Preparation method of lignin-based carbon nanofiber

A carbon nanofiber, lignin-based technology, applied in the chemical characteristics of fibers, textiles and papermaking, etc., can solve the problems of low CNF preparation efficiency, and achieve the effect of improving melting resistance and improving preparation efficiency.

Active Publication Date: 2015-09-30
NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, this would result in extremely inefficient preparation of CNFs

Method used

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  • Preparation method of lignin-based carbon nanofiber
  • Preparation method of lignin-based carbon nanofiber

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Embodiment 1

[0028] In this embodiment, the preparation method of lignin-based carbon nanofibers comprises the following steps:

[0029] (1) Add dimethyl sulfoxide, lignin and acryloyl chloride sequentially in the reactor at a weight ratio of 100:30:30, stir the esterification reaction at 25°C for 1 hour, and add a small amount of triethylamine (TEA) after the reaction is completed Neutralize the HCl produced by the esterification reaction, then add ether to precipitate the modified lignin, then filter, wash with absolute ethanol several times, remove TEA hydrochloride, and obtain esterified lignin modified with acryloyl chloride;

[0030] (2) Add dimethylformamide, acryloyl chloride-modified esterified lignin, acrylonitrile, azobisiso Butyronitrile, carry out the homogeneous solution free radical copolymerization reaction at 60°C under the protection of nitrogen for 20 hours, remove the unreacted acrylonitrile monomer in the polymerization solution under vacuum after the reaction, and the...

Embodiment 2

[0036] In this embodiment, the preparation method of lignin-based carbon nanofibers comprises the following steps:

[0037] (1) Add dimethyl sulfoxide, lignin and acryloyl chloride sequentially in the reactor at a weight ratio of 100:30:20, stir the esterification reaction at 35°C for 1 hour, and add a small amount of triethylamine (TEA) after the reaction is completed Neutralize the HCl produced by the esterification reaction, then add ether to precipitate the modified lignin, then filter, wash with absolute ethanol several times, remove TEA hydrochloride, and obtain esterified lignin modified with acryloyl chloride;

[0038] (2) Add dimethyl sulfoxide, acryloyl chloride-modified esterified lignin, acrylonitrile, azobisiso Butyronitrile, under the protection of nitrogen, carry out homogeneous solution free radical copolymerization reaction at 65 ℃ for 18 hours, after the reaction is finished, remove the unreacted acrylonitrile monomer in the polymerization solution under vacu...

Embodiment 3

[0043] In this embodiment, the preparation method of lignin-based carbon nanofibers comprises the following steps:

[0044] (1) Add dimethyl sulfoxide, unmodified lignin and acryloyl chloride sequentially in the reactor at a weight ratio of 100:30:10, stir the esterification reaction at 25°C for 4 hours, and add a small amount of triethylamine after the reaction (TEA) to neutralize the HCl produced by the esterification reaction, then add ether to precipitate the modified lignin, then filter and wash with absolute ethanol several times to remove TEA hydrochloride to obtain esterified lignin modified with acryloyl chloride white;

[0045] (2) Add dimethylformamide, acryloyl chloride-modified esterified lignin, acrylonitrile, azobisiso Valeronitrile, carry out homogeneous solution free radical copolymerization reaction at 65°C under nitrogen protection for 20 hours, remove unreacted acrylonitrile monomer in the polymerization solution under vacuum after the reaction, and then s...

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Abstract

The invention provides a preparation method of lignin-based carbon nanofiber. According to the preparation method, electrostatic spinning technology is adopted; a copolymer of lignin and acrylonitrile is adopted as a spinning solution to prepare fiber; the fiber is subjected to thermal stabilizing treatment and carbonizing treatment to be prepared into carbon fiber. Acrylonitrile chain segments are grafted on lignin molecules, chemical bonds are generated between lignin and acrylonitrile chain segments, and the melting resistance of fiber in the thermal stabilizing treatment process is improved by using the fact that acrylonitrile chain segments are good in heat stability, so that melting and merging between fibers are avoided, the heating rate in thermal stabilizing treatment can be improved to 10-50 DEG C/min or above, and the preparation efficiency is effectively improved.

Description

technical field [0001] The invention belongs to the technical field of carbon fiber preparation, and in particular relates to a preparation method of lignin-based carbon nanofibers. Background technique [0002] Carbon nanofiber (carbon nanofiber, CNF) is a new type of carbon material with a diameter between carbon nanotubes and conventional carbon fibers, which has excellent physical, mechanical, electrical and chemical properties, such as high specific surface area, high strength and good Conductivity, thermal stability and chemical stability have important application value in structural and functional composite materials, electrode materials, energy storage materials, filter materials, adsorbents, catalysts and other fields. [0003] There are two main methods for preparing CNFs: chemical vapor deposition and electrospinning. The former obtains CNFs through the pyrolysis reaction of hydrocarbons on the surface of metal catalysts. This method has realized the commercial...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D01F9/17C08F289/00C08H7/00
Inventor 欧阳琴夏克强汪绪兰陈友汜王雪飞杨建行
Owner NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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