CN104452270A - Spinning finish for asphalt carbon fiber - Google Patents
Spinning finish for asphalt carbon fiber Download PDFInfo
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- CN104452270A CN104452270A CN201410798868.0A CN201410798868A CN104452270A CN 104452270 A CN104452270 A CN 104452270A CN 201410798868 A CN201410798868 A CN 201410798868A CN 104452270 A CN104452270 A CN 104452270A
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- asphalt
- carbon fiber
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- based carbon
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Abstract
The invention belongs to the technical field of spinning auxiliary for an asphalt-based carbon fiber precursor fiber, and particularly relates to a spinning finish for an asphalt carbon fiber, and the spinning finish is mainly used for solving the problems that the existing spinning finish for asphalt-based carbon fiber can be molten when used for spinning a large bundle of asphalt-based carbon fibers. According to the technical scheme, the spinning finish for asphalt carbon fiber is prepared by performing ultrasonic mixing on the following raw materials in percentage by weight for 0.5h-3h: 5%-45% of carbon powder, 3%-6% of silicone oil, 0.1%-3% of antistatic agent, 0-0.3% of cohesive agent, 0.02%-2% of wetting agent, 0-0.2% of fiber splitting agent and the balance of deionized water. The spinning finish has the following advantages that the melting phenomenon in a process of spinning a large bundle of asphalt-based carbon fibers cannot exist, the friction and wear of fiber surface and a roller during production can be prevented, and the spinning finish has good antistatic property and toughness effect.
Description
Technical field
The invention belongs to a kind of for pitch based carbon fiber precursor fiber spinning used additives technical field, be specifically related to a kind of asphalt-based carbon fiber spinning finish.
Background technology
Finish is the important auxiliary agent of production high-performance precursor and Carbon fibe, the manufacture (particularly the manufacture of High Property Carbon Fibers) of Carbon fibe has strict requirement to spinning oil: as excellent resistance to elevated temperatures, to guarantee to play can prevent again the effect of precursor adhesion by boundling at High Temperature Pre oxidation and charing initial stage; Excellent antistatic property, to give the good convergence of precursor and processability, ensures carrying out smoothly of spinning and preoxidation process; Excellent lubricity and antiseized isolation, make fiber be easy to fibrillation to play the good monofilament adhesion that prevents at spinning, pre-oxidation and charing initial stage, greatly reduce or eliminate burr, doubling and fracture of wire; The wettability excellent to Carbon fibe, to make to oil evenly, guarantees the homogeneity of precursor, oxidization fiber and carbon filament quality.
Pitch based carbon fiber can be used as the fortifying fibre of advanced composite material, is indispensable new and high technology material in space flight and aviation and national defense industry.Pitch based carbon fiber production process is by pitch fibers after finish oils, and drying makes asphalt carbon fiber precursor, non-fusible in the air of 250-350 DEG C afterwards, makes non-fusible silk, the temperature charing then in 1000 DEG C of inert gases, obtained Carbon fibe.
The domestic finish being exclusively used in the spinning of pitch based carbon fiber precursor is few at present, the finish produced for PAN based carbon fiber is relatively many, but be organosilicon finish substantially, organosilicon finish itself has excellent performance, but act on asphalt carbon fiber and have following shortcoming: because organosilyl convergence is good, connect tight between tow but 98 machine silicon can be had effectively to separate, but such finish is in the infusible process of pitch fibers, cross-linking reaction can be there is and high viscosity in organosilicon finish because of heating, the comparatively strong oil film of one deck is formed on pitch fusion-free fibre surface, due to the fragility of pitch fusion-free fibre itself, crosslinked organosilicon membrane can make fibre bundle harden, and easily brittle failure.The difficulty that this firmly crisp fibre bundle makes follow-up production become.More burr can be produced and affect the quality of final products in the process of winding.
Application publication number be CN103757899A application discloses a kind of universal pitch-based carbon fiber spinning oil, although this finish can solve in universal pitch charcoal fibre preparation process exist easy adhesion, electrostatic and friction problem, but be only applicable to little synnema scope, when synnema reaches 1K, when curing process step, there will be molten also phenomenon.
Summary of the invention
The object of the invention is to solve the technical problem that there will be molten also phenomenon when existing asphalt base carbon fiber spinning finish exists for spinning large bundle pitch based carbon fiber silk, a kind of asphalt-based carbon fiber spinning finish is provided.
For solving the problems of the technologies described above, the technical solution used in the present invention is:
A kind of asphalt-based carbon fiber spinning finish, it is made up through ultrasonic mixing 0.5h ~ 3h according to following mass percent of following raw material: carbon element powder 5%-45%, silicone oil 3%-6%, antistatic additive 0.1%-3%, obvolvent agent 0-0.3%, wetting agent 0.02%-2% and point fine agent 0-0.2%, all the other are deionized water.
Described carbon element powder be in graphite powder, modified graphite powder, carbon black or Graphene any one or a few with arbitrarily than mixture, its particle size is 0.001 μm-2 μm.
Described silicone oil be in amino-modified silicone oil, epoxy modified polysiloxane, polyether modified silicon oil, hydroxy silicon oil, methyl-silicone oil, dimethicone, ethyl silicon oil or cyanoethyl methyl polysiloxane one or more with arbitrarily than mixture.
The preparation method of described modified graphite powder is: first graphite powder and red fuming nitric acid (RFNA) are mixed with the mass ratio of 1:2-4, then 70-100 DEG C is warming up to, stir 0.5-4h continuously again, finally with distilled water graphite water powder until pH value is 5-7, obtain the modified graphite powder that oxygen content is 0.1%-0.5%
The modification ammonia mass fraction of described amino-modified silicone oil is calculated as 0.001-0.05% to hold envelope ammonia-NH2; The modification amount of described epoxy modified polysiloxane is calculated as 0.001-0.05% with epoxy radicals-CHCH2O; The modified polyether mass fraction of described polyether modified silicon oil is between 0.2-0.7%, and the degree of polymerization of the construction unit of polyethers is between 5-25.
The invention has the beneficial effects as follows: the present invention is used in the spinning production process of pitch based carbon fiber precursor fiber, can at monofilament surface homogeneous film formation, the friction and wear of fiber surface and roller in process of production can be prevented, thus effectively avoid fiber surface to produce defect, due to the electric action of carbon element powder, finish has good antistatic behaviour, and pitch fibers has enough flexibilities after about 300 DEG C non-fusible, can not brittle failure in receipts silk process.Therefore, compared with background technology, the present invention has the advantage when being used for there will not be molten also phenomenon when spinning large bundle pitch based carbon fiber silk, preventing the friction and wear of fiber surface and roller in production process, good antistatic behaviour and good increasing tougheness.
Detailed description of the invention
Embodiment 1
A kind of asphalt-based carbon fiber spinning finish in the present embodiment, it is the graphite powder of 0.001 μm-2 μm by particle diameter, polyether modified silicon oil, amino-modified silicone oil, epoxy modified polysiloxane, alkylolamides, alkyl dimethyl ethoxyl quaternary ammonium salt, obvolvent agent, octanol polyethers, amidogen ether divides the raw material of fine agent and deionized water to make through ultrasonic mixing 0.5h, the mass percent of above-mentioned each raw material is: particle diameter is the graphite powder 5% of 0.001 μm-2 μm, polyether modified silicon oil 0.5%, amino-modified silicone oil 1.5%, epoxy modified polysiloxane 1%, alkylolamides 0.05%, alkyl dimethyl ethoxyl quaternary ammonium salt 0.05% and octanol polyethers 0.02%, all the other are deionized water.
The modification ammonia mass fraction of described amino-modified silicone oil is calculated as 0.001-0.05% to hold envelope ammonia-NH2; The modification amount of described epoxy modified polysiloxane is calculated as 0.001-0.05% with epoxy radicals-CHCH2O; The modified polyether mass fraction of described polyether modified silicon oil is between 0.2-0.7%, and the degree of polymerization of the construction unit of polyethers is between 5-25.
Embodiment 2
A kind of asphalt-based carbon fiber spinning finish in the present embodiment, it is by Graphene, amino-modified silicone oil, epoxy modified polysiloxane, alkylolamides, alkyl dimethyl ethoxyl quaternary ammonium salt, obvolvent agent, octanol polyethers, amidogen ether divides the raw material of fine agent and deionized water to make through ultrasonic mixing 3h, the mass percent of above-mentioned each raw material is: Graphene 45%, amino-modified silicone oil 3.5%, epoxy modified polysiloxane 2.5%, alkylolamides 2%, alkyl dimethyl ethoxyl quaternary ammonium salt 1%, obvolvent agent 0.3%, octanol polyethers 2% and amidogen ether divide fine agent 0.2%, all the other are deionized water.The particle size of described Graphene is 0.001 μm-2 μm.
The modification ammonia mass fraction of described amino-modified silicone oil is calculated as 0.001-0.05% to hold envelope ammonia-NH2; The modification amount of described epoxy modified polysiloxane is calculated as 0.001-0.05% with epoxy radicals-CHCH2O.
Embodiment 3
A kind of asphalt-based carbon fiber spinning finish in the present embodiment, it is the graphite powder of 0.001 μm-2 μm by particle diameter, polyether modified silicon oil, amino-modified silicone oil, epoxy modified polysiloxane, fatty alcohol-polyoxyethylene ether, alkyl dimethyl ethoxyl quaternary ammonium salt, obvolvent agent, octanol polyethers, amidogen ether divides the raw material of fine agent and deionized water to make through ultrasonic mixing 1h, the mass percent of above-mentioned each raw material is: particle diameter is the graphite powder 20% of 0.001 μm-2 μm, polyether modified silicon oil 2%, amino-modified silicone oil 2%, epoxy modified polysiloxane 1%, fatty alcohol-polyoxyethylene ether 1%, alkyl dimethyl ethoxyl quaternary ammonium salt 1%, obvolvent agent 0.2%, octanol polyethers 1% and amidogen ether divide fine agent 0.1%, all the other are deionized water.
The modification ammonia mass fraction of described amino-modified silicone oil is calculated as 0.001-0.05% to hold envelope ammonia-NH2; The modification amount of described epoxy modified polysiloxane is calculated as 0.001-0.05% with epoxy radicals-CHCH2O; The modified polyether mass fraction of described polyether modified silicon oil is between 0.2-0.7%, and the degree of polymerization of the construction unit of polyethers is between 5-25.
Graphite powder in above-described embodiment and Graphene can also be that any one in 0.001 μm-2 μm modified graphite powder or carbon black replaces with particle diameter, the preparation method of described modified graphite powder is: first graphite powder and red fuming nitric acid (RFNA) are mixed with the mass ratio of 1:2-4, then 70-100 DEG C is warming up to, stir 0.5-4h continuously again, finally with distilled water graphite water powder until pH value is 5-7, obtain the modified graphite powder that oxygen content is 0.1%-0.5%.
Alkylolamides in above-described embodiment and fatty alcohol-polyoxyethylene ether can also replace with polyoxyethylene carboxylate.
Alkyl dimethyl ethoxyl quaternary ammonium salt in above-described embodiment can also replace by methyl Trihydroxyethyl quaternary ammonium salt.
Claims (5)
1. an asphalt-based carbon fiber spinning finish, it is characterized in that: it is made up through ultrasonic mixing 0.5h ~ 3h according to following mass percent of following raw material: carbon element powder 5%-45%, silicone oil 3%-6%, antistatic additive 0.1%-3%, obvolvent agent 0-0.3%, wetting agent 0.02%-2% and point fine agent 0-0.2%, all the other are deionized water.
2. a kind of asphalt-based carbon fiber spinning finish according to claim 1, it is characterized in that: described carbon element powder be in graphite powder, modified graphite powder, carbon black or Graphene any one or a few with arbitrarily than mixture, its particle size is 0.001 μm-2 μm.
3. a kind of asphalt-based carbon fiber spinning finish according to claim 1, is characterized in that: described silicone oil be in amino-modified silicone oil, epoxy modified polysiloxane, polyether modified silicon oil, hydroxy silicon oil, methyl-silicone oil, dimethicone, ethyl silicon oil or cyanoethyl methyl polysiloxane one or more with arbitrarily than mixture.
4. a kind of asphalt-based carbon fiber spinning finish according to claim 2, it is characterized in that: the preparation method of described modified graphite powder is: first graphite powder and red fuming nitric acid (RFNA) are mixed with the mass ratio of 1:2-4, then 70-100 DEG C is warming up to, stir 0.5-4h continuously again, finally with distilled water graphite water powder until pH value is 5-7, obtain the modified graphite powder that oxygen content is 0.1%-0.5%.
5. a kind of asphalt-based carbon fiber spinning finish according to claim 3, is characterized in that: the modification ammonia mass fraction of described amino-modified silicone oil is calculated as 0.001-0.05% to hold envelope ammonia-NH2; The modification amount of described epoxy modified polysiloxane is calculated as 0.001-0.05% with epoxy radicals-CHCH2O; The modified polyether mass fraction of described polyether modified silicon oil is between 0.2-0.7%, and the degree of polymerization of the construction unit of polyethers is between 5-25.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201410798868.0A CN104452270A (en) | 2014-12-19 | 2014-12-19 | Spinning finish for asphalt carbon fiber |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410798868.0A CN104452270A (en) | 2014-12-19 | 2014-12-19 | Spinning finish for asphalt carbon fiber |
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| CN104452270A true CN104452270A (en) | 2015-03-25 |
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| CN201410798868.0A Pending CN104452270A (en) | 2014-12-19 | 2014-12-19 | Spinning finish for asphalt carbon fiber |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106521965A (en) * | 2016-11-04 | 2017-03-22 | 华峰重庆氨纶有限公司 | Ultra-strong antistatic spandex spinning oil and preparation method thereof |
| CN110195272A (en) * | 2019-05-21 | 2019-09-03 | 湖南东映碳材料科技有限公司 | A kind of method that Mesophase Pitch Fiberss oil |
| CN110241483A (en) * | 2019-05-21 | 2019-09-17 | 湖南东映碳材料科技有限公司 | A kind of method of Mesophase Pitch Fiberss rapid preoxidation |
| 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 |
| CN110608369A (en) * | 2019-09-20 | 2019-12-24 | 华东理工大学 | Heavy oil three-layer liquid forming method |
| CN111020748A (en) * | 2019-11-11 | 2020-04-17 | 上海高强高模新材料科技有限公司 | Pre-oxidation method of mesophase pitch fiber |
| CN111137881A (en) * | 2019-12-27 | 2020-05-12 | 北京光华纺织集团有限公司 | Siloxane modified graphene oxide, spandex spinning oil agent and preparation method thereof |
| CN111851073A (en) * | 2020-07-14 | 2020-10-30 | 科凯精细化工（上海）有限公司 | Antistatic spinning oil and preparation method thereof |
| CN113481721A (en) * | 2021-07-15 | 2021-10-08 | 杭州恒吉新材料科技有限公司 | Chemical fiber oiling agent composition for POY production and preparation method thereof |
| JP7018237B1 (en) | 2021-12-02 | 2022-02-10 | 竹本油脂株式会社 | Carbon fiber precursor treatment agent, carbon fiber precursor treatment agent-containing composition, and carbon fiber precursor |
| CN115787305A (en) * | 2022-11-18 | 2023-03-14 | 北京宝冠助剂有限公司 | Carbon fiber precursor oiling agent and preparation method thereof |
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| JPH0351319A (en) * | 1989-07-18 | 1991-03-05 | Mitsubishi Kasei Corp | Treating agent for pitch-based carbon fiber |
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| CN103122585A (en) * | 2011-11-18 | 2013-05-29 | 中国石油化工股份有限公司 | Oiling agent of large tow PAN (Polyacrylonitrile)-based carbon fiber precursors |
| CN103757899A (en) * | 2013-12-31 | 2014-04-30 | 陕西师范大学 | General grade pitch-based carbon fiber spinning oil |
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2014
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Patent Citations (4)
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| JPH0351319A (en) * | 1989-07-18 | 1991-03-05 | Mitsubishi Kasei Corp | Treating agent for pitch-based carbon fiber |
| JP2010007216A (en) * | 2008-06-30 | 2010-01-14 | Mitsubishi Rayon Co Ltd | Oil solution composition for carbon fiber precursor acrylic fiber, carbon fiber precursor acrylic fiber bundle, and method of production thereof |
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Cited By (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106521965B (en) * | 2016-11-04 | 2019-01-25 | 华峰重庆氨纶有限公司 | A kind of superpower antistatic urethane elastic fiber spinning oil and preparation method thereof |
| CN106521965A (en) * | 2016-11-04 | 2017-03-22 | 华峰重庆氨纶有限公司 | Ultra-strong antistatic spandex spinning oil and preparation method thereof |
| 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 |
| CN110195272A (en) * | 2019-05-21 | 2019-09-03 | 湖南东映碳材料科技有限公司 | A kind of method that Mesophase Pitch Fiberss oil |
| CN110241483A (en) * | 2019-05-21 | 2019-09-17 | 湖南东映碳材料科技有限公司 | A kind of method of Mesophase Pitch Fiberss rapid preoxidation |
| CN110195272B (en) * | 2019-05-21 | 2021-06-08 | 湖南东映碳材料科技有限公司 | Method for oiling mesophase pitch fibers |
| CN110241483B (en) * | 2019-05-21 | 2021-08-31 | 湖南东映碳材料科技有限公司 | Method for quickly pre-oxidizing mesophase pitch fibers |
| CN110608369A (en) * | 2019-09-20 | 2019-12-24 | 华东理工大学 | Heavy oil three-layer liquid forming method |
| CN111020748B (en) * | 2019-11-11 | 2022-06-24 | 上海高强高模新材料科技有限公司 | Pre-oxidation method of mesophase pitch fibers |
| CN111020748A (en) * | 2019-11-11 | 2020-04-17 | 上海高强高模新材料科技有限公司 | Pre-oxidation method of mesophase pitch fiber |
| CN111137881A (en) * | 2019-12-27 | 2020-05-12 | 北京光华纺织集团有限公司 | Siloxane modified graphene oxide, spandex spinning oil agent and preparation method thereof |
| CN111851073A (en) * | 2020-07-14 | 2020-10-30 | 科凯精细化工（上海）有限公司 | Antistatic spinning oil and preparation method thereof |
| CN113481721A (en) * | 2021-07-15 | 2021-10-08 | 杭州恒吉新材料科技有限公司 | Chemical fiber oiling agent composition for POY production and preparation method thereof |
| JP7018237B1 (en) | 2021-12-02 | 2022-02-10 | 竹本油脂株式会社 | Carbon fiber precursor treatment agent, carbon fiber precursor treatment agent-containing composition, and carbon fiber precursor |
| WO2023100711A1 (en) * | 2021-12-02 | 2023-06-08 | 竹本油脂株式会社 | Treatment agent for carbon fiber precursor, composition containing treatment agent for carbon fiber precursor, and carbon fiber precursor |
| JP2023082425A (en) * | 2021-12-02 | 2023-06-14 | 竹本油脂株式会社 | Carbon fiber precursor treatment agent, carbon fiber precursor treatment agent-containing composition, and carbon fiber precursor |
| CN115787305A (en) * | 2022-11-18 | 2023-03-14 | 北京宝冠助剂有限公司 | Carbon fiber precursor oiling agent and preparation method thereof |
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Application publication date: 20150325 |