CN101760807A - Method for reducing production of preoxidized broken filament during preparation of polyacrylonitrile-based carbon fiber - Google Patents
Method for reducing production of preoxidized broken filament during preparation of polyacrylonitrile-based carbon fiber Download PDFInfo
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- CN101760807A CN101760807A CN200910234308A CN200910234308A CN101760807A CN 101760807 A CN101760807 A CN 101760807A CN 200910234308 A CN200910234308 A CN 200910234308A CN 200910234308 A CN200910234308 A CN 200910234308A CN 101760807 A CN101760807 A CN 101760807A
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Abstract
The invention discloses a method for reducing the production of preoxidized broken filament during the preparation of polyacrylonitrile-based carbon fiber, characterized in that: dipping: polyacrylonitrile-based carbon fiber precursor is dipped with pure water until the water content in the precursor is 5-15wt%; or polyacrylonitrile-based carbon fiber precursor is dipped with epoxy ethane modified silicone oil emulsion or ammonia modified silicone oil emulsion until the water content in the precursor is 5-15wt% and attached amount of oil is 0.5-1wt%; and shaping: the dipped precursor is subject to shaping. Owing to the effect of surface tension of the pure water, a fiber bundle dipped with the pure water is increased in convergence property, and the generated broken filaments are adhered to the fiber bundle; a layer of protective film is formed on the surface of fiber by using the fiber bundle dipped with the oil emulsion, thereby preventing inter-fiber adhesion and doubling and simultaneously avoiding the physical damage to fibers by furnace rollers; and the shaping treatment can effectively relieve the internal stress generated in the production process of the precursor, thereby avoiding fibers from tension fracture in the process of preoxidation.
Description
Technical field
The present invention relates to the preparation method of polyacrylonitrile-based carbon fibre, reduce the method that the pre-oxidation lousiness produces in particularly a kind of polyacrylonitrile-based carbon fibre preparation.
Background technology
In the preparation process of polyacrylonitrile-based carbon fibre, the pre-oxidation stage is the stage the most consuming time.Fiber is through a plurality of active drawing roller, various roll bodies such as guide roller in preoxidation process.With the meeting that contacts of roll body fiber is caused the damage on surface repeatedly, the lousiness of generation such as untimely processing are easy to take place curling round the roll, with stablizing that influence is produced.Repeatedly the drawing-off meeting causes the fiber internal stress to increase in the precursor production process, makes the drawing-off in pre-oxidation stage be difficult to carry out.
Summary of the invention
Technical problem to be solved by this invention is at the deficiencies in the prior art, and a kind of lousiness that reduces the pre-oxidation stage is provided, and improves the convergence of fibre bundle, prevents that fiber from being damaged by roll body, avoids at pre-oxidation, carbonation stage because of too much curling round the roll of lousiness.
Technical problem to be solved by this invention is to realize by following technical scheme.The present invention reduces the method that the pre-oxidation lousiness produces in a kind of polyacrylonitrile-based carbon fibre preparation, is characterized in that its step is as follows:
(1) dipping: get polyacrylonitrile base carbon fiber precursors, with the pure water dipping, the moisture that is dipped into precursor is 5-15wt%; Perhaps with oxirane modified silicon oil emulsion dipping, the moisture that is dipped into precursor is 5-15wt%, and the finish adhesion amount is 0.5-1wt%; Perhaps with ammonia modified silicon oil emulsion dipping, the moisture that is dipped into precursor is 5-15wt%, and the finish adhesion amount is 0.5-1wt%;
(2) typing: will enter modular system processings of finalizing the design through the precursor of impregnation process, the temperature of the processing of finalizing the design is 100-180 ℃.
In the above-described technical scheme:
1, in step (1), during with pure water dipping acrylonitrile base carbon fiber precursor, the moisture that is dipped into precursor is elected 8-12wt% as.
2, in step (1), during with oxirane modified silicon oil emulsion dipping acrylonitrile base carbon fiber precursor, the moisture that is dipped into precursor is elected 8-12wt% as, and the finish adhesion amount is elected 0.6-0.8wt% as.
3, in step (1), during with ammonia modified silicon oil emulsion dipping polyacrylonitrile base carbon fiber precursors, the moisture that is dipped into precursor is elected 8-12wt% as, and the finish adhesion amount is elected 0.6-0.8wt% as.
4, in step (2), the temperature that typing is handled is preferably 130-150 ℃.
5, the modular system described in the present invention can adopt disclosed any modular system applicatory in the prior art.
Compared with prior art, the present invention is because the capillary effect of pure water, and the convergence of the fibre bundle that soaked into pure water can increase to some extent, and the lousiness of Chan Shenging just is attached on the fibre bundle like this.The fibre bundle that adopts the finish emulsion to soak into can form layer protecting film at fiber surface, prevents that pre-oxidation from being the generation of interfibrous adhesion and doubling, has also avoided the physical damnification of stove roll body to fiber simultaneously.And, in the processing of in temperature is 100-180 ℃ modular system, finalizing the design earlier behind the dipping, before precursor enters pre-oxidation furnace, can alleviate the internal stress that produces in the precursor production process effectively, avoid in the preoxidation process fiber to be broken.
The specific embodiment
Below further describe concrete technical scheme of the present invention,, and do not constitute restriction its right so that those skilled in the art understands the present invention further.
Embodiment 1.Reduce the method that the pre-oxidation lousiness produces in a kind of polyacrylonitrile-based carbon fibre preparation, its step is as follows:
(1) dipping: get polyacrylonitrile base carbon fiber precursors, with the pure water dipping, the moisture that is dipped into precursor is 5wt%;
(2) typing: will enter modular system processings of finalizing the design through the precursor of impregnation process, the temperature of the processing of finalizing the design is 100 ℃.
Embodiment 2.Reduce the method that the pre-oxidation lousiness produces in a kind of polyacrylonitrile-based carbon fibre preparation, its step is as follows:
(1) dipping: get polyacrylonitrile base carbon fiber precursors, with the pure water dipping, the moisture that is dipped into precursor is 15wt%;
(2) typing: will enter modular system processings of finalizing the design through the precursor of impregnation process, the temperature of the processing of finalizing the design is 180 ℃.
Embodiment 3.Reduce the method that the pre-oxidation lousiness produces in a kind of polyacrylonitrile-based carbon fibre preparation, its step is as follows:
(1) dipping: get polyacrylonitrile base carbon fiber precursors, with the pure water dipping, the moisture that is dipped into precursor is 8wt%;
(2) typing: will enter modular system processings of finalizing the design through the precursor of impregnation process, the temperature of the processing of finalizing the design is 120 ℃.
Embodiment 4.Reduce the method that the pre-oxidation lousiness produces in a kind of polyacrylonitrile-based carbon fibre preparation, its step is as follows:
(1) dipping: get polyacrylonitrile base carbon fiber precursors, with the pure water dipping, the moisture that is dipped into precursor is 12wt%;
(2) typing: will enter modular system processings of finalizing the design through the precursor of impregnation process, the temperature of the processing of finalizing the design is 160 ℃.
Embodiment 5.Reduce the method that the pre-oxidation lousiness produces in a kind of polyacrylonitrile-based carbon fibre preparation, its step is as follows:
(1) dipping: get polyacrylonitrile base carbon fiber precursors, with the pure water dipping, the moisture that is dipped into precursor is 10wt%;
(2) typing: will enter modular system processings of finalizing the design through the precursor of impregnation process, the temperature of the processing of finalizing the design is 150 ℃.
Embodiment 5.Reduce the method that the pre-oxidation lousiness produces in a kind of polyacrylonitrile-based carbon fibre preparation, its step is as follows:
(1) dipping: with oxirane modified silicon oil emulsion dipping, the moisture that is dipped into precursor is 5wt%, and the finish adhesion amount is 0.5wt%;
(2) typing: will enter modular system processings of finalizing the design through the precursor of impregnation process, the temperature of the processing of finalizing the design is 100 ℃.
Embodiment 6.Reduce the method that the pre-oxidation lousiness produces in a kind of polyacrylonitrile-based carbon fibre preparation, its step is as follows:
(1) dipping: with oxirane modified silicon oil emulsion dipping, the moisture that is dipped into precursor is 15wt%, and the finish adhesion amount is 1wt%;
(2) typing: will enter modular system processings of finalizing the design through the precursor of impregnation process, the temperature of the processing of finalizing the design is 180 ℃.
Embodiment 7.Reduce the method that the pre-oxidation lousiness produces in a kind of polyacrylonitrile-based carbon fibre preparation, its step is as follows:
(1) dipping: with oxirane modified silicon oil emulsion dipping, the moisture that is dipped into precursor is 5-15wt%, and the finish adhesion amount is 0.8wt%;
(2) typing: will enter modular system processings of finalizing the design through the precursor of impregnation process, the temperature of the processing of finalizing the design is 130 ℃.
Embodiment 8.Reduce the method that the pre-oxidation lousiness produces in a kind of polyacrylonitrile-based carbon fibre preparation, its step is as follows:
(1) dipping: with oxirane modified silicon oil emulsion dipping, the moisture that is dipped into precursor is 5-15wt%, and the finish adhesion amount is 0.9wt%;
(2) typing: will enter modular system processings of finalizing the design through the precursor of impregnation process, the temperature of the processing of finalizing the design is 160 ℃.
Embodiment 9.Reduce the method that the pre-oxidation lousiness produces in a kind of polyacrylonitrile-based carbon fibre preparation, its step is as follows:
(1) dipping: with oxirane modified silicon oil emulsion dipping, the moisture that is dipped into precursor is 5-15wt%, and the finish adhesion amount is 0.7wt%;
(2) typing: will enter modular system processings of finalizing the design through the precursor of impregnation process, the temperature of the processing of finalizing the design is 145 ℃.
Embodiment 10.Reduce the method that the pre-oxidation lousiness produces in a kind of polyacrylonitrile-based carbon fibre preparation, its step is as follows:
(1) dipping: with oxirane modified silicon oil emulsion dipping, the moisture that is dipped into precursor is 5-15wt%, and the finish adhesion amount is 0.6wt%;
(2) typing: will enter modular system processings of finalizing the design through the precursor of impregnation process, the temperature of the processing of finalizing the design is 140 ℃.
Embodiment 11.Reduce the method that the pre-oxidation lousiness produces in a kind of polyacrylonitrile-based carbon fibre preparation, its step is as follows:
(1) dipping: with ammonia modified silicon oil emulsion dipping, the moisture that is dipped into precursor is 5wt%, and the finish adhesion amount is 0.5wt%;
(2) typing: will enter modular system processings of finalizing the design through the precursor of impregnation process, the temperature of the processing of finalizing the design is 100 ℃.
Embodiment 12.Reduce the method that the pre-oxidation lousiness produces in a kind of polyacrylonitrile-based carbon fibre preparation, its step is as follows:
(1) dipping: with ammonia modified silicon oil emulsion dipping, the moisture that is dipped into precursor is 15wt%, and the finish adhesion amount is 1wt%;
(2) typing: will enter modular system processings of finalizing the design through the precursor of impregnation process, the temperature of the processing of finalizing the design is 180 ℃.
Embodiment 13.Reduce the method that the pre-oxidation lousiness produces in a kind of polyacrylonitrile-based carbon fibre preparation, its step is as follows:
(1) dipping: with ammonia modified silicon oil emulsion dipping, the moisture that is dipped into precursor is 5-15wt%, and the finish adhesion amount is 0.85wt%;
(2) typing: will enter modular system processings of finalizing the design through the precursor of impregnation process, the temperature of the processing of finalizing the design is 130 ℃.
Embodiment 14.Reduce the method that the pre-oxidation lousiness produces in a kind of polyacrylonitrile-based carbon fibre preparation, its step is as follows:
(1) dipping: with ammonia modified silicon oil emulsion dipping, the moisture that is dipped into precursor is 5-15wt%, and the finish adhesion amount is 0.7wt%;
(2) typing: will enter modular system processings of finalizing the design through the precursor of impregnation process, the temperature of the processing of finalizing the design is 155 ℃.
Embodiment 15.Reduce the method that the pre-oxidation lousiness produces in a kind of polyacrylonitrile-based carbon fibre preparation, its step is as follows:
(1) dipping: with ammonia modified silicon oil emulsion dipping, the moisture that is dipped into precursor is 5-15wt%, and the finish adhesion amount is 0.65wt%;
(2) typing: will enter modular system processings of finalizing the design through the precursor of impregnation process, the temperature of the processing of finalizing the design is 165 ℃.
Embodiment 16.Reduce the method that the pre-oxidation lousiness produces in a kind of polyacrylonitrile-based carbon fibre preparation, its step is as follows:
(1) dipping: with ammonia modified silicon oil emulsion dipping, the moisture that is dipped into precursor is 5-15wt%, and the finish adhesion amount is 0.9wt%;
(2) typing: will enter modular system processings of finalizing the design through the precursor of impregnation process, the temperature of the processing of finalizing the design is 175 ℃.
Claims (5)
1. reduce the method that the pre-oxidation lousiness produces in a polyacrylonitrile-based carbon fibre preparation, it is characterized in that its step is as follows:
(1) dipping: get polyacrylonitrile base carbon fiber precursors, with the pure water dipping, the moisture that is dipped into precursor is 5-15wt%; Perhaps with oxirane modified silicon oil emulsion dipping, the moisture that is dipped into precursor is 5-15wt%, and the finish adhesion amount is 0.5-1wt%; Perhaps with ammonia modified silicon oil emulsion dipping, the moisture that is dipped into precursor is 5-15wt%, and the finish adhesion amount is 0.5-1wt%;
(2) typing: will enter modular system processings of finalizing the design through the precursor of impregnation process, the temperature of the processing of finalizing the design is 100-180 ℃.
2. method according to claim 1 is characterized in that, in step (1), during with pure water dipping polyacrylonitrile base carbon fiber precursors, the moisture that is dipped into precursor is 8-12wt%.
3. method according to claim 1 is characterized in that, in step (1), during with oxirane modified silicon oil emulsion dipping polyacrylonitrile base carbon fiber precursors, the moisture that is dipped into precursor is 8-12wt%, and the finish adhesion amount is 0.6-0.8wt%.
4. method according to claim 1 is characterized in that, in step (1), during with ammonia modified silicon oil emulsion dipping polyacrylonitrile base carbon fiber precursors, the moisture that is dipped into precursor is 8-12wt%, and the finish adhesion amount is 0.6-0.8wt%.
5. method according to claim 1 is characterized in that, in step (2), the temperature that typing is handled is 130-150 ℃.
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| CN200910234308A CN101760807A (en) | 2009-11-24 | 2009-11-24 | Method for reducing production of preoxidized broken filament during preparation of polyacrylonitrile-based carbon fiber |
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| CN200910234308A CN101760807A (en) | 2009-11-24 | 2009-11-24 | Method for reducing production of preoxidized broken filament during preparation of polyacrylonitrile-based carbon fiber |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103074758A (en) * | 2011-10-25 | 2013-05-01 | 金发科技股份有限公司 | Ultrasonic atomization humidification method for production of carbon fiber |
| CN103451945A (en) * | 2012-05-28 | 2013-12-18 | 中国科学院宁波材料技术与工程研究所 | Preparation method of high-performance polyacrylonitrile-based carbon fibers |
| CN103806131A (en) * | 2012-11-06 | 2014-05-21 | 中国科学院化学研究所 | Organosilicon spinning oil agent for preparing polyacrylonitrile-based carbon fibers |
| CN104047070A (en) * | 2014-06-27 | 2014-09-17 | 陕西天策新材料科技有限公司 | Preparation method of high-modulus graphite fibers |
| CN104340764A (en) * | 2013-08-09 | 2015-02-11 | 中国石油天然气股份有限公司 | Humidification processing method and device for filament retreat during carbonization of polyacrylonitrile protofilaments for carbon fibers |
| CN110685029A (en) * | 2018-07-06 | 2020-01-14 | 中国石油化工股份有限公司 | Oiling method of polyacrylonitrile-based carbon fiber precursor |
| CN111691012A (en) * | 2020-07-29 | 2020-09-22 | 常州市宏发纵横新材料科技股份有限公司 | Electric control type polyacrylonitrile precursor microwave pre-oxidation process |
| CN111893668A (en) * | 2020-07-07 | 2020-11-06 | 山西钢科碳材料有限公司 | Homogenization treatment device and method, and preparation method of polyacrylonitrile-based carbon fiber |
-
2009
- 2009-11-24 CN CN200910234308A patent/CN101760807A/en active Pending
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103074758A (en) * | 2011-10-25 | 2013-05-01 | 金发科技股份有限公司 | Ultrasonic atomization humidification method for production of carbon fiber |
| CN103451945B (en) * | 2012-05-28 | 2016-03-09 | 中国科学院宁波材料技术与工程研究所 | A kind of preparation method of high-performance polyacrylonitrile-based carbon fiber |
| CN103451945A (en) * | 2012-05-28 | 2013-12-18 | 中国科学院宁波材料技术与工程研究所 | Preparation method of high-performance polyacrylonitrile-based carbon fibers |
| CN103806131A (en) * | 2012-11-06 | 2014-05-21 | 中国科学院化学研究所 | Organosilicon spinning oil agent for preparing polyacrylonitrile-based carbon fibers |
| CN104340764A (en) * | 2013-08-09 | 2015-02-11 | 中国石油天然气股份有限公司 | Humidification processing method and device for filament retreat during carbonization of polyacrylonitrile protofilaments for carbon fibers |
| CN104047070B (en) * | 2014-06-27 | 2016-05-18 | 陕西天策新材料科技有限公司 | A kind of preparation method of high modulus graphite fiber |
| CN104047070A (en) * | 2014-06-27 | 2014-09-17 | 陕西天策新材料科技有限公司 | Preparation method of high-modulus graphite fibers |
| CN110685029A (en) * | 2018-07-06 | 2020-01-14 | 中国石油化工股份有限公司 | Oiling method of polyacrylonitrile-based carbon fiber precursor |
| CN110685029B (en) * | 2018-07-06 | 2021-05-11 | 中国石油化工股份有限公司 | Oiling method of polyacrylonitrile-based carbon fiber precursor |
| CN111893668A (en) * | 2020-07-07 | 2020-11-06 | 山西钢科碳材料有限公司 | Homogenization treatment device and method, and preparation method of polyacrylonitrile-based carbon fiber |
| CN111893668B (en) * | 2020-07-07 | 2023-07-14 | 山西钢科碳材料有限公司 | Homogenization treatment device and method and preparation method of polyacrylonitrile-based carbon fiber |
| CN111691012A (en) * | 2020-07-29 | 2020-09-22 | 常州市宏发纵横新材料科技股份有限公司 | Electric control type polyacrylonitrile precursor microwave pre-oxidation process |
| CN111691012B (en) * | 2020-07-29 | 2020-12-25 | 常州市宏发纵横新材料科技股份有限公司 | Electric control type polyacrylonitrile precursor microwave pre-oxidation process |
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Open date: 20100630 |