CN110396732A - A kind of processing technology of modified carbon fiber - Google Patents
A kind of processing technology of modified carbon fiber Download PDFInfo
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- CN110396732A CN110396732A CN201910784000.8A CN201910784000A CN110396732A CN 110396732 A CN110396732 A CN 110396732A CN 201910784000 A CN201910784000 A CN 201910784000A CN 110396732 A CN110396732 A CN 110396732A
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- carbon fiber
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
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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
- 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
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- 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
- D06M10/00—Physical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. ultrasonic, corona discharge, irradiation, electric currents, or magnetic fields; Physical treatment combined with treatment with chemical compounds or elements
- D06M10/02—Physical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. ultrasonic, corona discharge, irradiation, electric currents, or magnetic fields; Physical treatment combined with treatment with chemical compounds or elements ultrasonic or sonic; Corona discharge
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- 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
- D06M13/322—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 nitrogen
- D06M13/35—Heterocyclic compounds
- D06M13/352—Heterocyclic compounds having five-membered heterocyclic rings
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- 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
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/40—Fibres of carbon
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- Chemical & Material Sciences (AREA)
- Textile Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Metallurgy (AREA)
- Materials Engineering (AREA)
- Electrochemistry (AREA)
- Physics & Mathematics (AREA)
- Plasma & Fusion (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
- Inorganic Fibers (AREA)
Abstract
The invention discloses a kind of processing technologys of modified carbon fiber, comprising the following steps: step a, moves back a line concentration, chooses precursor, connect Xin Si using heat resistance fiber with old silk after beam splitting, and be set up on line collecting plate;Step b, just dry, line collecting plate is sent into moisture dry in drying equipment, to contain in elimination precursor together with precursor;Step c, it pre-oxidizes;Step d, it carbonizes;Step e, electrolytic oxidation is modified;Step f, it impregnates and is modified.Beneficial effect is: 1, by using the mode of electrolytic oxidation, carbon fiber surface is modified, active function groups are introduced on the surface of carbon fiber, increase the carbon-oxygen bond of carbon fiber surface, the tightness contacted in recombination process with composite material surface is improved, the increase and decrease shear strength of synthetic composite material is improved;2, the interface binding power for improving faying face, to improve the tensile strength and impact strength of carbon fiber Yu resin base material composite material.
Description
Technical field
The present invention relates to carbon fiber production technical fields, and in particular to a kind of processing technology of modified carbon fiber.
Background technique
Carbon fiber be it is a kind of with high temperature resistant, anti-friction, conductive, thermally conductive and the characteristics such as corrosion-resistant fibrous novel-section
Material, can be processed as fabric or be compounded to form the composite material haveing excellent performance with organic material.In the prior art, carbon fiber is common
It is compound to make the progress such as reinforcing material and resin, metal, ceramics and charcoal, is processed into high-intensitive composite material, wherein carbon fiber
The specific strength and specific modulus of reinforced epoxy composite material are highest in existing engineering material.Due to carbon fiber surface light
It is sliding, after being that reinforcing material is compound, tend not to be in close contact with composite material, the performance of the composite material after leading to synthesis compared with
Difference.
Summary of the invention
The object of the invention is that a kind of processing technology of modified carbon fiber is provided to solve the above-mentioned problems, this hair
Preferred technical solution includes raising carbon fiber surface activity in many technical solutions of bright offer, improves itself and reinforcing material
In conjunction with tightness, improve the technical effects such as the performance of composite material, elaboration as detailed below.
To achieve the above object, the present invention provides following technical schemes:
A kind of processing technology of modified carbon fiber provided by the invention, comprising the following steps:
Step a, a line concentration is moved back, precursor is chosen, connect Xin Si using heat resistance fiber with old silk after beam splitting, and be set up in line concentration
On plate;
Step b, just dry, line collecting plate is sent into moisture dry in drying equipment, to contain in elimination precursor together with precursor;
Step c, it pre-oxidizes, the precursor after drying is sent into pre-oxidation furnace together with precursor and is pre-oxidized, pre-oxidation furnace is continuous
It is provided with 3, and the temperature range of three pre-oxidation furnaces is respectively 200 DEG C -230 DEG C, 220 DEG C -250 DEG C, 235 DEG C -245 DEG C,
Precursor through pre-oxidizing is converted into trapezium structure by linear molecule chain, and preoxidation time 75-110min ultimately forms pre- oxygen
Silk;
Step d, it carbonizes, the oxidization fiber after pre-oxidation is successively subjected to low-temperature carbonization and high temperature carbonization, wherein in low-temperature carbonization furnace
If 5 temperature ranges, respectively 350 DEG C, 450 DEG C, 550 DEG C, 650 DEG C, 750 DEG C;6 temperature ranges are set in high temperature carbonization furnace,
Respectively 1050 DEG C, 1150 DEG C, 1250 DEG C, 1350 DEG C, 1450 DEG C, 1400 DEG C form random layer after charing, inside oxidization fiber
Graphite-structure, and deviate from small molecule, form the charing silk with certain drafting force;
Step e, electrolytic oxidation is modified, will carbonize silk and carry out once as the first electrolyte bath for being loaded with causticity alkaline electrolyte
Electrolytic oxidation is modified, and the pH value of electrolyte is 9-11, and current density is 1.5-2.5A/ ㎡;After silk taking-up drying will then be carbonized,
Re-electrolysis oxidation modification is carried out as the second electrolyte bath for filling weak base electrolyte, the pH value of the weak base electrolyte is
7.5-8, current density 0.5-1A then take out drying, form primary modified carbon fiber;
Step f, it impregnates and is modified, make primary modified carbon fiber wash with distilled water, then dry, obtain clean primary modified carbon fiber
Clean primary modified carbon fiber is then placed in the dopamine hydrochloric acid solution of pH value 8-9, persistently stirs 16-24h, take out by dimension
It cleans, the modified carbon fiber in surface can be obtained after drying.
Preferably, just dry to use horizontal kiln, drying temperature is 80 DEG C -100 DEG C in the step b.
Preferably, three retorts are continuously arranged in the step c, and are interconnected, the precursor after drying is being conveyed
Successively carry out continuously carbonizings by three retorts under the conveying of equipment, the carbonization time in three retorts be respectively 30min,
30min and 40min, total 100min.
Preferably, once electrolytic oxidation modification and re-electrolysis oxidation modification time are 2min- in the step e
5min, the first electrolytic cell and the second electrolyte bath temperature are 30 DEG C -50 DEG C.
Preferably, the drying mode in the step e is vacuum drying, drying time 60min-80min.
Preferably, cleaning process is rinsed using deionized water in the step f, cleaning process continues to water for cleaning
Become colorless pellucidity.
Preferably, drying equipment is drying box in the step f, drying temperature is 60 DEG C, drying time 1h.
To sum up, the beneficial effects of the present invention are: 1, by using the mode of electrolytic oxidation, carbon fiber surface is changed
Property, active function groups are introduced on the surface of carbon fiber, increase the carbon-oxygen bond of carbon fiber surface, are improved in recombination process and multiple
The tightness of condensation material surface contact, improves the increase and decrease shear strength of synthetic composite material;
2, twice-modified to carbon fiber progress using dopamine hydrochloric acid solution after electrolytic oxidation, it can be formed in carbon fiber surface more
Bar amine coating, increases the roughness of carbon fiber surface, with resin base material compound tense, connecing for carbon fiber and resin base material can be improved
Contacting surface product, so that the interface binding power of faying face is improved, to improve in conjunction with resin base material by the functional group of dopamine
The tensile strength and impact strength of carbon fiber and resin base material composite material.
Specific embodiment
To make the object, technical solutions and advantages of the present invention clearer, technical solution of the present invention will be carried out below
Detailed description.Obviously, described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Base
Embodiment in the present invention, those of ordinary skill in the art are obtained all without making creative work
Other embodiment belongs to the range that the present invention is protected.
The present invention provides a kind of processing technologys of modified carbon fiber, comprising the following steps:
Step a, a line concentration is moved back, precursor is chosen, connect Xin Si using heat resistance fiber with old silk after beam splitting, and be set up in line concentration
On plate;
Step b, just dry, line collecting plate is sent into moisture dry in drying equipment, to contain in elimination precursor together with precursor, so as to
It is preferably reacted after precursor enters pre-oxidation furnace;Just dry to use horizontal kiln, drying temperature is 80 DEG C -100 DEG C;
Step c, it pre-oxidizes, the precursor after drying is sent into pre-oxidation furnace together with precursor and is pre-oxidized, pre-oxidation furnace is continuous
It is provided with 3, and the temperature range of three pre-oxidation furnaces is respectively 200 DEG C -230 DEG C, 220 DEG C -250 DEG C, 235 DEG C -245 DEG C,
Precursor through pre-oxidizing is converted into trapezium structure by linear molecule chain, and preoxidation time 75-110min ultimately forms pre- oxygen
Silk, three retorts are continuously arranged, and are interconnected, and the precursor after drying successively passes through three charcoals under the conveying of conveying equipment
Change furnace and carry out continuously carbonizing, the carbonization time in three retorts is respectively 30min, 30min and 40min, total 100min, pre- oxygen
Change is the committed step of carbon fiber production, and precursor is converted into heat-resisting trapezoidal after pre-oxidizing structure by linear molecule chain
Structure can play solid oxygen carbon sequestration for later carbonization process, and a series of cyclisation, oxidation and dehydrogenation occur in the process
Deng reaction, the linear chain structure based on σ key original first forms a large amount of delocalizedπelectron, forms the conjugated structure to add lustre to.So that
Precursor is gradually deepened by pure white color: white → faint yellow → ecru → light brown → brown → black.PAN occurs during this
A large amount of small molecules are sloughed in chemical reaction, and recurring structure variation need to apply certain drafting force and guarantee that solution does not occur and takes for the structure of silk
To guaranteeing the intensity of oxidization fiber, at 240 DEG C or so, oxygen content is risen rapidly;In oxidation process, temperature is kept in burner hearth
Uniformly, and circulation air takes away the small molecule generated in reaction and impurity and reaction heat, to guarantee that oxidation can be continuous
It carries out, is continuously arranged using three pre-oxidation furnaces, precursor can continuously be pre-oxidized, save preoxidation time, improve carbon
The production efficiency of fiber;In pre-oxidation, pyrolysis and polycondensation reaction occur for oxidization fiber, can generate a large amount of exhaust gas and tar, answer
Guarantee production is discharged in time by exhaust outlet to stablize;
Step d, it carbonizes, the oxidization fiber after pre-oxidation is successively subjected to low-temperature carbonization and high temperature carbonization, wherein in low-temperature carbonization furnace
If 5 temperature ranges, respectively 350 DEG C, 450 DEG C, 550 DEG C, 650 DEG C, 750 DEG C;6 temperature ranges are set in high temperature carbonization furnace,
Respectively 1050 DEG C, 1150 DEG C, 1250 DEG C, 1350 DEG C, 1450 DEG C, 1400 DEG C form random layer after charing, inside oxidization fiber
Graphite-structure, and deviate from small molecule, form the charing silk with certain drafting force;
Step e, electrolytic oxidation is modified, will carbonize silk and carry out once as the first electrolyte bath for being loaded with causticity alkaline electrolyte
Electrolytic oxidation is modified, and the pH value of electrolyte is 9-11, and current density is 1.5-2.5A/ ㎡;After silk taking-up drying will then be carbonized,
Re-electrolysis oxidation modification is carried out as the second electrolyte bath for filling weak base electrolyte, the pH value of the weak base electrolyte is
7.5-8, current density 0.5-1A then take out drying, and drying mode is vacuum drying, and drying time 70min is formed just
Grade modified carbon fiber;
Step f, it impregnates and is modified, make primary modified carbon fiber wash with distilled water, then dry, obtain clean primary modified carbon fiber
Clean primary modified carbon fiber is then placed in the dopamine hydrochloric acid solution of pH value 8-9, persistently stirs 16-24h, take out by dimension
It cleans, cleaning process is rinsed using deionized water, and cleaning process continues to water for cleaning the pellucidity that becomes colorless, using running water
The cleanliness of carbon fiber cleaning can be improved in cleaning, the modified carbon fiber in surface can be obtained after drying, drying equipment is drying
Case, drying temperature are 60 DEG C, drying time 1h.
By using the mode of electrolytic oxidation, carbon fiber surface is modified, introduces active official on the surface of carbon fiber
It can roll into a ball, increase the carbon-oxygen bond of carbon fiber surface, improve the tightness contacted in recombination process with composite material surface, improve
The increase and decrease shear strength of synthetic composite material;
It is twice-modified to carbon fiber progress using dopamine hydrochloric acid solution after electrolytic oxidation, DOPA can be formed in carbon fiber surface
Amine coating increases the roughness of carbon fiber surface, with resin base material compound tense, contact of the carbon fiber with resin base material can be improved
Area, so that the interface binding power of faying face is improved, to improve carbon in conjunction with resin base material by the functional group of dopamine
The tensile strength and impact strength of fiber and resin base material composite material.
The above description is merely a specific embodiment, but scope of protection of the present invention is not limited thereto, any
Those familiar with the art in the technical scope disclosed by the present invention, can easily think of the change or the replacement, and should all contain
Lid is within protection scope of the present invention.Therefore, protection scope of the present invention should be based on the protection scope of the described claims.
Claims (7)
1. a kind of processing technology of modified carbon fiber, which comprises the following steps:
Step a, a line concentration is moved back, precursor is chosen, connect Xin Si using heat resistance fiber with old silk after beam splitting, and be set up in line concentration
On plate;
Step b, just dry, line collecting plate is sent into moisture dry in drying equipment, to contain in elimination precursor together with precursor;
Step c, it pre-oxidizes, the precursor after drying is sent into pre-oxidation furnace together with precursor and is pre-oxidized, pre-oxidation furnace is continuous
It is provided with 3, and the temperature range of three pre-oxidation furnaces is respectively 200 DEG C -230 DEG C, 220 DEG C -250 DEG C, 235 DEG C -245 DEG C,
Precursor through pre-oxidizing is converted into trapezium structure by linear molecule chain, and preoxidation time 75-110min ultimately forms pre- oxygen
Silk;
Step d, it carbonizes, the oxidization fiber after pre-oxidation is successively subjected to low-temperature carbonization and high temperature carbonization, wherein in low-temperature carbonization furnace
If 5 temperature ranges, respectively 350 DEG C, 450 DEG C, 550 DEG C, 650 DEG C, 750 DEG C;6 temperature ranges are set in high temperature carbonization furnace,
Respectively 1050 DEG C, 1150 DEG C, 1250 DEG C, 1350 DEG C, 1450 DEG C, 1400 DEG C form random layer after charing, inside oxidization fiber
Graphite-structure, and deviate from small molecule, form the charing silk with certain drafting force;
Step e, electrolytic oxidation is modified, will carbonize silk and carry out once as the first electrolyte bath for being loaded with causticity alkaline electrolyte
Electrolytic oxidation is modified, and the pH value of electrolyte is 9-11, and current density is 1.5-2.5A/ ㎡;After silk taking-up drying will then be carbonized,
Re-electrolysis oxidation modification is carried out as the second electrolyte bath for filling weak base electrolyte, the pH value of the weak base electrolyte is
7.5-8, current density 0.5-1A then take out drying, form primary modified carbon fiber;
Step f, it impregnates and is modified, make primary modified carbon fiber wash with distilled water, then dry, obtain clean primary modified carbon fiber
Clean primary modified carbon fiber is then placed in the dopamine hydrochloric acid solution of pH value 8-9, persistently stirs 16-24h, take out by dimension
It cleans, the modified carbon fiber in surface can be obtained after drying.
2. a kind of processing technology of modified carbon fiber according to claim 1, it is characterised in that: just dry in the step b
Using horizontal kiln, drying temperature is 80 DEG C -100 DEG C.
3. a kind of processing technology of modified carbon fiber according to claim 1, it is characterised in that: in the step c, three charcoals
Change furnace to be continuously arranged, and be interconnected, the precursor after drying is successively carried out by three retorts under the conveying of conveying equipment
Continuously carbonizing, the carbonization time in three retorts is respectively 30min, 30min and 40min, total 100min.
4. a kind of processing technology of modified carbon fiber according to claim 1, it is characterised in that: in the step e, primary electricity
It solves oxidation modification and the re-electrolysis oxidation modification time is 2min-5min, the first electrolytic cell and the second electrolyte bath temperature
It is 30 DEG C -50 DEG C.
5. a kind of processing technology of modified carbon fiber according to claim 1, it is characterised in that: the drying in the step e
Mode is vacuum drying, drying time 60min-80min.
6. a kind of processing technology of modified carbon fiber according to claim 1, it is characterised in that: in the step f, cleaned
Cheng Caiyong deionized water is rinsed, and cleaning process continues to water for cleaning the pellucidity that becomes colorless.
7. a kind of processing technology of modified carbon fiber according to claim 1, it is characterised in that: in the step f, drying is set
Standby is drying box, and drying temperature is 60 DEG C, drying time 1h.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN110791265A (en) * | 2019-11-26 | 2020-02-14 | 陕西博世威科技有限责任公司 | Preparation method of carbon fiber toughening agent for oil well cement |
CN114855307A (en) * | 2022-05-25 | 2022-08-05 | 昆山盛夏复合材料科技有限公司 | Carbon fiber composite material and preparation method thereof |
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CN110791265A (en) * | 2019-11-26 | 2020-02-14 | 陕西博世威科技有限责任公司 | Preparation method of carbon fiber toughening agent for oil well cement |
CN110791265B (en) * | 2019-11-26 | 2021-10-01 | 四川盛年同缔实业有限公司 | Preparation method of carbon fiber toughening agent for oil well cement |
CN114855307A (en) * | 2022-05-25 | 2022-08-05 | 昆山盛夏复合材料科技有限公司 | Carbon fiber composite material and preparation method thereof |
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