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Naphthoxazine-based polymer and naphthoxazine-based porous carbon fiber, and preparation methods thereof

A technology of naphthoxazine-based and naphthoxazine-based acrylates is applied in the fields of naphthoxazine-based polymers and naphthoxazine-based porous carbon fibers and their preparation fields, and can solve the problem that thermoplastic phenolic resins are not easily cured, and thermosetting phenolic resins are difficult to cure. The problems of poor spinnability of resin and uneven pore size can achieve the effect of improving electrochemical performance, improving high curing temperature and uniform pore size distribution.

Active Publication Date: 2014-08-27
GUANGZHOU CHEM CO LTD CHINESE ACADEMY OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the above method has achieved certain results in the preparation of porous carbon nanofibers, there are still shortcomings such as uneven pore size and uneven distribution. Therefore, how to prepare porous carbon with uniform pore size and uniform distribution in electrospinning Nanofibers are still a problem we need to explore and address
[0003] Phenolic resin fiber is a kind of material that is very suitable as the substrate of activated carbon fiber. However, there are some problems in the preparation technology of phenolic-based electrospun carbon fiber, such as thermoplastic phenolic resin is not easy to cure, thermosetting phenolic resin has poor spinnability and carbon yield. inferior

Method used

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  • Naphthoxazine-based polymer and naphthoxazine-based porous carbon fiber, and preparation methods thereof
  • Naphthoxazine-based polymer and naphthoxazine-based porous carbon fiber, and preparation methods thereof
  • Naphthoxazine-based polymer and naphthoxazine-based porous carbon fiber, and preparation methods thereof

Examples

Experimental program
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Effect test

Embodiment 11

[0051] Under the condition of passing through the inert gas argon, 22.9g of naphthoxazine containing alcoholic hydroxyl group, 229ml of toluene and 10.1g of triethylamine were successively added to a 500ml four-necked flask with a condensing device and a stirring device, and the solution was completely dissolved. (stirring speed is 300r / min, stirring time is 20min) to obtain a mixed solution; after diluting 9.05g of acryloyl chloride with 9ml of toluene, slowly add it dropwise (dropping speed: 1 drop / second) to the mixing solution at 0°C In the solution, stir while adding dropwise and react for 6 hours (stirring speed is 300r / min), obtain the reaction product; The reaction product is extracted and washed with 5wt%NaOH solution until the water layer is colorless and transparent, then washed with distilled water to neutral , dried with anhydrous sodium sulfate, filtered to obtain an organic layer, and then the solvent was removed by rotary distillation to obtain a yellow liquid (...

Embodiment 12

[0054] Add the above 22.9g alcoholic hydroxyl-containing naphthoxazine, 115ml toluene and 10.1g triethylamine into a 500ml four-necked flask with a condensing device stirring device, stir and dissolve (the stirring speed is 400r / min, and the stirring time is 30min ), to obtain a mixed solution; after diluting 10.45g methacryloyl chloride with 5.23ml toluene, under ice bath (0°C), slowly add it dropwise (the drop rate is 1 drop / 3 seconds) into the mixed solution, while dropping Stirring and reacting for 24 hours to obtain the reaction product (stirring speed is 400r / min); the reaction product was extracted and washed with 5wt% NaOH solution until the water layer was colorless and transparent, washed with distilled water until neutral, and dried with anhydrous sodium sulfate , filtered to obtain an organic layer, and then the solvent was removed by rotary distillation to obtain a yellow liquid (ie, naphthoxazinyl acrylate).

[0055] At room temperature and under the condition of...

Embodiment 13

[0057] Under the condition of feeding inert gas nitrogen, 22.9g of alcoholic hydroxyl-containing naphthoxazine, 70ml of chloroform and 20g of triethylamine are added successively in a 500ml four-necked flask with a condensing device and a stirring device, and the dissolution is complete (stirring) The speed is 600r / min, the stirring time is 10min) to obtain a mixed solution; after diluting 10.45g of methacryloyl chloride with 5.23ml of toluene, slowly add it dropwise to the mixed solution at 5°C, the dropping speed is every 5 Drop 1 drop per second (that is, 1 drop / 5 seconds), and stir the reaction for 24 hours while adding dropwise (stirring speed is 600r / min). After the reaction is complete, directly extract and wash with 5wt% sodium bicarbonate solution until the water layer is colorless and transparent, then wash with distilled water until neutral, dry with anhydrous sodium sulfate, filter, and obtain the organic layer by rotary distillation to remove the solvent toluene. ...

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Abstract

The invention discloses a naphthoxazine-based polymer and a naphthoxazine-based porous carbon fiber and preparation methods thereof, belonging to the technical field of carbon fibers. According to the invention, naphthoxazine containing an alcoholic hydroxyl group reacts with an acyl chloride reagent under certain conditions so as to prepare naphthoxazine-based acrylate, and then under the action of an initiator, naphthoxazine-based acrylate undergoes polymerization so as to obtain the naphthoxazine-based polymer; the polymer, a pore forming agent and a solvent are mixed, and static spinning is carried out so as to prepare naphthoxazine-based protofilament; and the protofilament is subjected to curing at a constant temperature of 160 to 250 DEG C for 2 to 5 h, then to carbonization at a constant temperature of 600 to 1200 DEG C for 60 to 200 min and finally cooled to room temperature so as to obtain the naphthoxazine-based porous carbon fiber. The carbon fiber prepared in the invention has the advantages of a high carbon yield ratio, low shrinkage, simple carbonization, a hierarchical pore structure and uniform particle size distribution and can be used in the field of energy storage electrode materials.

Description

technical field [0001] The invention belongs to the technical field of carbon fibers, and in particular relates to a naphthoxazine-based polymer, a naphthoxazine-based porous carbon fiber and a preparation method thereof. Background technique [0002] Porous carbon fiber is a kind of carbon fiber material developed by chemical or physical activation method on the basis of traditional carbon fiber. Compared with traditional carbon fiber, porous carbon fiber has a super high specific surface area, which can generally reach 800-1500m 2 / g, the highest specific surface area is even as high as 3000m 2 / g or more, it can be used as a very ideal carrier material for adsorption materials, catalyst supports, energy storage materials, supercapacitors and electrode materials, etc. At present, the main precursor raw materials generally include viscose, polyacrylonitrile, pitch, polyimide fiber and phenolic resin. Electrospinning is one of the simplest processes for preparing nano-sca...

Claims

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Application Information

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IPC IPC(8): C08F120/36D01F9/21D01F6/52D01D5/00D01F11/06C07D265/14
Inventor 许凯林伟鸿付子恩辛明亮彭军邢玉秀陈鸣才
Owner GUANGZHOU CHEM CO LTD CHINESE ACADEMY OF SCI
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