CN110273300A - A kind of pitch fibers aoxidize dedicated isolation finish and its application method - Google Patents
A kind of pitch fibers aoxidize dedicated isolation finish and its application method Download PDFInfo
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- CN110273300A CN110273300A CN201910392247.5A CN201910392247A CN110273300A CN 110273300 A CN110273300 A CN 110273300A CN 201910392247 A CN201910392247 A CN 201910392247A CN 110273300 A CN110273300 A CN 110273300A
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- Prior art keywords
- pitch fibers
- finish
- aoxidize
- oil
- pitch
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Classifications
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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
-
- 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
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/73—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof
- D06M11/74—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof with carbon or graphite; with carbides; with graphitic acids or their salts
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/10—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
- D06M13/165—Ethers
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/10—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
- D06M13/184—Carboxylic acids; Anhydrides, halides or salts thereof
- D06M13/207—Substituted carboxylic acids, e.g. by hydroxy or keto groups; Anhydrides, halides or salts thereof
- D06M13/21—Halogenated carboxylic acids; Anhydrides, halides or salts thereof
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/643—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain
- D06M15/657—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain containing fluorine
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- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Inorganic Fibers (AREA)
Abstract
The present invention relates to a kind of pitch fibers to aoxidize dedicated isolation finish and its application method.The mass percentage of each ingredient are as follows: fluoroalkyl polyoxy silane 10-40wt%, fluorine-containing emulsifier 0.5-5wt%, organic oxidation accelerator 0.05-10wt%, nanoscale charcoal oxygenerating solid particle interleaving agent 0.05-5wt%, ethyl alcohol 5-50wt%, remaining is deionized water.Finish is isolated using the lotion for being preceding configured to solid content 1-5wt%, oil in spinning clustering process or pitch fibers boundling after immerse ultrasonication 0.2-1min re-dry acquisition in lotion and oil pitch fibers beam.Thermal stability of the present invention is good, with the spreadability of pitch fibers it is good, oil after pitch fibers beam drying time it is short, oxidization time is short, molten and probability is low.Solve the disadvantage that spinning oil and pitch fibers poor compatibility are especially easy delay heat release and influence graphite microcrystal in subsequent high temperature treatment process to arrange.
Description
Technical field
The invention belongs to pitch fibers to aoxidize oil solution dedicated field, and in particular to it is a kind of pitch fibers oxidation stage can be with
It is effectively isolated fiber and avoids molten pitch fibers protection finish and its application method simultaneously.
Background technique
Asphalt base carbon fiber has high thermal conductivity, the characteristic of high-modulus, the jewel being known as on carbon fiber field imperial crown.It is made
Standby technique generally uses the spinning of mesophase pitch melt extruded and pitch strand is made in boundling, then through oxidation, charing, graphitization etc.
Asphalt base carbon fiber beam and graphite fibre beam is made in process.Because pitch fibers brittleness is big, intensity is extremely low (5-10MPa), spinning
Journey, which needs to carry out fiber boundling, just can be carried out the oxidation of next stage, but generally commercially available finish be mainly used for boundling, antistatic,
Smooth reduction friction etc., but up to 300 DEG C when pitch fibers aoxidize of technological temperature, such as general silicone oil system oil cannot be coped with
Although agent can sprawl to form good protective film in fiber surface, in the drying process, because the difference of mass-transfer efficiency is easily
Form non-uniform oil film.And when carrying out high-temperature oxydation, thicker oil film not only hinders the diffusion of oxygen, and oil film oxidation itself is also
Chap is easily formed, causes the chap layer of oxidized fibre to form stress and concentrates, easily brittle failure.In oxidation process, pitch fibers beam
It not only needs to keep preferable boundling form, it is also necessary to which finish forms uniform isolation film, isolation film in each fiber surface
Play the role of protection in fibre bundle transmission process, need to prevent fiber very exothermic in oxidation process, avoids fiber molten
And.
In subsequent high temperature heat treatment process, the inorganic elements such as metallic impurity elements, phosphorus sulphur can be all catalyzed asphalt-based carbon fiber
The development of graphite microcrystal and then the arrangement for influencing graphite fibre crystallite, cause performance to decline, therefore the composition of pitch fibers finish
It needs to reduce the miscellaneous elements such as poisonous metal, phosphorus sulphur as far as possible.
At present market conventional spinning oil cannot function as pitch fibers oxidation it is oil solution dedicated, main cause includes thermal stability
It is universal it is poor, with the contact angle of pitch fibers it is excessive, oil after finish slow drying speed cause oil film thickness unevenness, containing largely having
Evil element etc..
Chen Long mesophase pitch-based carbon fibers spinning oil and its post-processing research Beijing (D): Beijing University of Chemical Technology,
2010. have studied phenyl silicone oil, amido silicon oil, dimethicone configuration influence of the spinning oil to oxidation technology, discovery cream
SiClx oil and pitch fibers contact angle are larger, are unfavorable for forming a film, and oil film slows down the heat release of pitch fibers, heat easy to form
It is molten simultaneously in turn result in fiber for point.
Patent 201310751350.7 discloses a kind of pitch fibers spinning oil, the ethyl silicon oil of use, amido silicon oil,
Dimethicone, methyl phenyl silicone oil all have preferable thermal stability, but the thermal stability of other surfaces activating agent is relatively low, after
It is molten simultaneously in turn result in fiber for the easily heat build-up due to decomposition of itself in continuous oxidation technology；Also, this lotion is in pitch fibers
Also easily break lotion after oiling during moisture drying and balance to form oil film thickness unevenness in surface.The equilibrium modifier of use
For any one in methanol, acetone, dimethylformamide, n-hexane, carbon disulfide, carbon tetrachloride, mix with pitch part,
It is particularly unsuitable for soluble mesophase pitch.
Summary of the invention
Present invention is generally directed to be not easy to sprawl existing for existing pitch fibers spinning oil (big with pitch fibers contact angle),
Thermal stability is poor, obstruction aoxidizes, it is molten to easily cause and the problem of waiting a series of interference pitch fibers to aoxidize and easy containing harmful element
The problem of destroying the arrangement of high-temperature heat treatment crystallite, provide it is a kind of without harmful element, low-temperature oxidation can be effectively facilitated avoid height
Warm spot, fine heat-resisting performance and the dedicated isolation finish of pitch fibers oxidation operation and its user that can effectively sprawl film forming
Method.
The technical solution that the present invention takes to achieve the above object are as follows:
A kind of dedicated isolation finish of pitch fibers oxidation, is grouped as by the group without metal, phosphorus element sulphur.
Wherein fluoroalkyl polyoxy silane 10-40wt%, fluorine-containing emulsifier 0.5-5wt%, organic oxidation accelerator 0.05-
10wt%, nanoscale charcoal oxygenerating solid particle interleaving agent 0.05-5wt%, ethyl alcohol 5-50wt%, remaining be deionized water.
The fluoroalkylpolysiloxane is closed by the quality of 1-3:1 than water-bath using containing carboxylic acid fluoride and amido silicon oil
At fluoroalkyl mass fraction accounts for 40% or more, molecular weight 40000-120000.
The preferred perfluoroalkyl ethyoxyl ether alcohol of the fluorine-containing emulsifier, perfluorooctanoic acid.
The organic oxidation accelerator is one or more of halogenated carboxylic acid mixture, preferably ten trifluoros octanoic acid.
The nanoscale charcoal oxygenerating solid particle interleaving agent is that 270 DEG C of softening point or more of mesophase pitch is milled to
Below 2000 mesh, 50wt% perchloric acid, 68wt% nitric acid 1-2:5-10:2-5 in mass ratio mixed, airtight heating to 30-
80 DEG C of reaction 1-10hr, then wash suction filtration and ammoniate water washing to pH > 10, ethyl alcohol dissolution is added, lysate removal ethyl alcohol obtains
Obtain ethanol soluble nanoscale charcoal oxygenerating solid particle interleaving agent.
The dedicated isolation finish can oil in spinning clustering process, and inventive formulation is configured to solid content 1-
The dedicated isolation finish emulsion of 5wt%, is oiled in pitch fibers clustering process using oiling roller, after boundling 30-50 DEG C of drying be
It can get the pitch fibers beam that oils.
(boundling can be carried out using common finish such as Tween 80) after being also possible to pitch fibers boundling, immerse solid content 1-
In the dedicated isolation finish emulsion of 5wt%, ultrasonic oscillation is provided in finish emulsion, processing 0.2-1min passes through draw roll again
It is dry to obtain the pitch fibers beam that oils.
The present invention by adopting the above technical scheme, compared with prior art, has the advantages that
(1) it is made of main finish, oxidation accelerator, the solid particle of better heat stability, other helper component contents are non-
It is often low, it not only ensure that finish in the thermal stability of the formed oil film in pitch fibers surface, moreover it is possible to effectively avoid auxiliary surface living
Property agent thermal decomposition heat release cause it is molten simultaneously；
(2) spreadability of fluoroalkyl polyoxy silane and pitch fibers is good, the 1-5wt% solid content emulsion contacts finally configured
Angle can achieve 3-10 °；
(3) without to the harmful metal of subsequent high temperature graphitization processing, phosphorus sulphur impurity；
(4) the pitch fibers drying time after oiling is short, effectively reduces finish quadratic distribution, and form a film good evenness；
(5) use of oxidation accelerator makes that the pitch fibers oxidization time after oiling is short, temperature is low, effectively reduces molten and general
Rate.
Detailed description of the invention
Fig. 1 is that the embodiment of the present invention 1 oils 100,000 times of 1 surface of pitch fibers shape appearance figure；
Fig. 2 is that the embodiment of the present invention 2 oils 100,000 times of 1 surface of pitch fibers shape appearance figure.
Specific embodiment
Embodiment 1
A kind of pitch fibers aoxidize dedicated isolation finish, wherein fluoroalkyl polyoxy silane 30wt%, perfluoroalkyl ethyoxyl
Ether alcohol 2wt%, ten trifluoro octanoic acid 10wt%, nanoscale charcoal oxygenerating solid particle interleaving agent 2wt%, ethyl alcohol 30wt%, remaining
For deionized water.
Fluoroalkylpolysiloxane is closed using ten trifluoro octanoic acids and commercially available amido silicon oil in 80 DEG C of water-baths of ratio of 3:1
At gained fluoroalkyl mass fraction accounts for 52%, molecular weight 65000.
Nanoscale charcoal oxygenerating solid particle interleaving agent is that 275 DEG C of softening point of naphthalene system mesophase pitch is milled to 2000
Mesh, 50% perchloric acid, 68% nitric acid 1:5:5 in mass ratio are mixed, airtight heating to 60 DEG C of reaction 10hr, then wash suction filtration
And water washing is ammoniated to pH > 10, excess ethyl alcohol dissolution is added, gained lysate removes ethyl alcohol and obtains ethanol soluble nanoscale charcoal
Oxygenerating solid particle interleaving agent.
Inventive formulation is added to the deionized water and alcohol mixed solution of mass ratio 1:1, is configured to solid content 2wt%'s
Dedicated isolation finish emulsion, and 3.5 ° of pitch fibers contact angle, lotion impregnates 15 days without obvious muddy with precipitating.
It oils in pitch fibers clustering process using two oiling rollers are two-sided, entire tow spool is dried at 45 DEG C after boundling
30min obtains the pitch fibers beam that oils.
Gained oils oil film dense uniform under pitch fibers beam Electronic Speculum, and oxidization time can be with compared with the pitch fibers that do not oil
Shorten 30min.
Embodiment 2
A kind of pitch fibers aoxidize dedicated isolation finish, wherein fluoroalkyl polyoxy silane 20wt%, perfluoroalkyl ethyoxyl
Ether alcohol 3wt%, ten trifluoro octanoic acid 8wt%, nanoscale charcoal oxygenerating solid particle interleaving agent 3wt%, ethyl alcohol 20wt%, remaining be
Deionized water.
Fluoroalkylpolysiloxane is synthesized using perfluor certain herbaceous plants with big flowers acid and commercially available amido silicon oil in 80 DEG C of water-baths of ratio of 1:1,
Gained fluoroalkyl mass fraction accounts for 40%, molecular weight 70000.
Nanoscale charcoal oxygenerating solid particle interleaving agent is that 275 DEG C of softening point of naphthalene system mesophase pitch is milled to 2000
Mesh, 50% perchloric acid, 68% nitric acid 1:3:5 in mass ratio are mixed, airtight heating to 80 DEG C of reaction 8hr, then wash suction filtration
And water washing is ammoniated to pH > 10, excess ethyl alcohol dissolution is added, gained lysate removes ethyl alcohol and obtains ethanol soluble nanoscale charcoal
Oxygenerating solid particle interleaving agent.
Inventive formulation is added to the deionized water and alcohol mixed solution of mass ratio 1:2, is configured to solid content 4wt%'s
Dedicated isolation finish emulsion, and 3 ° of pitch fibers contact angle, lotion impregnates 15 days without obvious muddy with precipitating.
Pitch fibers carry out boundling using Tween 80, and fibre bundle crosses de-ionized water tank cleaning first, then immerses solid content 4%
Dedicated isolation finish emulsion in, ultrasonic oscillation handles 0.5min, and, winding dry finally by draw roll obtains upper oil asphalt
Fibre bundle.Gained oils oil film dense uniform under pitch fibers beam Electronic Speculum, and oxidization time can be with compared with the pitch fibers that do not oil
Shorten 20min.
Embodiment 3
A kind of pitch fibers aoxidize dedicated isolation finish, wherein fluoroalkyl polyoxy silane 20wt%, perfluorooctanoic acid
1.5wt%, ten trifluoro octanoic acid 10wt%, nanoscale charcoal oxygenerating solid particle interleaving agent 3wt%, ethyl alcohol 20wt%, remaining be
Deionized water.
Fluoroalkylpolysiloxane is synthesized using perfluor certain herbaceous plants with big flowers acid and commercially available amido silicon oil in 80 DEG C of water-baths of ratio of 1:1,
Gained fluoroalkyl mass fraction accounts for 40%, molecular weight 70000.
Nanoscale charcoal oxygenerating solid particle interleaving agent is that 275 DEG C of softening point of naphthalene system mesophase pitch is milled to 2000
Mesh, 50% perchloric acid, 68% nitric acid 1:3:5 in mass ratio are mixed, airtight heating to 80 DEG C of reaction 8hr, then wash suction filtration
And water washing is ammoniated to pH > 10, excess ethyl alcohol dissolution is added, gained lysate removes ethyl alcohol and obtains ethanol soluble nanoscale charcoal
Oxygenerating solid particle interleaving agent.
Inventive formulation is added to the deionized water and alcohol mixed solution of mass ratio 1:2, is configured to solid content 4wt%'s
Dedicated isolation finish emulsion, and 3 ° of pitch fibers contact angle, lotion impregnates 15 days without obvious muddy with precipitating.
Pitch fibers carry out boundling using Tween 80, and fibre bundle crosses de-ionized water tank cleaning first, then immerses solid content 4%
Dedicated isolation finish emulsion in, ultrasonic oscillation handles 0.5min, and, winding dry finally by draw roll obtains upper oil asphalt
Fibre bundle.The gained pitch fibers beam oxidization time that oils can shorten 20min compared with the pitch fibers that do not oil.
Claims (6)
1. a kind of pitch fibers aoxidize dedicated isolation finish, it is characterised in that the mass percentage of each ingredient are as follows: fluoroalkyl is poly-
Oxosilane 10-40wt%, fluorine-containing emulsifier 0.5-5wt%, organic oxidation accelerator 0.05-10wt%, nanoscale charcoal oxygen
Change solid particle interleaving agent 0.05-5wt%, ethyl alcohol 5-50wt%, remaining be deionized water, the fluoroalkylpolysiloxane,
It being synthesized by the quality of 1-3:1 than water-bath using containing carboxylic acid fluoride with amido silicon oil, fluoroalkyl mass fraction accounts for 40% or more, point
Son amount 40000-120000.
2. a kind of pitch fibers according to claim 1 aoxidize dedicated isolation finish, it is characterised in that: the fluorine-containing emulsification
Agent is perfluoroalkyl ethyoxyl ether alcohol or perfluorooctanoic acid.
3. a kind of pitch fibers according to claim 1 aoxidize dedicated isolation finish, it is characterised in that: the organic
Oxidation accelerator is one or more of halogenated carboxylic acid mixture.
4. a kind of pitch fibers according to claim 1 aoxidize dedicated isolation finish, it is characterised in that: the organic
Oxidation accelerator is that halogenated carboxylic acid is ten trifluoros octanoic acid.
5. a kind of pitch fibers according to claim 1 aoxidize dedicated isolation finish, it is characterised in that: the nanoscale
Charcoal oxygenerating solid particle interleaving agent is that 270 DEG C of softening point or more of mesophase pitch is milled to 2000 mesh or less, 50% high chlorine
Acid, 68% nitric acid 1-2:5-10:2-5 in mass ratio are mixed, airtight heating to 30-80 DEG C of reaction 1-10hr, then wash pumping
It filters and ammoniates water washing to pH > 10, ethyl alcohol dissolution is added, lysate removes ethyl alcohol and obtains ethanol soluble nanoscale charcoal oxygenerating
Solid particle interleaving agent.
6. a kind of pitch fibers described in -5 aoxidize the application method of dedicated isolation finish according to claim 1, it is characterised in that:
The isolation finish is that the deionized water of 1:0.1-10 and alcohol mixed solution are configured to solid content 1- using preceding addition mass ratio
The lotion of 5wt%, oil in spinning clustering process or pitch fibers boundling after immerse lotion in ultrasonication 0.2-
1min re-dry obtains the pitch fibers beam that oils；The solid content refers to that finish, remaining matter after 100 DEG C of dry 1hr is isolated in 1g
Amount.
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| CN201910392247.5A CN110273300A (en) | 2019-05-13 | 2019-05-13 | A kind of pitch fibers aoxidize dedicated isolation finish and its application method |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS62110923A (en) * | 1985-11-07 | 1987-05-22 | Nitto Boseki Co Ltd | Infusibilization of pitch fiber |
| JPS62289616A (en) * | 1986-06-09 | 1987-12-16 | Toa Nenryo Kogyo Kk | Production of carbon and graphite fiber |
| CN103757899A (en) * | 2013-12-31 | 2014-04-30 | 陕西师范大学 | General grade pitch-based carbon fiber spinning oil |
| 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 |
| CN107904698A (en) * | 2017-11-07 | 2018-04-13 | 东华大学 | A kind of preparation method of asphalt base carbon fiber |
-
2019
- 2019-05-13 CN CN201910392247.5A patent/CN110273300A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS62110923A (en) * | 1985-11-07 | 1987-05-22 | Nitto Boseki Co Ltd | Infusibilization of pitch fiber |
| JPS62289616A (en) * | 1986-06-09 | 1987-12-16 | Toa Nenryo Kogyo Kk | Production of carbon and graphite fiber |
| CN103757899A (en) * | 2013-12-31 | 2014-04-30 | 陕西师范大学 | General grade pitch-based carbon fiber spinning oil |
| 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 |
| CN107904698A (en) * | 2017-11-07 | 2018-04-13 | 东华大学 | A kind of preparation method of asphalt base carbon fiber |
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