CN105350115A - Preparation method of pre-oxidized fibre - Google Patents
Preparation method of pre-oxidized fibre Download PDFInfo
- Publication number
- CN105350115A CN105350115A CN201510928489.3A CN201510928489A CN105350115A CN 105350115 A CN105350115 A CN 105350115A CN 201510928489 A CN201510928489 A CN 201510928489A CN 105350115 A CN105350115 A CN 105350115A
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- CN
- China
- Prior art keywords
- preparation
- spinning
- solvent
- fibre
- oxidization fiber
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- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Classifications
-
- 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
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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
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Artificial Filaments (AREA)
Abstract
The invention discloses a preparation method of pre-oxidized fibre, comprising the specific steps of 1) putting an acrylonitrile monomer and a comonomer into a solvent, and polymerizing to obtain a spinning dope; 2) preparing the spinning dope obtained in step 1) into nascent fibre by using a dry-jet wet spinning method; 3) drafting, washing, oiling and drying-compacting the nascent fibre obtained in step 2), thus obtaining protofilaments; 4) putting the protofilaments obtained in step 3) into an air oxidation furnace with a temperature gradient of 180-300 DEG C for pre-oxidation, thus obtaining the pre-oxidized fibre. In this way, according to the preparation method of the pre-oxidized fiber, the green and recyclable solvent is used for preparing, safety and environment friendliness are realized, and the work efficiency of a spinning machine is favorably improved.
Description
Technical field
The present invention relates to field of textiles, particularly relate to a kind of preparation method of oxidization fiber.
Background technology
High-performance polyacrylonitrile carbon fiber has light weight, high strength, high-modulus, conduction, high temperature resistant, corrosion-resistant.Antiscour and sputtering and good designability, can the irreplaceable premium properties of a series of other materials such as plyability, at present relate to the strategic meaning department of defence and military and civilian high-tech field is widely used at Aeronautics and Astronautics etc., in polyacrylonitrile carbon fiber preparation process, the preparation of oxidization fiber is one of important step determining carbon fiber performance.
Summary of the invention
The technical problem that the present invention mainly solves is to provide a kind of preparation method of oxidization fiber.
For solving the problems of the technologies described above, the technical scheme that the present invention adopts is: a kind of preparation method of oxidization fiber, and concrete steps comprise:
1) acrylonitrile monemer and comonomer are put into solvent to be polymerized and to make spinning solution;
2) use the method for dry-wet spinning that the spinning solution that step (1) obtains is made as-spun fibre;
3) step (2) is obtained as-spun fibre through drawing-off, wash, oil and make precursor after compacting by drying technique;
4) step (4) is obtained precursor to put into the air oxidation stove with 180 DEG C ~ 300 DEG C of thermogrades and carry out pre-oxidation, thus obtain oxidization fiber.
In a preferred embodiment of the present invention, described in step (1), comonomer is methyl acrylate.
In a preferred embodiment of the present invention, solvent described in step (1) is 1-butyl-3-methylimidazole tetrafluoro boric acid.
The invention has the beneficial effects as follows: the preparation method of a kind of oxidization fiber of the present invention, this preparation method adopts green callable solvent to be prepared, safety and environmental protection, and contributes to the operating efficiency improving spinning machine.
Detailed description of the invention
Below preferred embodiment of the present invention is described in detail, can be easier to make advantages and features of the invention be readily appreciated by one skilled in the art, thus more explicit defining is made to protection scope of the present invention.
The embodiment of the present invention comprises: a kind of preparation method of oxidization fiber, and concrete steps comprise:
1) acrylonitrile monemer and comonomer are put into solvent to be polymerized and to make spinning solution, described comonomer is methyl acrylate, described solvent is 1-butyl-3-methylimidazole tetrafluoro boric acid, with acrylonitrile monemer: methyl acrylate: 1-butyl-3-methylimidazole tetrafluoro boric acid=94: the ratio formula of 4: 2, polymerisation in solution in polymeric kettle, by controlling initiator amount, polymerization temperature, polymerization time controls polymerisation conversion, the copolymer of spinning requirement is all met with obtained molecular weight and molecualr weight distribution, namely the polymer solution obtained obtains polyacrylonitrile spinning solution after removing monomer.
Described comonomer is that methyl acrylate plays a part to delay cyano-cyclization reaction, and serves useful effect to the cortex content improving polyacrylonitrile.
Described solvent is 1-butyl-3-methylimidazole tetrafluoro boric acid, have when 1-butyl-3-methylimidazole tetrafluoro boric acid and acrylonitrile reactor that polymerization rate is fast, the feature of the large and narrow molecular weight distribution of molecular weight, and 1-butyl-3-methylimidazole tetrafluoro boric acid belongs to ionic liquid and has the green character being beneficial to recycling.
2) use the method for dry-wet spinning that the spinning solution that step (1) obtains is made as-spun fibre, dry-wet spinning spinning speed compared with general wet spinning is fast, the spinning head that aperture is larger can be adopted, adopt concentration higher, the spinning solution that viscosity is larger, the ability of spinning machine can be significantly improved, be conducive to obtaining the precursor of any surface finish without groove.
3) step (2) is obtained as-spun fibre through drawing-off, wash, oil and make precursor after compacting by drying technique, drawing-off makes the PAN strand in precursor arrange vertically, improves the degree of orientation of polymer, improves the mechanical property of fiber.
Wash in ionized water, reduce solvent residual in as-spun fibre.
Oil and make to form film at fiber surface, prevent adhesion or doubling between monofilament.
Compacting by drying is uneven for the structure eliminated in spinning process of setting caused by solvent and the counterdiffusion of coagulating agent phase, and consequent for counting cavity that is heavily many, that differ in size and fissured structure.
4) step (4) is obtained precursor to put into the air oxidation stove with 180 DEG C ~ 300 DEG C of thermogrades and carry out pre-oxidation, thus obtain oxidization fiber.
Compared with prior art, the preparation method of a kind of oxidization fiber of the present invention, this preparation method adopts green callable solvent to be prepared, safety and environmental protection, and contributes to the operating efficiency improving spinning machine.
The foregoing is only embodiments of the invention; not thereby the scope of the claims of the present invention is limited; every utilize description of the present invention to do equivalent structure or equivalent flow process conversion; or be directly or indirectly used in other relevant technical fields, be all in like manner included in scope of patent protection of the present invention.
Claims (3)
1. a preparation method for oxidization fiber, is characterized in that, concrete steps comprise:
1) acrylonitrile monemer and comonomer are put into solvent to be polymerized and to make spinning solution;
2) use the method for dry-wet spinning that the spinning solution that step (1) obtains is made as-spun fibre;
3) step (2) is obtained as-spun fibre through drawing-off, wash, oil and make precursor after compacting by drying technique;
4) step (4) is obtained precursor to put into the air oxidation stove with 180 DEG C ~ 300 DEG C of thermogrades and carry out pre-oxidation, thus obtain oxidization fiber.
2. the preparation method of a kind of oxidization fiber according to claim 1, is characterized in that: described in step (1), comonomer is methyl acrylate.
3. the preparation method of a kind of oxidization fiber according to claim 1, is characterized in that: solvent described in step (1) is 1-butyl-3-methylimidazole tetrafluoro boric acid.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510928489.3A CN105350115A (en) | 2015-12-15 | 2015-12-15 | Preparation method of pre-oxidized fibre |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510928489.3A CN105350115A (en) | 2015-12-15 | 2015-12-15 | Preparation method of pre-oxidized fibre |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN105350115A true CN105350115A (en) | 2016-02-24 |
Family
ID=55326171
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510928489.3A Pending CN105350115A (en) | 2015-12-15 | 2015-12-15 | Preparation method of pre-oxidized fibre |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105350115A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110106584A (en) * | 2019-04-26 | 2019-08-09 | 全球能源互联网研究院有限公司 | A kind of preoxidized fiber and preparation method thereof |
| CN110863269A (en) * | 2019-12-01 | 2020-03-06 | 陈佳宇 | Pretreatment device and method for carbon fiber PAN precursor ionic solution |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101067214A (en) * | 2007-06-12 | 2007-11-07 | 东华大学 | Dry-jet wet-spinning technique for producing polyacrylonitrile fibre |
| CN101760791A (en) * | 2009-11-24 | 2010-06-30 | 中复神鹰碳纤维有限责任公司 | Method for preparing high-performance polyacrylonitrile-based carbon fiber protofilament through dry spraying and wet spinning |
| CN104630937A (en) * | 2015-02-12 | 2015-05-20 | 南通市苏中纺织有限公司 | Polyacrylonitrile (PAN)-based high-strength and high-modulus carbon fiber |
-
2015
- 2015-12-15 CN CN201510928489.3A patent/CN105350115A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101067214A (en) * | 2007-06-12 | 2007-11-07 | 东华大学 | Dry-jet wet-spinning technique for producing polyacrylonitrile fibre |
| CN101760791A (en) * | 2009-11-24 | 2010-06-30 | 中复神鹰碳纤维有限责任公司 | Method for preparing high-performance polyacrylonitrile-based carbon fiber protofilament through dry spraying and wet spinning |
| CN104630937A (en) * | 2015-02-12 | 2015-05-20 | 南通市苏中纺织有限公司 | Polyacrylonitrile (PAN)-based high-strength and high-modulus carbon fiber |
Non-Patent Citations (1)
| Title |
|---|
| 林康等: "《干喷湿纺聚丙烯腈原丝的预氧化和碳化工艺》", 《合成纤维》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110106584A (en) * | 2019-04-26 | 2019-08-09 | 全球能源互联网研究院有限公司 | A kind of preoxidized fiber and preparation method thereof |
| CN110106584B (en) * | 2019-04-26 | 2021-11-30 | 全球能源互联网研究院有限公司 | Pre-oxidized fiber and preparation method thereof |
| CN110863269A (en) * | 2019-12-01 | 2020-03-06 | 陈佳宇 | Pretreatment device and method for carbon fiber PAN precursor ionic solution |
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Application publication date: 20160224 |
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