CN103757899B - Universal pitch-based carbon fiber spinning oil - Google Patents
Universal pitch-based carbon fiber spinning oil Download PDFInfo
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- CN103757899B CN103757899B CN201310751350.7A CN201310751350A CN103757899B CN 103757899 B CN103757899 B CN 103757899B CN 201310751350 A CN201310751350 A CN 201310751350A CN 103757899 B CN103757899 B CN 103757899B
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- carbon fiber
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Abstract
The invention discloses a kind of universal pitch-based carbon fiber spinning oil, this finish adopts deionized water, lubricant, antistatic additive, emulsifying agent and equilibrium modifier, mixes at stirring.Its viscosity is 2 ~ 20mPa.s, and light transmittance is 80% ~ 98%, is sprayed on fiber surface and can plays antistatic property, makes to have certain cohesive force between fibre single thread, reaches the effect of boundling, and stops fiber adhesion.Fiber surface forms thin finish film and not only protects monofilament surface in spinning from damage; and same anti-stick buffer action is also played in non-fusible and carbonisation, the problem such as easy adhesion, electrostatic and wearing and tearing existed can be solved in universal pitch-based carbon fiber preparation process.Result of the test shows, universal pitch-based carbon fiber spinning oil of the present invention and fiber surface contact angle are 0 ~ 5 °, can be coated in fiber surface well, and fibre strength conservation rate is 95% ~ 100%, and the TENSILE STRENGTH of finish on fiber does not affect substantially.
Description
Technical field
The present invention relates to the auxiliary agent that synthetic fiber filament uses in spinning process, particularly relate to a kind of universal pitch-based carbon fiber spinning oil.
Background technology
Universal pitch-based carbon fiber be a kind of with isotropism asphalt or coal tar pitch for raw material, through refining, the melt spinning of pitch, pre-oxidation, carbonization and special fibre that obtained phosphorus content is greater than 92%.Universal pitch-based carbon fiber raw material resources are enriched, there is higher carbonization rate compared with polyacrylonitrile-based carbon fibre, and cost is well below high-performance mesophase pitch-based carbon fibers, be widely used prospect, can be used for the fields such as asbestos alternative, cement intensifier, plastic modifier, also can be used for heat insulation, encapsulant, abrasion brake material, the application on acoustical material and fuel cell electrode is also quite wide.In addition, the carbon fiber through overactivation as catalyst or can also be used for purifying water body.
Universal asphalt base carbon fiber is high molecular polymer, hygroscopicity is little, poorly conductive, coefficient of friction is large, easily sticks together or doubling in melt spinning process between monofilament, and they easily produce electrostatic when spinning and textile process, affect production and processing, simultaneously in spinning and non-fusible, carbonisation, the tow of operation need through many actives or driven roll, its surface is very easily damaged to the friction of monofilament surface, produces new blemish.
Summary of the invention
Technical problem to be solved by this invention is to overcome the problem such as easy adhesion, electrostatic and wearing and tearing existed in above-mentioned universal asphalt base carbon fiber preparation process, provides a kind of universal pitch-based carbon fiber spinning oil with antistatic, lubrication and anti-stick buffer action.
Solving the problems of the technologies described above adopted scheme is that it is made up of the raw material of following proportion by weight:
Above-mentioned universal pitch-based carbon fiber spinning oil, is preferably made up of the raw material of following proportion by weight:
Above-mentioned universal pitch-based carbon fiber spinning oil, is more preferably made up of the raw material of following proportion by weight:
Above-mentioned lubricant is any one in methyl-silicone oil, ethyl silicon oil, amido silicon oil, dimethicone, methyl phenyl silicone oil; Antistatic additive is any one in polyethylene glycol, polypropylene glycol, octadecyldimethyl ethoxy quaternary ammonium nitrate, Polyethylene Glycol Oleate, wherein the mean molecule quantity of polyethylene glycol is 200,4000 or 6000, and the mean molecule quantity of polypropylene glycol is 200,400 or 600; Emulsifying agent is any one in the condensation product (model is OP-4, OP-6, OP-7) of sorbitan fatty acid ester (model is S-20, S-40, S-60, S-80 or S-85), alkyl phenol and oxirane, polyoxyethylene sorbitan monooleate, fatty alcohol-polyoxyethylene ether (model is AEO-2, AEO-3, AEO-7 or AEO-9); Equilibrium modifier is any one in methyl alcohol, acetone, dimethyl formamide, n-hexane, carbon disulfide, carbon tetrachloride.
The preparation method of universal pitch-based carbon fiber spinning oil of the present invention is: deionized water, lubricant, antistatic additive, emulsifying agent and equilibrium modifier are warming up to 30 ~ 80 DEG C under stirring, and constant temperature stirs 30 minutes, then ultrasonic 15 minutes.
The using method of universal pitch-based carbon fiber spinning oil of the present invention is: employing spray pattern finish is sprayed on as-spun fibre or pre-oxidized fibers or at carbon fiber surface, oil applying rate is 0.01% ~ 5.0%.
The viscosity of general purpose grade asphalt-based carbon fiber spinning oil of the present invention is 2 ~ 20mPa.s, light transmittance is 80% ~ 98%, be sprayed on fiber surface and can play antistatic property, make that there is between fibre single thread certain cohesive force, the effect reaching boundling stops fiber adhesion, monofilament surface forms thin finish film can play anti-stick buffer action, and protect monofilament surface at the volley from damage, and same anti-stick buffer action is also played in non-fusible and carbonisation, the easy adhesion existed can be solved in universal pitch-based carbon fiber preparation process, the problem such as electrostatic and wearing and tearing.Result of the test shows, universal pitch-based carbon fiber spinning oil of the present invention and fiber surface contact angle are 0 ~ 5 °, can be coated in fiber surface well, and fibre strength conservation rate is 95% ~ 100%, and the TENSILE STRENGTH of finish on fiber does not affect substantially.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is described in more detail, but the invention is not restricted to these embodiments.
The universal pitch-based carbon fiber spinning oil that below prepared by embodiment adopts NDJ-5S rotation viscometer (Shanghai Ping Xuan scientific instrument Co., Ltd) to measure viscosity at room temperature 25 DEG C; U-3900/3900H ultraviolet-uisible spectrophotometer (Hitachi, Ltd) is adopted to measure light transmittance; OCA20 video optics contact angle measurement (German Dataphysics company provides) is adopted to measure the contact angle of finish and asphalt surface; Place and observe finish outward appearance after three months and measure finish viscosity and light transmittance, if with freshly prepd finish outward appearance, viscosity substantially identical with light transmittance without lamination, illustrate that its stability is better; The TENSILE STRENGTH of carbon fiber and elongation at break (pre-applied force: 0.001N after adopting Q800DMA type dynamic visco-elasticity analyser (TA company of the U.S. provides) to measure to oil; 25 DEG C of constant temperature 5 minutes, the upper limit of power: 10N; Slope power: 0.03N/min; Poisson's ratio: 0.44; Fibre length 15mm, the mean value calculation with 20 monofilament), and by formula: TENSILE STRENGTH × 100% of the TENSILE STRENGTH/carbon fiber that do not oil of carbon fiber after fibre strength conservation rate=oil, calculates fibre strength conservation rate.
Embodiment 1
To prepare universal pitch-based carbon fiber spinning oil deionized water 100g used, other raw materials and quality proportioning as follows:
Its preparation method is: be that the polypropylene glycol of 200,6g sorbitan fatty acid ester S-20 and 20g acetone join successively in beaker under stirring by 100g deionized water, 2g methyl phenyl silicone oil, 5g mean molecule quantity, be warming up to 50 DEG C, constant temperature stirs 30 minutes, then supersonic wave cleaning machine is used ultrasonic 15 minutes, obtain universal pitch-based carbon fiber spinning oil, it is placed after 3 months without lamination, its viscosity is 8mPa.s after tested, light transmittance is 90%, substantially identical with light transmittance with freshly prepd finish outward appearance, viscosity, illustrate that its stability is better.
Embodiment 2
To prepare universal pitch-based carbon fiber spinning oil deionized water 100g used, other raw materials and quality proportioning as follows:
Its preparation method is identical with embodiment 1, and the finish obtained is placed without lamination after 3 months, and its viscosity is 2mPa.s after tested, and light transmittance is 85%.
Embodiment 3
To prepare universal pitch-based carbon fiber spinning oil deionized water 100g used, other raw materials and quality proportioning as follows:
Its preparation method is identical with embodiment 1, and the finish obtained is placed without lamination after 3 months, and its viscosity is 10mPa.s after tested, and light transmittance is 98%.
Embodiment 4
To prepare universal pitch-based carbon fiber spinning oil deionized water 100g used, other raw materials and quality proportioning as follows:
Its preparation method is identical with embodiment 1, and the finish obtained is placed without lamination after 3 months, and its viscosity is 20mPa.s after tested, and light transmittance is 95%.
Embodiment 5
To prepare universal pitch-based carbon fiber spinning oil deionized water 100g used, other raw materials and quality proportioning as follows:
Its preparation method is identical with embodiment 1, and the finish obtained is placed without lamination after 3 months, and its viscosity is 18mPa.s after tested, and light transmittance is 80%.
Embodiment 6
In embodiment 1 ~ 5, the amido silicon oil of the quality such as methyl phenyl silicone oil use used is replaced, mean molecule quantity to be the mean molecule quantity of the quality such as the polypropylene glycol use of 200 be 4000 polyethylene glycol replace, the alkyl phenols of quality such as sorbitan fatty acid ester S-20 use and the condensation product OP-4 of oxirane replace, the methyl alcohol of the quality such as acetone use is replaced, and is prepared into universal pitch-based carbon fiber spinning oil.
Embodiment 7
In embodiment 1 ~ 5, the methyl-silicone oil of the quality such as methyl phenyl silicone oil use used is replaced, mean molecule quantity is that the octadecyldimethyl ethoxy quaternary ammonium nitrate of the quality such as the polypropylene glycol use of 200 is replaced, the polyoxyethylene sorbitan monooleate of the quality such as sorbitan fatty acid ester S-20 use is replaced, the dimethyl formamide of the quality such as acetone use is replaced, and is prepared into universal pitch-based carbon fiber spinning oil.
Embodiment 8
In embodiment 1 ~ 5, the ethyl silicon oil of the quality such as methyl phenyl silicone oil use used is replaced, mean molecule quantity is that the Polyethylene Glycol Oleate of the quality such as the polypropylene glycol use of 200 is replaced, the fatty alcohol-polyoxyethylene ether AEO-7 of the quality such as sorbitan fatty acid ester S-20 use replaces, the n-hexane of the quality such as acetone use is replaced, and is prepared into universal pitch-based carbon fiber spinning oil.
Embodiment 9
In embodiment 1 ~ 5, the dimethicone of the quality such as methyl phenyl silicone oil use used is replaced, mean molecule quantity to be the mean molecule quantity of the quality such as the polypropylene glycol use of 200 be 600 polypropylene glycol replace, the sorbitan fatty acid ester S-80 of the quality such as sorbitan fatty acid ester S-20 use replaces, the carbon disulfide of the quality such as acetone use is replaced, and is prepared into universal pitch-based carbon fiber spinning oil.
Embodiment 10
In embodiment 1 ~ 5, mean molecule quantity used to be the mean molecule quantity of the quality such as the polypropylene glycol use of 200 be 6000 polyethylene glycol replace, the alkyl phenols of quality such as sorbitan fatty acid ester S-20 use and the condensation product OP-7 of oxirane replace, the carbon tetrachloride of the quality such as acetone use is replaced, and is prepared into universal pitch-based carbon fiber spinning oil.
What more than enumerate is only specific embodiments of the invention, and all distortion that those of ordinary skill in the art can directly derive from content disclosed by the invention or associate are all in protection scope of the present invention.
In order to prove beneficial effect of the present invention, inventor adopts spray pattern, universal pitch-based carbon fiber spinning oil prepared by embodiment 1 ~ 5 is sprayed on as-spun fibre surface respectively, and test contact angle and the fibre strength conservation rate of finish and as-spun fibre respectively, result of the test is in table 1.
Table 1 finish of the present invention oils effect
| Finish | Oil applying rate | Contact angle | Fibre strength conservation rate |
| Embodiment 1 | 0.05% | 5° | 96% |
| Embodiment 2 | 0.25% | 3° | 95% |
| Embodiment 3 | 0.35% | 0° | 100% |
| Embodiment 4 | 0.01% | 3° | 99% |
| Embodiment 5 | 0.50% | 4° | 98% |
From table 1, when oil applying rate is 0.01% ~ 5.0%, finish and fiber surface contact angle are 0 ~ 5 °, can be coated in fiber surface well, and fibre strength conservation rate is 95% ~ 100%, illustrate that the TENSILE STRENGTH of finish on fiber does not affect substantially.In addition; experimental phenomena shows; finish of the present invention can play antistatic property at fiber surface; make that there is between fibre single thread certain cohesive force; the effect reaching boundling stops fiber adhesion; monofilament surface forms thin oil film, protects its surface at the volley from damage, and also without doubling phenomena after fiber preoxidation and carbonization.
Claims (2)
1. a universal pitch-based carbon fiber spinning oil, is characterized in that it is made up of the raw material of following proportion by weight:
Above-mentioned lubricant is any one in ethyl silicon oil, amido silicon oil, dimethicone, methyl phenyl silicone oil; Antistatic additive is any one in polyethylene glycol, polypropylene glycol, octadecyldimethyl ethoxy quaternary ammonium nitrate, Polyethylene Glycol Oleate, wherein the mean molecule quantity of polyethylene glycol is 200,4000 or 6000, and the mean molecule quantity of polypropylene glycol is 200,400 or 600; Emulsifying agent is any one in the condensation product of sorbitan fatty acid ester, alkyl phenol and oxirane, polyoxyethylene sorbitan monooleate, fatty alcohol-polyoxyethylene ether; Equilibrium modifier is any one in methyl alcohol, acetone, dimethyl formamide, n-hexane, carbon disulfide, carbon tetrachloride.
2., according to universal pitch-based carbon fiber spinning oil according to claim 1, it is characterized in that it is made up of the raw material of following proportion by weight:
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| CN201310751350.7A CN103757899B (en) | 2013-12-31 | 2013-12-31 | Universal pitch-based carbon fiber spinning oil |
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| CN103757899B true CN103757899B (en) | 2016-01-20 |
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104452270A (en) * | 2014-12-19 | 2015-03-25 | 四川创越炭材料有限公司 | Spinning finish for asphalt carbon fiber |
| CN104674555B (en) * | 2015-03-06 | 2016-09-21 | 苏州爱立方服饰有限公司 | A kind of fabric antistatic treatment agent and preparation method thereof |
| CN105200789A (en) * | 2015-09-17 | 2015-12-30 | 无锡市长安曙光手套厂 | Antistatic agent and preparation method and application thereof |
| WO2017060845A1 (en) * | 2015-10-08 | 2017-04-13 | Stora Enso Oyj | A process for the manufacture of a precursor yarn |
| CN105671944B (en) * | 2016-02-25 | 2018-02-09 | 中国人民解放军国防科学技术大学 | A kind of continuous polycarbosilane fiber spinning oil and its preparation and application |
| CN109722744B (en) * | 2018-12-21 | 2021-07-09 | 中芳特纤股份有限公司 | Para-aramid oiling agent |
| CN110273300A (en) * | 2019-05-13 | 2019-09-24 | 湖南东映碳材料科技有限公司 | A kind of pitch fibers aoxidize dedicated isolation finish and its application method |
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| CN102454109A (en) * | 2010-10-21 | 2012-05-16 | 威海拓展纤维有限公司 | Method for treating carbon fiber precursor fiber and special oil agent thereof |
| CN103014922A (en) * | 2011-09-22 | 2013-04-03 | 中国科学院化学研究所 | Organosilicon spinning oil agent used for preparing polyacrylonitrile-based carbon fiber, and preparation method thereof |
| CN103122505A (en) * | 2011-11-18 | 2013-05-29 | 中国石油化工股份有限公司 | Oiling agent for small tow PAN (Polyacrylonitrile)-based carbon fiber precursors |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2001172879A (en) * | 1999-10-08 | 2001-06-26 | Sanyo Chem Ind Ltd | Oil agent for production of carbon fiber |
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| CN102454109A (en) * | 2010-10-21 | 2012-05-16 | 威海拓展纤维有限公司 | Method for treating carbon fiber precursor fiber and special oil agent thereof |
| CN103014922A (en) * | 2011-09-22 | 2013-04-03 | 中国科学院化学研究所 | Organosilicon spinning oil agent used for preparing polyacrylonitrile-based carbon fiber, and preparation method thereof |
| CN103122505A (en) * | 2011-11-18 | 2013-05-29 | 中国石油化工股份有限公司 | Oiling agent for small tow PAN (Polyacrylonitrile)-based carbon fiber precursors |
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| "用于高性能碳纤维制造的纺丝油剂的研究";黄英等;《复合材料-基础、创新、高效：第十四届全国复合材料学术会议论文集（上）》;20061015;第58-62页 * |
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