ions, as many amidoxime groups as possible were grafted on the surface of carbon materials to increase the adsorption sites of metal ions, so the distribution of metal ions was relatively dense. Agglomeration easily occurs during the preparation of metal elemental particles by ion reduction
In addition, in the process of reusing the adsorbed metal ions, the electric reduction or thermal reduction method with relatively extensive condition control is often used, and the obtained metal particles are mostly in the micron size, or obviously agglomerated, and the dispersion degree It is also poor, which greatly affects the catalytic performance

Method used

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  • A kind of ultra-fine size metal-pan-based carbon fiber and preparation method thereof

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Embodiment 1

[0050] A preparation method of ultra-fine size manganese nanoparticles-PAN-based carbon fiber, comprising the steps of:

[0051] (1) Soak the polyacrylonitrile fiber with a diameter of 100nm obtained by electrospinning in water, add hydroxylamine hydrochloride, adjust the pH value to 7 with sodium carbonate, and then heat to react (the temperature is 80°C, and the time is 60min), the reaction Finally, the fiber is rinsed and vacuum-dried (the temperature is 60° C.) to obtain amidoxime-modified polyacrylonitrile fibers; wherein, the mass ratio of polyacrylonitrile fibers to water is 1:750; the mass ratio of polyacrylonitrile fibers to hydroxylamine hydrochloride is 1:0.03;

[0052] (2) The polyacrylonitrile fiber that will make amidoxime modification is immersed in the continuous stirring (the rotating speed of magnetic stirring is 220rpm) containing manganese salt (MnCl 2 4H 2 (2) in aqueous solution, carry out self-assembly reaction (temperature is 180 ℃, time is 30min) in ...

Embodiment 2

[0056] A preparation method of ultra-fine size iron nanoparticles-PAN-based carbon fiber, comprising the steps of:

[0057] (1) Soak the polyacrylonitrile fibers with a diameter of 50nm obtained by electrospinning in water, add hydroxylamine hydrochloride, adjust the pH value to 8 with potassium hydroxide, and then heat to react (the temperature is 30°C, and the time is 180min). After the reaction, the polyacrylonitrile fiber was washed and vacuum-dried (at a temperature of 70°C) to obtain amidoxime-modified polyacrylonitrile fiber; wherein, the mass ratio of polyacrylonitrile fiber to water was 1:500; polyacrylonitrile fiber and The mass ratio of hydroxylamine hydrochloride is 1:0.05;

[0058] (2) The polyacrylonitrile fiber that the prepared amidoxime is modified is immersed in the continuous stirring (the rotating speed of magnetic stirring is 320rpm) containing iron salt (FeCl 3 ·6H 2 (2) in an aqueous solution, then carry out self-assembly in a hydrothermal kettle (the ...

Embodiment 3

[0062] A preparation method of ultra-fine size cobalt nanoparticles-PAN-based carbon fiber, comprising the steps of:

[0063] (1) Soak the polyacrylonitrile fiber with a diameter of 500nm obtained by electrospinning in water, add hydroxylamine hydrochloride, adjust the pH value to 9 with sodium hydroxide, then heat to react (the temperature is 80°C, and the time is 70min) and then , after the reaction, the product is separated, washed and vacuum-dried (at a temperature of 80° C.) to obtain amidoxime-modified polyacrylonitrile fibers; wherein, the mass ratio of polyacrylonitrile fibers to water is 1:250; PAN fibers and hydroxylamine hydrochloride The mass ratio is 1:0.05;

[0064] (2) Immerse the polyacrylonitrile fiber modified amidoxime made into the cobalt salt (CoCl 2 ·6H 2 (0) in aqueous solution, carry out self-assembly reaction (temperature is 120 ℃, time is 30min) in hydrothermal tank subsequently, after reaction finishes, product is separated and washed, wherein, the...

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Abstract

The invention relates to an ultra-fine size metal-PAN-based carbon fiber and a preparation method thereof. The preparation method is as follows: performing self-assembly reaction on amidoxime-modified polyacrylonitrile fiber and metal salt under hydrothermal conditions, and then calcining under reducing atmosphere , to obtain ultra-fine size metal-PAN-based carbon fibers; the prepared ultra-fine-sized metal-PAN-based carbon fibers are composed of PAN-based carbon fibers, carbon nanotubes and metal nanoparticles coated with graphite layers on the surface; carbon nanotubes are dispersed in PAN-based carbon fibers The surface of the carbon nanotubes, and the carbon nanotubes are interlaced to form a nano-mesoscopic pore structure; the metal nanoparticles coated with the graphite layer are confined to the ends of the carbon nanotubes, and the metal nanoparticles are in a monodisperse state and are evenly dispersed. The size is uniform, and the average particle size is 5-20nm. The ultra-fine size metal-PAN-based carbon fiber of the present invention has strong adsorption performance, and the confinement effect of the carbon nanotubes on the metal nanoparticles avoids the agglomeration between the metal nanoparticles.

Description

technical field [0001] The invention belongs to the technical field of inorganic nano synthesis, and relates to an ultrafine size metal-PAN-based carbon fiber and a preparation method thereof. Background technique [0002] Carbon fiber (carbon fiber) is generally converted from organic fibers through a series of heat treatments. It is a special fiber composed of carbon elements. Carbon fiber also takes into account the inherent advantages of carbon materials such as low density, light weight, good electrical conductivity, corrosion resistance, and good compatibility with other materials, as well as the good flexibility and designability of fiber materials. advantage. Therefore, carbon fiber is often regarded as an ideal carrier material and is widely used in the preparation of composite materials. [0003] Patent (CN109295442A) discloses a method for colloidal copper activated carbon fiber and one-step preparation of electroless copper-nickel double metal layer. The core s...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): D01F9/22
CPCD01F9/22
Inventor 杨建平陈俊良乌婧王华平马元元
Owner DONGHUA UNIV
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