A kind of preparation method of nitrogen-doped lignin-based carbon fiber composite material

A technology of lignin-based and composite materials, which is applied in the field of preparation of lignin-based carbon fiber composite materials, can solve the problems of not being able to apply supercapacitors well, and achieve the effects of improving electrochemical performance, simple equipment, and strong operability

Active Publication Date: 2020-04-07
BEIJING FORESTRY UNIVERSITY
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  • Abstract
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Problems solved by technology

[0005] In the prior art, there are many methods for preparing lignin-based nanofibers by electrospinning technology, such as Chinese patents 201180026569.X, 201010104518.1 and 201710043185.4, etc., but these existing lignin nanofibers cannot For supercapacitor applications, further development of nanofibers with electrochemical properties such as higher specific capacitance is also required

Method used

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  • A kind of preparation method of nitrogen-doped lignin-based carbon fiber composite material
  • A kind of preparation method of nitrogen-doped lignin-based carbon fiber composite material
  • A kind of preparation method of nitrogen-doped lignin-based carbon fiber composite material

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Embodiment 2

[0037]At room temperature, dissolve 0.65g of PAN and 0.1g of LN in 5ml of DMF, stir fully on a magnetic stirrer until completely dissolved, add 0.08g of urea to the prepared polymer solution, continue stirring until completely dissolved, and obtain a spinning liquid. Use a 10ml syringe to extract the spinning solution, set the spinning voltage to 15kv, the receiving distance to 15cm, and the advancing rate to 0.5ml / h, and use tinfoil to collect the nanofiber precursor produced by high-voltage electrospinning, and dry it in the air for 12h. The dried nanofiber precursor is immersed in a solution of 0.1% aniline / hydrochloric acid (hydrochloric acid concentration is 1mol / L, 40ml) for 12h with a weight percentage concentration, and then 40ml hydrochloric acid (1mol / L ) solution, and keep the temperature at 0-4°C for 4h. The obtained nanofibers were washed several times with deionized water, dried in a drying oven at 60 °C for 12 h, and then pre-oxidized in a tube furnace at 260 °...

Embodiment 3

[0043] Except that the pre-oxidized fibers were calcined under an inert nitrogen atmosphere in a tube furnace, the heating rate was 5°C / h, the calcining temperature was 900°C, and the calcining time was 2h, to obtain LCNFs / PANI / N-9 carbon fibers, the rest Same as Example 2.

[0044] Electrochemical performance test: In 1mol / l sulfuric acid electrolyte, the current density is 1A / g, and the specific capacitance of LCNFs / PANI / N-9 carbon fiber is 199.5F / g.

[0045] figure 1 It is a scanning electron micrograph of the carbon fiber prepared according to this embodiment. It can be seen from the figure that the size of the carbon nanofiber is relatively uniform, and PANI is compounded on the surface. figure 2 a is the transmission electron micrograph of the carbon fiber prepared according to the present embodiment, figure 2 b is a distribution diagram of the diameters of carbon fibers prepared according to this embodiment.

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Abstract

The invention discloses a preparation method of a nitrogen-doped lignin-based carbon fiber composite material. The preparation method comprises the following steps: (1) dissolving a polymer into an organic solvent, and then adding urea to prepare a spinning solution; (2) preparing a nanofiber precursor through electrostatic spinning; (3) after the nanofiber precursor obtained in the step (2) is dried in air, immerging the dried nanofiber precursor into an aniline / hydrochloric acid solution, then dropwise adding a hydrochloric acid solution of ammonium persulfate, and carrying out heat preservation; (4) carrying out pre-oxidation; (5) carrying out calcination inside a tubular furnace so as to obtain nitrogen-doped lignin-based carbon fiber. Used alkali lignin is taken as a raw material, thesource is wide, and environmentally friendly, and the production cost is low. The used urea and polyaniline are taken as nitrogen sources, the nitrogen content of the carbon fiber is increased, and simultaneously the nitrogen distribution is uniform, so that the electrochemical performance of the carbon fiber can be improved effectively.

Description

technical field [0001] The invention belongs to the field of materials, and in particular relates to a preparation method and application of a nitrogen-doped lignin-based carbon fiber composite material. Background technique [0002] Supercapacitors, also known as electrochemical capacitors, are promising devices due to their high power density, fast charge / discharge rates, and excellent cycle life. According to their charge storage mechanism, supercapacitors are generally divided into two types: electric double layer capacitors, in which capacitance is generated by reversible ion adsorption / desorption on the electrode / electrolyte surface; and pseudocapacitors, in which Capacitance comes from reversible redox reactions. Most carbon materials, such as activated carbon, carbon nanofibers, carbon nanotubes, and graphene, usually have electric double layer capacitance. Whereas conductive polymers such as polyaniline and polypyrrole are commonly used as pseudocapacitors. Becau...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): D01F9/17D01F1/10H01G11/24H01G11/30H01G11/40H01G11/44D01D5/00
CPCD01D5/003D01D5/0092D01F1/10D01F9/17H01G11/24H01G11/30H01G11/40H01G11/44Y02E60/13
Inventor 马明国刘姗马畅李志文敬凡尘曹文涛王波
Owner BEIJING FORESTRY UNIVERSITY
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