Polyacrylonitrile mesopore-macropore ultrafine carbon fiber and its preparation method

A technology of polyacrylonitrile-based mesoporous and ultra-fine carbon fibers, which is applied in the fields of fiber chemical characteristics, chemical instruments and methods, and other chemical processes. It can solve the problems that fibers do not have a porous structure, and achieve large specific surface area and small fiber diameter. , easy to adjust the effect

Inactive Publication Date: 2006-12-27
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Korean patent KR2002008227 provides a method for manufacturing carbon nanofibers for supercapacitors by high-voltage electrospinning, but the fibers do no

Method used

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  • Polyacrylonitrile mesopore-macropore ultrafine carbon fiber and its preparation method
  • Polyacrylonitrile mesopore-macropore ultrafine carbon fiber and its preparation method
  • Polyacrylonitrile mesopore-macropore ultrafine carbon fiber and its preparation method

Examples

Experimental program
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Example Embodiment

[0020] Example 1

[0021] 4 grams of polyacrylonitrile and 6 grams of acrylonitrile-methyl methacrylate copolymer with a composition ratio of 1:9 are dissolved in 250 grams of dimethylformamide solution using high-voltage electrostatic spinning to obtain ultra-fine fibers, fiber mats or no Spinning cloth. The spinning voltage is at 30,000 volts, and the spinning speed is at 0.5 ml / h. The distance between the spinneret and the receiver is 15 cm. The obtained electrospun fiber see figure 1 , The diameter of the fiber is about 100 to 500 nanometers. The fiber mat obtained by electrospinning was vacuum dried at 80°C, and then pre-oxidized at 280°C for 2 hours, and then slowly heated to 800°C under the protection of nitrogen, and kept for 1 hour, with a nitrogen flow rate of 10 ml / min. Among them, the pyrolyzable polymer is completely decomposed to obtain mesoporous-macroporous ultrafine carbon fiber, such as figure 2 As shown, the diameter of the carbon fiber is below 500 nanometers...

Example Embodiment

[0022] Example 2

[0023] 2 grams of polyacrylonitrile and 8 grams of acrylonitrile-methyl methacrylate-polystyrene copolymer with a composition ratio of 1:8.5:0.5 are dissolved in 250 grams of dimethyl sulfoxide solution, and the fiber is obtained by high-voltage electrostatic spinning felt. The spinning voltage is 30,000 volts, and the spinning speed is 2 ml / h. The distance between the spinneret and the receiver is 15 cm. The drying and pre-oxidation are the same as in Example 1, the carbonization temperature is 700°C, and the time is 2 hours. After carbonization, the fibers are obviously porous, and there is adhesion between each other (see image 3 Shown). Its specific surface area is 92 square meters / g measured by nitrogen adsorption method. The obtained mesoporous-macroporous ultrafine carbon fiber was activated with carbon dioxide at 800°C, and the specific surface area was measured by nitrogen adsorption method to be 245 square meters / g.

Example Embodiment

[0024] Example 3

[0025] 5 grams of polyacrylonitrile and 5 grams of acrylonitrile-methyl methacrylate-butyl methacrylate terpolymer with a composition ratio of 1:8:1 were dissolved in 250 grams of dimethylacetamide solution and used high-voltage electrostatic Spinning to obtain fiber mat. The spinning voltage is 20,000 volts, and the spinning speed is 5 ml / h. The distance between the spinneret and the receiver is 15 cm. The drying and pre-oxidation are the same as in Example 1, the carbonization temperature is 1000° C., and the time is 2 hours. The diameter of the fiber is 5 microns. The fiber contains a large number of micropores, the diameter of which is about 100 nanometers. Its specific surface area is 54 square meters / g measured by nitrogen adsorption method.

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Abstract

The invention discloses a making method of polyacrylonitile hole-large hole ultra-fine carbon fiber, which comprises the following steps: dissolving polymerization to decompose completely under non-oxidizing environment through heat and polyacrylonitile or polyacrylonitile copolymer in the solvent; preparing super-fine fiber through high-pressure electrostatic spinning method; drying fiber; preoxidizing at 100-300 deg.c; carbonizing at 300-1800 deg.c in the nitrogen or other inert gas environment; decomposing heat-decomposable polymerization to remain 1-200 nanometer millipore in the fiber; fitting for certain large-size particle adsorption and separation (such as virus, bacteria and so on).

Description

technical field [0001] The invention relates to ultrafine carbon fibers with mesoporous or macroporous structures and a preparation method thereof, in particular to a polyacrylonitrile-based mesoporous or macroporous ultrafine carbon fiber and a preparation method thereof, Background technique [0002] Porous carbon fiber has important application value in material adsorption, separation, catalyst carrier, hydrogen storage material, special activated carbon for supercapacitor, etc. Pore ​​size and distribution have a decisive influence on the properties of porous carbon fibers. At present, the method of preparing porous carbon fiber is mainly to carbonize the organic polymer fiber obtained by solution spinning or melt spinning at high temperature, then activate it with water vapor, carbon monoxide, carbon dioxide and other atmospheres at high temperature, and various small molecule additives Such as metal ions, phosphoric acid (CN00117577.7), boric acid (CN99116239.0), etc....

Claims

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Application Information

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IPC IPC(8): D01F9/22B01J20/20B01D71/02
Inventor 彭懋沈烈李大松陈颖
Owner ZHEJIANG UNIV
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