CN105332098A - Carbon fiber activation process - Google Patents
Carbon fiber activation process Download PDFInfo
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- CN105332098A CN105332098A CN201510825689.6A CN201510825689A CN105332098A CN 105332098 A CN105332098 A CN 105332098A CN 201510825689 A CN201510825689 A CN 201510825689A CN 105332098 A CN105332098 A CN 105332098A
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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
- D01F9/21—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products from macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D01F9/22—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products from macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds from polyacrylonitriles
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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
- D01F11/00—Chemical after-treatment of artificial filaments or the like during manufacture
- D01F11/10—Chemical after-treatment of artificial filaments or the like during manufacture of carbon
- D01F11/14—Chemical after-treatment of artificial filaments or the like during manufacture of carbon with organic compounds, e.g. macromolecular compounds
-
- 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
- D01F11/00—Chemical after-treatment of artificial filaments or the like during manufacture
- D01F11/10—Chemical after-treatment of artificial filaments or the like during manufacture of carbon
- D01F11/16—Chemical after-treatment of artificial filaments or the like during manufacture of carbon by physicochemical methods
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
- Inorganic Fibers (AREA)
Abstract
The invention relates to a carbon fiber activation process and belongs to the technical field of production of carbon fiber. According to the technical scheme, the carbon fiber activation process comprises the following steps: step one, preparing polyacrylonitrile-based carbon fiber; step two, taking argon/oxygen mixed gas as a mixed atmosphere, introducing a large quantity of oxygen-containing groups into the carbon fiber surface in a plasma treatment process so as to improve the hydrophilia of the carbon fiber surface; and step three, starching, and remedying defects of the carbon fiber surface subjected to the plasma treatment to a certain extent. Through the carbon fiber activation process, the mechanical strength of the carbon fiber is improved; the beneficial effect is significant.
Description
Technical field
The present invention relates to a kind of carbon fiber activating process, belong to carbon fiber production technical field.
Background technology
Carbon fiber (carbonfiber is called for short CF) is the tencel material of the high strength of a kind of phosphorus content more than 95%, high modulus fibre.It to be piled up along fiber axial direction by organic fibers such as flake graphite crystallites to form, the micro crystal graphite material obtained through carbonization and graphitization processing.Carbon fiber " soft outside but hard inside ", quality is lighter than metallic aluminium, but intensity is higher than iron and steel, and there is characteristic that is corrosion-resistant, high-modulus, applied in space flight, aviation and the industry various fields such as civilian by people, it not only has the intrinsic intrinsic property of material with carbon element, has both again the soft machinability of textile fabric, is fortifying fibre of new generation.
Carbon fibre composite (CFRP) mainly with carbon fiber be reinforcing material, matrix is resin, metal, pottery etc., produce through combination process, the component that its combination property is more single is more excellent.And in this composite, the structure of carbon fiber then serves critical effect.In general carbon fiber production technology, its surface smoothing of the carbon fiber of the graphite-structure after high temperature cabonization, surface energy is lower, active function groups is few, carbon fiber and the organic polymer matrix wettability of this kind of structure are very poor, thus need through activation processing, to improve carbon fiber surface activity and composite material combination property.
The surface modification of carbon fiber is generally divided into physical treatment and chemical treatment two class: wherein physical treatment method comprises coating, heat treating process etc., improves the physics interlocking between carbon fiber and matrix by the specific area and roughness improving carbon fiber; And chemical rule comprises anodizing, plasma oxidation method, Graft Method etc., utilize the increase of carbon fiber surface chemical functional group, improve the bond strength of chemical bond, although but improve the group numbers of carbon fiber surface after chemical treatment, also reduce the intensity of carbon fiber body to a certain extent.
Summary of the invention
For solving problems of the prior art, the invention provides a kind of carbon fiber activating process, concrete technical scheme is as follows:
A kind of carbon fiber activating process, comprises the following steps: step one, prepared by polypropylene itrile group carbon fiber; Step 2, Cement Composite Treated by Plasma; Step 3, carbon fiber starching;
In described step 2, under normal pressure, in plasma generator, pass into argon/oxygen gas mixture as reaction atmosphere, reaction time 30s ~ 120s, voltage 5kV ~ 10kV, electric current 10mA ~ 30mA, obtain the carbon mono-filaments after plasma treatment;
In described step 3, by the carbon mono-filaments after Cement Composite Treated by Plasma after the slurry that over-richness is 0.5% ~ 1.5%, dry and be positioned in drier and make activated carbon fiber.
As the improvement of technique scheme, in described step 2, in argon/oxygen gas mixture, the flow of argon gas is 2L/min ~ 4L/min, and the flow of oxygen is 10ml/min ~ 50ml/min.
As the improvement of technique scheme, in described step 3, slurry is water-based emulsion polyurethane.
As the improvement of technique scheme, it is characterized in that, described step one is divided into two steps:
(1) preparation of polyacrylonitrile fibril, carries out copolymerization, ammonification by acrylonitrile stoste, obtains polyacrylonitrile matrix, deaeration after multiple segment filters, and after coagulation forming, water-bath stretches, and carries out pre-oxidation and obtain polyacrylonitrile fibril after compacting by drying;
(2) carbonization, first carries out low-temperature carbonization at 1200 DEG C ~ 1800 DEG C to polyacrylonitrile fibril, then carries out high temperature cabonization at 2600 DEG C ~ 3000 DEG C to it, obtain polypropylene itrile group carbon fiber.
Technique scheme is in step 2, by argon/oxygen gas mixture as mixed atmosphere, can in plasma treatment process, introduce a large amount of oxy radical to carbon fiber surface, thus improve the hydrophily of carbon fiber surface, in step 3, through starching process, make up the defect of carbon fiber surface after plasma treatment to a certain extent, improve the mechanical strength of carbon fiber, beneficial effect is remarkable.
Detailed description of the invention
The invention provides a kind of carbon fiber activating process, comprise the following steps: step one, prepared by polypropylene itrile group carbon fiber; Step 2, Cement Composite Treated by Plasma; Step 3, carbon fiber starching;
Described step one is divided into two steps:
(1) preparation of polyacrylonitrile fibril, carries out copolymerization, ammonification by acrylonitrile stoste, obtains polyacrylonitrile matrix, deaeration after multiple segment filters, and after coagulation forming, water-bath stretches, and carries out pre-oxidation and obtain polyacrylonitrile fibril after compacting by drying;
(2) carbonization, first carries out low-temperature carbonization at 1200 DEG C ~ 1800 DEG C to polyacrylonitrile fibril, then carries out high temperature cabonization at 2600 DEG C ~ 3000 DEG C to it, obtain polypropylene itrile group carbon fiber.
In described step 2, under normal pressure, argon/oxygen gas mixture is passed into as reaction atmosphere in plasma generator, reaction time 30s ~ 120s, voltage 5kV ~ 10kV, electric current 10mA ~ 30mA, obtain the carbon mono-filaments after plasma treatment, wherein in argon/oxygen gas mixture, the flow of argon gas is 2L/min ~ 4L/min, and the flow of oxygen is 10ml/min ~ 50ml/min;
In described step 3, by the carbon mono-filaments after Cement Composite Treated by Plasma after the slurry that over-richness is 0.5% ~ 1.5%, wherein slurry is water-based emulsion polyurethane, dries and is positioned in drier and make activated carbon fiber.
In technique scheme, in step 2, by argon/oxygen gas mixture as mixed atmosphere, in plasma treatment process, a large amount of oxy radical can be introduced to carbon fiber surface, thus improve the hydrophily of carbon fiber surface, in step 3, through starching process, make up the defect of carbon fiber surface after plasma treatment to a certain extent, improve the mechanical strength of carbon fiber.
Be described further below in conjunction with specific embodiment.
Embodiment one
Activated carbon fiber is prepared according to following steps:
Step one, prepared by polypropylene itrile group carbon fiber:
(1) preparation of polyacrylonitrile fibril, carries out copolymerization, ammonification by acrylonitrile stoste, obtains polyacrylonitrile matrix, deaeration after multiple segment filters, and after coagulation forming, water-bath stretches, and carries out pre-oxidation and obtain polyacrylonitrile fibril after compacting by drying;
(2) carbonization, first carries out low-temperature carbonization at 1200 DEG C to polyacrylonitrile fibril, then carries out high temperature cabonization at 2600 DEG C to it, obtain polypropylene itrile group carbon fiber.
Step 2, Cement Composite Treated by Plasma: under normal pressure, argon/oxygen gas mixture is passed into as reaction atmosphere in plasma generator, reaction time 30s, voltage 5kV, electric current 30mA, obtain the carbon mono-filaments after plasma treatment, wherein in argon/oxygen gas mixture, the flow of argon gas is 2L/min, and the flow of oxygen is 10ml/min;
Step 3, carbon fiber starching: be in the water-based emulsion polyurethane slurry of 0.5% through over-richness by the carbon mono-filaments after Cement Composite Treated by Plasma, dry and be positioned in drier and make activated carbon fiber.
The dynamic contact angle of the activated carbon fiber obtained and ethylene glycol, deionized water is carried out record respectively, and calculates the surface energy of carbon fiber, record data in table 1.
Embodiment two
Activated carbon fiber is prepared according to following steps:
Step one, prepared by polypropylene itrile group carbon fiber:
(1) preparation of polyacrylonitrile fibril, carries out copolymerization, ammonification by acrylonitrile stoste, obtains polyacrylonitrile matrix, deaeration after multiple segment filters, and after coagulation forming, water-bath stretches, and carries out pre-oxidation and obtain polyacrylonitrile fibril after compacting by drying;
(2) carbonization, first carries out low-temperature carbonization at 1400 DEG C to polyacrylonitrile fibril, then carries out high temperature cabonization at 2700 DEG C to it, obtain polypropylene itrile group carbon fiber.
Step 2, Cement Composite Treated by Plasma: under normal pressure, argon/oxygen gas mixture is passed into as reaction atmosphere in plasma generator, reaction time 40s, voltage 7kV, electric current 25mA, obtain the carbon mono-filaments after plasma treatment, wherein in argon/oxygen gas mixture, the flow of argon gas is 2L/min, and the flow of oxygen is 30ml/min;
Step 3, carbon fiber starching: be in the water-based emulsion polyurethane slurry of 1.0% through over-richness by the carbon mono-filaments after Cement Composite Treated by Plasma, dry and be positioned in drier and make activated carbon fiber.
The dynamic contact angle of the activated carbon fiber obtained and ethylene glycol, deionized water is carried out record respectively, and calculates the surface energy of carbon fiber, record data in table 1.
Embodiment three
Activated carbon fiber is prepared according to following steps:
Step one, prepared by polypropylene itrile group carbon fiber:
(1) preparation of polyacrylonitrile fibril, carries out copolymerization, ammonification by acrylonitrile stoste, obtains polyacrylonitrile matrix, deaeration after multiple segment filters, and after coagulation forming, water-bath stretches, and carries out pre-oxidation and obtain polyacrylonitrile fibril after compacting by drying;
(2) carbonization, first carries out low-temperature carbonization at 1600 DEG C to polyacrylonitrile fibril, then carries out high temperature cabonization at 2800 DEG C to it, obtain polypropylene itrile group carbon fiber.
Step 2, Cement Composite Treated by Plasma: under normal pressure, argon/oxygen gas mixture is passed into as reaction atmosphere in plasma generator, reaction time 70s, voltage 8kV, electric current 20mA, obtain the carbon mono-filaments after plasma treatment, wherein in argon/oxygen gas mixture, the flow of argon gas is 2L/min, and the flow of oxygen is 50ml/min;
Step 3, carbon fiber starching: be in the water-based emulsion polyurethane slurry of 1.5% through over-richness by the carbon mono-filaments after Cement Composite Treated by Plasma, dry and be positioned in drier and make activated carbon fiber.
The dynamic contact angle of the activated carbon fiber obtained and ethylene glycol, deionized water is carried out record respectively, and calculates the surface energy of carbon fiber, record data in table 1.
Embodiment four
Activated carbon fiber is prepared according to following steps:
Step one, prepared by polypropylene itrile group carbon fiber:
(1) preparation of polyacrylonitrile fibril, carries out copolymerization, ammonification by acrylonitrile stoste, obtains polyacrylonitrile matrix, deaeration after multiple segment filters, and after coagulation forming, water-bath stretches, and carries out pre-oxidation and obtain polyacrylonitrile fibril after compacting by drying;
(2) carbonization, first carries out low-temperature carbonization at 1800 DEG C to polyacrylonitrile fibril, then carries out high temperature cabonization at 3000 DEG C to it, obtain polypropylene itrile group carbon fiber.
Step 2, Cement Composite Treated by Plasma: under normal pressure, argon/oxygen gas mixture is passed into as reaction atmosphere in plasma generator, reaction time 120s, voltage 10kV, electric current 10mA, obtain the carbon mono-filaments after plasma treatment, wherein in argon/oxygen gas mixture, the flow of argon gas is 4L/min, and the flow of oxygen is 50ml/min;
Step 3, carbon fiber starching: be in the water-based emulsion polyurethane slurry of 1.0% through over-richness by the carbon mono-filaments after Cement Composite Treated by Plasma, dry and be positioned in drier and make activated carbon fiber.
The dynamic contact angle of the activated carbon fiber obtained and ethylene glycol, deionized water is carried out record respectively, and calculates the surface energy of carbon fiber, record data in table 1.
Table 1 different parameters is on the impact of carbon fibre surface energy
Claims (4)
1. a carbon fiber activating process, comprises the following steps: step one, prepared by polypropylene itrile group carbon fiber; Step 2, Cement Composite Treated by Plasma; Step 3, carbon fiber starching; It is characterized in that,
In described step 2, under normal pressure, in plasma generator, pass into argon/oxygen gas mixture as reaction atmosphere, reaction time 30s ~ 120s, voltage 5kV ~ 10kV, electric current 10mA ~ 30mA, obtain the carbon mono-filaments after plasma treatment;
In described step 3, by the carbon mono-filaments after Cement Composite Treated by Plasma after the slurry that over-richness is 0.5% ~ 1.5%, dry and be positioned in drier and make activated carbon fiber.
2. a kind of carbon fiber activating process as claimed in claim 1, is characterized in that, in described step 2, in argon/oxygen gas mixture, the flow of argon gas is 2L/min ~ 4L/min, and the flow of oxygen is 10ml/min ~ 50ml/min.
3. a kind of carbon fiber activating process as claimed in claim 2, is characterized in that, in described step 3, slurry is water-based emulsion polyurethane.
4. a kind of carbon fiber activating process according to any one of claim 1-3, it is characterized in that, described step one is divided into two steps:
(1) preparation of polyacrylonitrile fibril, carries out copolymerization, ammonification by acrylonitrile stoste, obtains polyacrylonitrile matrix, deaeration after multiple segment filters, and after coagulation forming, water-bath stretches, and carries out pre-oxidation and obtain polyacrylonitrile fibril after compacting by drying;
(2) carbonization, first carries out low-temperature carbonization at 1200 DEG C ~ 1800 DEG C to polyacrylonitrile fibril, then carries out high temperature cabonization at 2600 DEG C ~ 3000 DEG C to it, obtain polypropylene itrile group carbon fiber.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510825689.6A CN105332098A (en) | 2015-11-25 | 2015-11-25 | Carbon fiber activation process |
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| CN201510825689.6A CN105332098A (en) | 2015-11-25 | 2015-11-25 | Carbon fiber activation process |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108368646A (en) * | 2016-08-25 | 2018-08-03 | 仓敷纺绩株式会社 | The manufacturing method of carbon fiber fibrillation sheet material |
| CN108978178A (en) * | 2018-08-06 | 2018-12-11 | 合肥岑遥新材料科技有限公司 | A kind of activating process of carbon fiber |
| TWI663124B (en) * | 2016-11-23 | 2019-06-21 | 永虹先進材料股份有限公司 | Carbon fiber manufacturing method |
| CN110761067A (en) * | 2019-10-30 | 2020-02-07 | 中国人民解放军空军工程大学 | Carbon fiber surface continuous treatment method and device based on normal-pressure DBD discharge |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH03287860A (en) * | 1990-04-04 | 1991-12-18 | Toray Ind Inc | Production of carbon fiber |
| CN102720061A (en) * | 2012-06-29 | 2012-10-10 | 东华大学 | Preparation method for improving interfacial properties of carbon fiber composite material |
| CN103361768A (en) * | 2012-03-30 | 2013-10-23 | 上海斯瑞聚合体科技有限公司 | Surface modification method of polyacrylonitrile-based carbon fiber |
-
2015
- 2015-11-25 CN CN201510825689.6A patent/CN105332098A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH03287860A (en) * | 1990-04-04 | 1991-12-18 | Toray Ind Inc | Production of carbon fiber |
| CN103361768A (en) * | 2012-03-30 | 2013-10-23 | 上海斯瑞聚合体科技有限公司 | Surface modification method of polyacrylonitrile-based carbon fiber |
| CN102720061A (en) * | 2012-06-29 | 2012-10-10 | 东华大学 | Preparation method for improving interfacial properties of carbon fiber composite material |
Non-Patent Citations (2)
| Title |
|---|
| 张焕侠: "碳纤维表面和界面性能研究及评价", 《中国博士学位论文全文数据库 工程科技І辑》 * |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108368646A (en) * | 2016-08-25 | 2018-08-03 | 仓敷纺绩株式会社 | The manufacturing method of carbon fiber fibrillation sheet material |
| TWI663124B (en) * | 2016-11-23 | 2019-06-21 | 永虹先進材料股份有限公司 | Carbon fiber manufacturing method |
| CN108978178A (en) * | 2018-08-06 | 2018-12-11 | 合肥岑遥新材料科技有限公司 | A kind of activating process of carbon fiber |
| CN110761067A (en) * | 2019-10-30 | 2020-02-07 | 中国人民解放军空军工程大学 | Carbon fiber surface continuous treatment method and device based on normal-pressure DBD discharge |
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