CN110983494A - Preparation method of aramid-based carbon fiber - Google Patents
Preparation method of aramid-based carbon fiber Download PDFInfo
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- CN110983494A CN110983494A CN201911320046.0A CN201911320046A CN110983494A CN 110983494 A CN110983494 A CN 110983494A CN 201911320046 A CN201911320046 A CN 201911320046A CN 110983494 A CN110983494 A CN 110983494A
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- aramid
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
- D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
- D01F9/14—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments
- D01F9/20—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products
- D01F9/24—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products from macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D01F9/28—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products from macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds from polyamides
- D01F9/30—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products from macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds from polyamides from aromatic polyamides
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- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Artificial Filaments (AREA)
- Inorganic Fibers (AREA)
Abstract
The invention discloses a preparation method of aramid fiber-based carbon fiber, which comprises the steps of ultrasonically cleaning modified aramid fiber in a pretreating agent, washing the fiber by a stirring cleaning machine, fishing out the fiber, and drying by a low-temperature drying box to obtain modified aramid fiber as a spun fiber; and placing the modified aramid fiber spun fiber in an oxygen atmosphere, carrying out pre-oxidation treatment, and placing the fiber in an ammonia-containing atmosphere for carbonization treatment to obtain the nitrogen-doped aramid fiber-based carbon fiber. After the processing according to the steps of the method, compared with the traditional product, the finished product is greatly improved, the modified meta-aramid carbon fiber can enable meta-aramid insulating fiber with excellent performance to inhibit space charge accumulation, the prepared aramid-based carbon fiber has good flexibility and stable tensile strength, and the prepared multistage hole carbon fiber has high mechanical strength.
Description
Technical Field
The invention relates to the technical field of carbon fiber processing, in particular to a preparation method of aramid fiber-based carbon fiber.
Background
At present, carbon fiber is a new material with excellent mechanical properties. Its specific weight is less than 1/4 of steel, and is lighter than aluminium, and its specific strength is 20 times of iron, and compared with metal materials of titanium, steel and aluminium, the carbon fibre has the characteristics of large strength, high modulus, low density and small linear expansion coefficient, etc. in the aspect of physical property, it can be called "king of new material". Therefore, carbon fibers are widely used in military fields such as aircraft manufacturing, industrial fields such as wind power generation blades, and sports and leisure fields such as gold clubs.
In addition to the properties of a general carbon material: the carbon fiber reinforced epoxy resin composite material has the advantages of high temperature resistance, abrasion resistance, electric conduction, heat conduction, corrosion resistance and the like, has obvious anisotropy and softness in appearance, can be processed into various fabrics, shows high strength along the fiber axis direction due to small specific gravity, and has the highest comprehensive indexes of specific strength and specific modulus in the existing structural materials. At present, almost no other materials have a series of excellent performances like carbon fibers, so that the carbon fiber composite material has irreplaceable advantages in the fields with strict requirements on the stiffness, the rigidity, the gravity, the fatigue property and the like and in the occasions requiring high temperature and high chemical stability.
Accordingly, one skilled in the art provides a method for preparing an aramid-based carbon fiber to solve the problems set forth in the above background art.
Disclosure of Invention
The invention aims to provide a preparation method of aramid-based carbon fiber, which aims to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme:
a preparation method of aramid-based carbon fiber comprises the following steps:
1) mixing the meta-aramid chopped fiber and the meta-aramid fiber pulp, and preparing a mixed solution through dispersion, defibering and pulping;
2) mixing and defibering the mixed solution and a nano TiO2 deionized water solution, and pulping to prepare a nano TiO2 modified meta-aramid mixed solution;
3) adding a nano TiO2 modified meta-aramid mixed solution into a metal citrate, uniformly mixing to form a spinning solution, feeding the spinning solution into a water bath through a spinneret plate for solidification, stretching the spinning solution through a solvent to obtain fibers, washing the fibers with water, and performing dry heating to obtain modified aramid fibers;
4) ultrasonically cleaning modified aramid fibers in a pretreating agent, washing the fibers with water by using a stirring cleaning machine, fishing out the fibers, and drying the fibers by using a low-temperature drying box to obtain modified aramid fiber as a spun fiber;
5) and placing the modified aramid fiber spun fiber in an oxygen atmosphere, carrying out pre-oxidation treatment, and placing the fiber in an ammonia-containing atmosphere for carbonization treatment to obtain the nitrogen-doped aramid fiber-based carbon fiber.
As a further scheme of the invention: in the step 5), the meta-aramid fiber is stretched by a yarn guide machine, and is pre-oxidized in an oxygen atmosphere at the temperature of 250-350 ℃ for 3-10 min.
As a still further scheme of the invention: and in the step 7), stretching the meta-aramid precursor fiber treated in the step 6 by using a yarn guide machine, and simultaneously performing high-temperature carbonization on the meta-aramid precursor fiber in a nitrogen atmosphere at 1800 ℃ for 2-15 min.
Compared with the prior art, the invention has the beneficial effects that:
this modified meta-aramid carbon fiber can make itself just have excellent performance meta-aramid insulating fiber and can restrain space charge and gather, and the aramid base carbon fiber pliability that makes is good, and tensile strength is stable, and the mechanical strength of the multistage hole carbon fiber of making is high.
Detailed Description
The technical solution of the present invention will be described in further detail with reference to specific embodiments.
The first embodiment is as follows:
a preparation method of aramid-based carbon fiber comprises the following steps:
1) mixing the meta-aramid chopped fiber and the meta-aramid fiber pulp, and preparing a mixed solution through dispersion, defibering and pulping;
2) mixing and defibering the mixed solution and a nano TiO2 deionized water solution, and pulping to prepare a nano TiO2 modified meta-aramid mixed solution;
3) adding a nano TiO2 modified meta-aramid mixed solution into a metal citrate, uniformly mixing to form a spinning solution, feeding the spinning solution into a water bath through a spinneret plate for solidification, stretching the spinning solution through a solvent to obtain fibers, washing the fibers with water, and performing dry heating to obtain modified aramid fibers;
4) ultrasonically cleaning modified aramid fibers in a pretreating agent, washing the fibers with water by using a stirring cleaning machine, fishing out the fibers, and drying the fibers by using a low-temperature drying box to obtain modified aramid fiber as a spun fiber;
5) placing the modified aramid fiber spun fiber in an oxygen atmosphere, carrying out pre-oxidation treatment, and placing the fiber in an ammonia-containing atmosphere for carbonization treatment to obtain nitrogen-doped aramid fiber-based carbon fiber;
6) stretching the meta-aramid fiber by a yarn guide machine, and simultaneously pre-oxidizing the meta-aramid fiber in an oxygen atmosphere at the temperature of 250-350 ℃ for 3-10 min;
7) and (3) stretching the meta-aramid protofilament treated in the step (6) by using a filament guide machine, and simultaneously placing the meta-aramid protofilament in a nitrogen atmosphere with the temperature of 400-1800 ℃ for high-temperature carbonization for 2-15 min.
Example two:
a preparation method of aramid-based carbon fiber comprises the following steps:
1) mixing the meta-aramid chopped fiber and the meta-aramid fiber pulp, and preparing a mixed solution through dispersion, defibering and pulping;
2) mixing and defibering the mixed solution and a nano TiO2 deionized water solution, and pulping to prepare a nano TiO2 modified meta-aramid mixed solution;
3) adding a nano TiO2 modified meta-aramid mixed solution into a metal citrate, uniformly mixing to form a spinning solution, feeding the spinning solution into a water bath through a spinneret plate for solidification, stretching the spinning solution through a solvent to obtain fibers, washing the fibers with water, and performing dry heating to obtain modified aramid fibers;
4) ultrasonically cleaning modified aramid fibers in a pretreating agent, washing the fibers with water by using a stirring cleaning machine, fishing out the fibers, and drying the fibers by using a low-temperature drying box to obtain modified aramid fiber as a spun fiber;
5) placing the modified aramid fiber spun fiber in an oxygen atmosphere, carrying out pre-oxidation treatment, and placing the fiber in an ammonia-containing atmosphere for carbonization treatment to obtain nitrogen-doped aramid fiber-based carbon fiber;
6) stretching the meta-aramid fiber by a yarn guide machine, and simultaneously pre-oxidizing the meta-aramid fiber in an oxygen atmosphere of 200-380 ℃ for 5-15 min;
7) and (3) stretching the meta-aramid protofilament treated in the step (6) by using a filament guide machine, and simultaneously placing the meta-aramid protofilament in a nitrogen atmosphere with the temperature of 500-1700 ℃ for high-temperature carbonization for 5-15 min.
The working principle of the invention is as follows:
through a plurality of experiments, the nano TiO2 modified meta-aramid insulating fiber is found to be utilized, the meta-aramid insulating fiber with excellent performance can inhibit space charge accumulation, the insulating property and the mechanical property are excellent, the prepared aramid-based carbon fiber is suitable for a strong electric field environment, the flexibility is good, the carbon content is reasonable, the tensile strength is stable, and the carbonization yield is high.
While the preferred embodiments of the present invention have been described in detail, the present invention is not limited to the above embodiments, and various changes can be made without departing from the spirit of the present invention within the knowledge of those skilled in the art.
Claims (5)
1. The preparation method of the aramid-based carbon fiber is characterized by comprising the following steps of:
1) mixing the meta-aramid chopped fiber and the meta-aramid fiber pulp, and preparing a mixed solution through dispersion, defibering and pulping;
2) mixing and defibering the mixed solution and a nano TiO2 deionized water solution, and pulping to prepare a nano TiO2 modified meta-aramid mixed solution;
3) adding a nano TiO2 modified meta-aramid mixed solution into a metal citrate, uniformly mixing to form a spinning solution, feeding the spinning solution into a water bath through a spinneret plate for solidification, stretching the spinning solution through a solvent to obtain fibers, washing the fibers with water, and performing dry heating to obtain modified aramid fibers;
4) ultrasonically cleaning modified aramid fibers in a pretreating agent, washing the fibers with water by using a stirring cleaning machine, fishing out the fibers, and drying the fibers by using a low-temperature drying box to obtain modified aramid fiber as a spun fiber;
5) and placing the modified aramid fiber spun fiber in an oxygen atmosphere, carrying out pre-oxidation treatment, and placing the fiber in an ammonia-containing atmosphere for carbonization treatment to obtain the nitrogen-doped aramid fiber-based carbon fiber.
2. The method for preparing aramid-based carbon fiber as claimed in claim 1, wherein in the step 5), the meta-aramid fiber is stretched by a yarn guide machine, and is pre-oxidized in an oxygen atmosphere at 380 ℃ and 200 ℃ for 5-15 min.
3. The method for preparing aramid-based carbon fiber as claimed in claim 1, wherein in the step 7), the meta-aramid fiber precursor treated in the step 6 is stretched by a filament guide machine, and the meta-aramid fiber precursor is carbonized at high temperature in nitrogen atmosphere at 1800 ℃ and 400 ℃ for 2-15 min.
4. The method for preparing aramid-based carbon fiber according to claim 1, wherein in the step 5), the content of ammonia in the ammonia-containing atmosphere is not less than 50%.
5. The method for preparing aramid-based carbon fiber according to claim 1, wherein in the step 3), the solid content of the nano TiO2 modified meta-aramid mixed solution is 15-20%.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111560667A (en) * | 2020-05-15 | 2020-08-21 | 安徽众诚环境检测有限公司 | Preparation method of modified electrospun carbon nanofiber for wastewater detection |
| CN112026320A (en) * | 2020-09-04 | 2020-12-04 | 周鹏 | Textile fabric with antistatic and antibacterial functions and preparation method thereof |
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| CN102517693A (en) * | 2011-11-21 | 2012-06-27 | 圣欧（苏州）安全防护材料有限公司 | Preparation method of aramid-based carbon fiber |
| CN103850148A (en) * | 2014-03-17 | 2014-06-11 | 陕西科技大学 | Preparation method of nano-silica reinforced meta-aramid paper |
| CN107044073A (en) * | 2017-06-06 | 2017-08-15 | 国家电网公司 | Suppress the preparation method of the meta-aramid insulating paper of space charge accumulation |
| CN108396408A (en) * | 2018-01-30 | 2018-08-14 | 东莞市联洲知识产权运营管理有限公司 | A kind of preparation method of the multistage hole carbon fiber of aramid fiber base enhancing of N doping |
| US11072743B1 (en) * | 2015-12-04 | 2021-07-27 | Savannah Ashley Cofer | Fire resistant materials based on endothermic alumina-silica hydrate fibers |
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2019
- 2019-12-19 CN CN201911320046.0A patent/CN110983494A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102174771A (en) * | 2011-01-28 | 2011-09-07 | 钟洲 | Method for making additive meta-aramid paper |
| CN102517693A (en) * | 2011-11-21 | 2012-06-27 | 圣欧（苏州）安全防护材料有限公司 | Preparation method of aramid-based carbon fiber |
| CN103850148A (en) * | 2014-03-17 | 2014-06-11 | 陕西科技大学 | Preparation method of nano-silica reinforced meta-aramid paper |
| US11072743B1 (en) * | 2015-12-04 | 2021-07-27 | Savannah Ashley Cofer | Fire resistant materials based on endothermic alumina-silica hydrate fibers |
| CN107044073A (en) * | 2017-06-06 | 2017-08-15 | 国家电网公司 | Suppress the preparation method of the meta-aramid insulating paper of space charge accumulation |
| CN108396408A (en) * | 2018-01-30 | 2018-08-14 | 东莞市联洲知识产权运营管理有限公司 | A kind of preparation method of the multistage hole carbon fiber of aramid fiber base enhancing of N doping |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111560667A (en) * | 2020-05-15 | 2020-08-21 | 安徽众诚环境检测有限公司 | Preparation method of modified electrospun carbon nanofiber for wastewater detection |
| CN111560667B (en) * | 2020-05-15 | 2022-06-17 | 安徽众诚环境检测有限公司 | Preparation method of modified electrospun carbon nanofiber for wastewater detection |
| CN112026320A (en) * | 2020-09-04 | 2020-12-04 | 周鹏 | Textile fabric with antistatic and antibacterial functions and preparation method thereof |
| CN112026320B (en) * | 2020-09-04 | 2023-04-18 | 普宁市晨盛纺织有限公司 | Textile fabric with antistatic and antibacterial functions and preparation method thereof |
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Application publication date: 20200410 |