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Preparation of a nano-carbon fiber with high specific surface area

A nano-carbon fiber, high specific surface area technology, applied in the direction of fiber chemical characteristics, conjugated synthetic polymer rayon, textiles and papermaking, etc., can solve problems such as corrosion, low efficiency, pore structure, etc., to achieve good dispersion, The effect of simple process and controllable conditions

Active Publication Date: 2018-07-06
TIANJIN POLYTECHNIC UNIV
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Problems solved by technology

[0004] The structural characteristics of carbon nanofibers determine its performance to a large extent. Porous carbon nanofibers with high specific surface area, high pore volume and suitable pore size show excellent performance in all aspects. The activation method is currently the most commonly used method. A method to increase the specific surface area of ​​carbon materials, but the activation method generally has defects such as complicated process, high production cost, difficult control, and pore structure.
For example chemical activation method generally adopts KOH or NaOH as activator, and Chinese patent document CN 1807235A (application number: 200610038065.0) discloses a kind of preparation method of phenolic resin base high specific surface area active carbon, after pulverizing phenolic resin and curing agent and mixing it in The activator KOH or NaOH is mixed, and the mass ratio of the activator to the phenolic resin can reach up to 7:1. The high content of strong alkali will not only cause a certain degree of corrosion to the equipment, but also affect the subsequent treatment of the product due to the introduction of potassium ions or sodium ions. Bringing challenges, the Chinese literature patent CN 101700885A (application number 200910219704.7) discloses a method for preparing activated carbon with a high specific surface area. Although the carbon-base ratio is reduced, the activation gas H 2 or H 2 With inert gas, it not only increases the cost but also brings certain dangers Compared with the chemical activation method, although the physical activation method is environmentally friendly, it often requires a longer cycle, and the defects of high energy consumption and low efficiency greatly increase the production cost. Chinese document patent CN101397136A (application number 200810233530.5) discloses a method for preparing granular activated carbon with high specific surface area by physical activation method. The introduction of microwave radiation device in this method shortens the carbonization time to a certain extent, but the introduction of new device will also increase the cost
Chinese patent document CN102627276A (application number 201210079041.5) discloses a method for preparing activated carbon from fruit shells by pyrolysis activation method and activated carbon. This method does not require activated gas to directly pyrolyze activated carbon in one step, but there is still the problem that the carbonization time is too long. Therefore, It is necessary to find a simpler and more effective method to increase the specific surface area of ​​carbon materials As a method that can effectively control the pore structure, template method plays an important role in the research of porous carbon materials. product of

Method used

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  • Preparation of a nano-carbon fiber with high specific surface area
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  • Preparation of a nano-carbon fiber with high specific surface area

Examples

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Effect test

Embodiment 1

[0035] Phenol, formaldehyde solution and catalyst NH 3 ·H 2 O mixed, the molar ratio of phenol and aldehyde is: 1:0.5, adjust the pH to 9, raise the temperature to 70°C, and keep the temperature for 80min; after the reaction, cool the product to room temperature, adjust the pH to neutral with HCl solution, and The product is subjected to vacuum distillation to remove the moisture in the product, and the obtained phenolic resin is formulated into a 20% ethanol solution;

[0036] Mix 5g of methyl orthosilicate and 95g of absolute ethanol, add 2g of HCl solution (2moL / L), and stir for 2h in a water bath at 40°C. Then add 50 g of phenolic resin ethanol solution (20 wt %), and continue to stir for 2 h. Then add 50g of PVP ethanol solution (20wt%) and stir for 2h to obtain a uniformly mixed spinning dope. The spinning parameters are: the dope flow rate is 3ml / h, the applied voltage is 20Kv, and the spinning distance is 20cm. Put the obtained as-spun fibers in the air for 24 hours...

Embodiment 2

[0038] Dissolve resorcinol and acetaldehyde in the catalyst NsOH, the molar ratio of phenol and aldehyde is: 1:0.8, adjust the pH to 12, raise the temperature to 70°C, and keep the temperature constant for 60 minutes; after the reaction, cool the product to room temperature and wash it with HCl solution The pH was adjusted to neutral, the product was distilled under reduced pressure at 60° C. to remove the moisture in the product, and the obtained phenolic resin was formulated into a 40% ethanol solution.

[0039]Mix 10 g of ethyl orthosilicate and 90 g of absolute ethanol, and add 3 g of HCl to dissolve (2moL / L). Stir in a water bath at 40°C for 3h. Then add 25g phenolic resin ethanol solution (40wt%), continue to stir for 2h and then add 50g polyvinyl acetal ethanol solution (30wt%), stir for 2h, obtain the spinning stock solution that mixes, spinning parameter is: stock solution flow rate is 3ml / h, the applied voltage is 20Kv, the spinning distance is 20cm, the obtained a...

Embodiment 3

[0042] Phloroglucinol, furfural dissolved in catalyst Na 2 CO 3 , the molar ratio of phenol and aldehyde is: 1:0.8, adjust the pH to 10, raise the temperature to 70°C, and keep the temperature constant for 70min; after the reaction, cool the product to room temperature, adjust the pH to neutral with HCl solution, and test the product at 55°C The moisture in the product was removed by distillation under reduced pressure, and the obtained phenolic resin was formulated into a 30% ethanol solution.

[0043] Mix 20g of propyl orthosilicate and 80g of absolute ethanol, and add 4g of HCl to dissolve (2moL / L), and stir for 4h in a water bath at 40°C. Then add 33g phenolic resin ethanol solution (30wt%), continue to stir for 2h, then add 50gPVP ethanol solution (40wt%), stir for 2h, obtain the spinning dope that mixes homogeneously, spinning parameter is: dope flow velocity is 3ml / h, apply The voltage is 20Kv, and the spinning distance is 20cm. The obtained as-spun fiber was left to...

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Abstract

The invention discloses a preparation method of nano-carbon fiber with high specific surface area. The method uses the resol resin with low molecular weight as a carbon precursor, uses the polymer with high molecular weight as a spinning auxiliary agent, and obtains a spinning dope by adding organic matter containing silicon into a stock solution. The as-spun fibre having nanoscale is prepared by electrospinning technique, and the porous nano-carbon fibre having high specific surface area is prepared by the processes such as solidification, carbonization, and acid pickling. The method can adjust and control the specific surface area of the nano-carbon fibre by controlling the addition of the pore forming agent, and has advantages such as simple technology and strong operability.

Description

Technical field: [0001] The invention relates to a preparation method of nano carbon fiber, in particular to a preparation method of nano carbon fiber with high specific surface area. Background technique [0002] Carbon materials are widely used in energy storage, industrial catalysis and other fields due to their low price, stable physical and chemical properties, and different morphologies. Especially in recent years, the discovery of new carbon materials such as carbon nanotubes, fullerenes, and graphene has made people's research on carbon materials continue to deepen. It can be expected that new carbon materials will be a research hotspot in the field of new materials in the future. [0003] As a new type of carbon material, carbon nanofiber has many advantages. It not only has the inherent characteristics of traditional carbon fiber, such as good thermal conductivity and corrosion resistance, but also has the advantages of small size effect and large specific surface ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): D01F9/24D01F9/21D01F9/20D01F8/16D01F8/10
CPCD01F8/10D01F8/16D01F9/20D01F9/21D01F9/24
Inventor 马昌盛杰王冉冉谢震宇张海霞史景利
Owner TIANJIN POLYTECHNIC UNIV