CN109137263A - A kind of high-specific surface area polyacrylonitrile carbon fiber non-woven fabrics and preparation method - Google Patents
A kind of high-specific surface area polyacrylonitrile carbon fiber non-woven fabrics and preparation method Download PDFInfo
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- CN109137263A CN109137263A CN201810641705.XA CN201810641705A CN109137263A CN 109137263 A CN109137263 A CN 109137263A CN 201810641705 A CN201810641705 A CN 201810641705A CN 109137263 A CN109137263 A CN 109137263A
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- woven fabrics
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- surface area
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- polyacrylonitrile
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- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/70—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres
- D04H1/72—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged
- D04H1/728—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged by electro-spinning
-
- 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
- D01F9/14—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments
- D01F9/145—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from pitch or distillation residues
-
- 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
- D01F9/14—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments
- D01F9/20—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products
- D01F9/21—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products from macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D01F9/22—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products from macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds from polyacrylonitriles
-
- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
- D04H1/42—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece
- D04H1/4282—Addition polymers
- D04H1/43—Acrylonitrile series
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06C—FINISHING, DRESSING, TENTERING OR STRETCHING TEXTILE FABRICS
- D06C7/00—Heating or cooling textile fabrics
- D06C7/04—Carbonising or oxidising
Abstract
A kind of specific surface area of high-specific surface area polyacrylonitrile carbon fiber non-woven fabrics is 400-800 m2 g‑1, the microcellular structure for being 0.5-2nm with pore diameter range, carbon yield 40-70%, carbon fiber diameter is 200-600nm in non-woven fabrics.The spinning solution being made of pitch, polyacrylonitrile and organic solvent obtains after electrostatic spinning technique, pre-oxidation and carbonization treatment.The present invention has the advantages that there is preferable flexible and self-supporting, high-specific surface area.
Description
Technical field
The present invention relates to carbon fiber preparation fields, more particularly relate to a kind of high-specific surface area polyacrylonitrile carbon fiber nonwoven
Cloth and preparation method.
Technical background
With the fast development of global economy, the exhaustion of fossil fuel and therewith bring problem of environmental pollution, so that seeking
Ask the sustainable energy of high-efficiency cleaning extremely urgent, energy stores also have become a hot topic of research with conversion.Carbon fiber nonwoven fabric tool
Have to be overlapped by fiber and be formed, (this body structure has self-maintaining, can cut out with shorter ion transmission channel and preferable mouldability
Directly as electrode use after cutting) the advantages that, it is energy storage and conversion equipment preferred electrode materials.Method of electrostatic spinning is to prepare
A kind of very easy and efficient method of carbon fiber, and everybody extensive concern is received due to low in cost.But
The carbon fiber of common method of electrostatic spinning preparation is the carbon fiber of non-porous structure, and specific surface area is all lower, and which greatly limits carbon
Application of the fiber in energy storage and transfer field.For this disadvantage, high-ratio surface carbon fiber and its preparation cause in recent years
People extensive research interests, become the hot spot of research and development.
At present about preparing the method for high-specific surface area carbon fiber mainly with soft template method, hard mold method or by pore creating material
(PMMA, aluminium oxide, ammonium chloride etc.) is added in spinning solution, by calcining pore-creating；Furthermore using physically activated or chemical work
Change pore-creating.Approach described above preparation flow is complicated, at high cost, it is difficult to realize industrialization.More importantly the above side
Method has seriously affected the flexibility of gained high-specific surface area carbon fiber, and then limits the application range of high-specific surface area carbon fiber.
Summary of the invention
The object of the present invention is to provide a kind of with preferable flexible and self-supporting, the polyacrylonitrile carbon fiber of high-specific surface area
Tie up non-woven fabrics and preparation method.
In order to overcome disadvantage mentioned above, the present invention forms the mechanism of microporous carbon using asphalt high-temperature processing, by pitch and poly- third
Alkene nitrile, which is blended, carries out spinning, and obtaining after pre-oxidation and carbonization treatment has high-specific surface area polyacrylonitrile-based carbon fibre non-woven fabrics.
Gained non-woven fabrics has many advantages, such as preferable flexible and self-supporting, becomes the preferred material of energy storage and conversion devices.
The purpose of the present invention is realized by following experimental program:
A kind of high-specific surface area polyacrylonitrile carbon fiber non-woven fabrics, non-woven fabrics specific surface area are 400-800 m2 g-1, there is aperture
Range is the microcellular structure of 0.5-2nm, and carbon yield 40-70%, carbon fiber diameter is 200-600nm in non-woven fabrics.
A kind of preparation method of high-specific surface area polyacrylonitrile carbon fiber non-woven fabrics is by pitch, polyacrylonitrile and organic molten
The spinning solution of agent composition, obtains after electrostatic spinning technique, pre-oxidation and carbonization treatment.Wherein, pitch is pore creating material.
A kind of preparation method of high-specific surface area polyacrylonitrile carbon fiber non-woven fabrics, the specific steps are as follows:
(1) pitch is dissolved in tetrahydrofuran solution, pitch Solute mass fraction is 5-70%, and polyacrylonitrile is dissolved in N, N- diformazan
In yl acetamide solution, polyacrylonitrile Solute mass fraction is 6-35%, and two kinds of solution obtain spinning solution after being mixed,
Wherein the mass ratio of pitch and polyacrylonitrile is 2:7-35:3.
(2) spinning solution receives distance 12-25 cm in spinning voltage 8-18 Kv, humidity 10-60%, and fltting speed is
Electrostatic spinning is carried out under the spinning condition of 0.5-3 ml/h, obtains nascent non-woven fabrics；
(3) nascent non-woven fabrics is subjected to pre-oxidation treatment, pre-oxidation treatment condition are as follows: under air atmosphere, throughput 20-80
Ml/min is warming up to the heating rate of 0.5-5 DEG C/min in 100-160 DEG C of holding 1-7h, the heating of 0.5-5 DEG C later/min
Speed is warming up to 230-290 DEG C of holding 1-7h；
(4) pre-oxidation non-woven fabrics is subjected to carbonization treatment, i.e., in an inert gas atmosphere, with the heating rate liter of 5-15 DEG C/min
After temperature to 700-1300 DEG C of holding 1-10h, it is cooled to room temperature, obtains high-specific surface area polyacrylonitrile carbon fiber non-woven fabrics.
Pitch as described above is one of asphalt, coal tar pitch.
Inert gas atmosphere as described above is high pure nitrogen or argon gas.
High-specific surface area polyacrylonitrile carbon fiber non-woven fabrics of the invention can be used for catalyst carrier, energy storage device electrode material
The fields such as material, flexible device electrode material or filter membrane.
The invention has the following advantages over the prior art:
1, preparation process of the present invention is simple, at low cost, is easy to industrialization；
2, present invention gained high-specific surface area polyacrylonitrile carbon fiber non-woven fabrics has good flexible and self-supporting；
3, the present invention using low cost, high carbon residue and is easily formed the pitch of microcellular structure to be that pore creating material one-step method is prepared for micro-
Prosperity high-specific surface area polyacrylonitrile carbon fiber non-woven fabrics in hole is deviate from without template, at high-temperature process and subsequent soda acid
Reason；
4, the present invention expands the application range of pitch.
Detailed description of the invention
Fig. 1 is the optical photograph of 1 gained high-specific surface area polyacrylonitrile carbon fiber non-woven fabrics of embodiment.
Fig. 2 is 2 gained high-specific surface area polyacrylonitrile carbon fiber non-woven fabrics adsorption desorption curve graph (2a) of embodiment and aperture
Scatter chart (2b).
Fig. 3 is 2 gained high-specific surface area polyacrylonitrile carbon fiber non-woven fabrics SEM of embodiment figure.
Fig. 4 is 3 gained high-specific surface area polyacrylonitrile carbon fiber non-woven fabrics hot weight curve of embodiment.
Specific embodiment
In order to be best understood from the content of present invention, below by specific embodiment, the present invention is further described, but this hair
Bright claimed range is not limited to range described in embodiment.
Embodiment 1
10 g asphalt are dissolved in 190 g tetrahydrofuran solutions, solution A is denoted as；35 g polyacrylonitrile are dissolved in 65 g
In n,N-Dimethylformamide solution, it is denoted as solution B；Magnetic agitation after two kinds of solution of the above A and B are mixed, can be obtained spinning
Silk stock solution.Gained spinning solution is subjected to spinning by electrostatic spinning machine, spinning voltage is 8 Kv, and ambient humidity 60% receives
Distance is 12 cm, and fltting speed is 2 ml/h, and can must come into being non-woven fabrics.To gained come into being non-woven fabrics carry out pre-oxidation treatment,
Pre-oxidizing conditions are as follows: in air atmosphere, gas flow rate is 20 mL/min, is warming up to 100 with the heating rate of 5 DEG C/minoC
After keep 7 h, 300 DEG C of 1 h of holding are warming up to the heating rate of 5 DEG C/min again later, thus obtain pre-oxidation non-woven fabrics；It will
Gained pre-oxidized fibers non-woven fabrics is under high-purity argon gas atmosphere protection, with the heating rate of 10 DEG C/min, in 700 DEG C of constant temperature 10
H can obtain high-specific surface area polyacrylonitrile carbon fiber non-woven fabrics (as shown in Figure 1).The Residual carbon of gained carbon fiber nonwoven fabric is
40%, specific surface area is 600 m2 g-1, pore diameter range is 0.7-1.5 nm；Carbon fiber diameter concentrates in carbon fiber nonwoven fabric
200 nm。
Embodiment 2
70 g asphalt are dissolved in 30 g tetrahydrofuran solutions, solution A is denoted as；6 g polyacrylonitrile are dissolved in 94 g
In n,N-Dimethylformamide solution, it is denoted as solution B；Magnetic agitation after two kinds of solution of the above A and B are mixed, can be obtained spinning
Silk stock solution.Gained spinning solution is subjected to spinning by electrostatic spinning machine, spinning voltage is 18 Kv, and ambient humidity 10% connects
It is 18cm, fltting speed 0.5ml/h by distance, can must come into being non-woven fabrics.Gained non-woven fabrics of coming into being is carried out at pre-oxidation
Reason, pre-oxidizing conditions are as follows: in air atmosphere, gas flow rate 50mL/min, with 0.5oThe heating rate of C/min is warming up to
130o3h is kept after C, later again with 0.5oThe heating rate of C/min is warming up to 280oC keeps 7h, to obtain pre-oxidation nonwoven
Cloth；By gained pre-oxidized fibers non-woven fabrics under high pure nitrogen atmosphere protection, with 5oThe heating rate of C/min, 900oC is permanent
3 h of temperature, can obtain high-specific surface area polyacrylonitrile carbon fiber non-woven fabrics.The Residual carbon of gained carbon fiber nonwoven fabric is 70%, compares table
Area is 800 m2 g-1(as shown in Figure 2), pore diameter range 0.2-1.5nm；Carbon fiber diameter concentrates in carbon fiber nonwoven fabric
400 nm。
Embodiment 3
40 g asphalt are dissolved in 60 g tetrahydrofuran solutions, solution A is denoted as；10 g polyacrylonitrile are dissolved in 90 g
In n,N-Dimethylformamide solution, it is denoted as solution B；Magnetic agitation after two kinds of solution of the above A and B are mixed, can be obtained spinning
Silk stock solution.Gained spinning solution is subjected to spinning by electrostatic spinning machine, spinning voltage is 12 Kv, and ambient humidity 30% connects
It is 25 cm by distance, fltting speed is 3 ml/h, and can must come into being non-woven fabrics.Gained non-woven fabrics of coming into being is carried out at pre-oxidation
Reason, pre-oxidizing conditions are as follows: in air atmosphere, gas flow rate is 80 mL/min, with 3oThe heating rate of C/min is warming up to
160 o5 h are kept after C, later again with 3oThe heating rate of C/min is warming up to 230oC keeps 3 h, to obtain pre-oxidation nothing
Woven fabric；By gained pre-oxidized fibers non-woven fabrics under high-purity argon gas atmosphere protection, with 15oThe heating rate of C/min, 800oC
1 h of constant temperature can obtain high-specific surface area polyacrylonitrile carbon fiber non-woven fabrics.The Residual carbon of gained carbon fiber nonwoven fabric be 63%(such as
Shown in Fig. 4), specific surface area is 560 m2 g-1, pore diameter range is 0.8-2 nm；Carbon fiber diameter is concentrated in carbon fiber nonwoven fabric
In 600 nm.
Embodiment 4
20 g coal tar pitches are dissolved in 100 g tetrahydrofuran solutions, solution A is denoted as；10 g polyacrylonitrile are dissolved in 80 g
In n,N-Dimethylformamide solution, it is denoted as solution B；Magnetic agitation after two kinds of solution of the above A and B are mixed, can be obtained spinning
Silk stock solution.Gained spinning solution is subjected to spinning by electrostatic spinning machine, spinning voltage is 10 Kv, and ambient humidity 40% connects
It is 15 cm by distance, fltting speed is 1 ml/h, and can must come into being non-woven fabrics.Gained non-woven fabrics of coming into being is carried out at pre-oxidation
Reason, pre-oxidizing conditions are as follows: in air atmosphere, gas flow rate is 50 mL/min, with 1oThe heating rate of C/min is warming up to
100 o1 h is kept after C, later again with 2oThe heating rate of C/min is warming up to 300oC keeps 3 h, to obtain pre-oxidation nothing
Woven fabric；By gained pre-oxidized fibers non-woven fabrics under high-purity argon gas atmosphere protection, with 8oThe heating rate of C/min, 1300oC
4 h of constant temperature can obtain high-specific surface area polyacrylonitrile carbon fiber non-woven fabrics.The Residual carbon of gained carbon fiber nonwoven fabric is 46%, than
Surface area is 460 m2 g-1, pore diameter range is 0.5-1.8 nm；Carbon fiber diameter concentrates on 500 nm in carbon fiber nonwoven fabric.
Embodiment 5
10 g coal tar pitches are dissolved in 100 g tetrahydrofuran solutions, solution A is denoted as；35 g polyacrylonitrile are dissolved in 65 g
In n,N-Dimethylformamide solution, it is denoted as solution B；Magnetic agitation after two kinds of solution of the above A and B are mixed, can be obtained spinning
Silk stock solution.Gained spinning solution is subjected to spinning by electrostatic spinning machine, spinning voltage is 10 Kv, and ambient humidity 20% connects
It is 12 cm by distance, fltting speed is 1.2 ml/h, and can must come into being non-woven fabrics.Gained non-woven fabrics of coming into being is pre-oxidized
Processing, pre-oxidizing conditions are as follows: in air atmosphere, gas flow rate is 30 mL/min, with 2oThe heating rate of C/min is warming up to
140 o7 h are kept after C, later again with 3oThe heating rate of C/min is warming up to 280oC keeps 3 h, to obtain pre-oxidation nothing
Woven fabric；By gained pre-oxidized fibers non-woven fabrics under high-purity argon gas atmosphere protection, with 10oThe heating rate of C/min, 800oC
7 h of constant temperature can obtain high-specific surface area polyacrylonitrile carbon fiber non-woven fabrics.The Residual carbon of gained carbon fiber nonwoven fabric is 53%, than
Surface area is 630 m2 g-1, pore diameter range is 0.8-1.5 nm；Carbon fiber diameter concentrates on 400nm in carbon fiber nonwoven fabric.
Claims (4)
1. a kind of high-specific surface area polyacrylonitrile carbon fiber non-woven fabrics, it is characterised in that non-woven fabrics specific surface area is 400-800 m2
G-1 has pore diameter range for the microcellular structure of 0.5-2nm, carbon yield 40-70%, and carbon fiber diameter is 200- in non-woven fabrics
600nm。
2. a kind of preparation method of high-specific surface area polyacrylonitrile carbon fiber non-woven fabrics as described in claim 1, feature exist
In including the following steps:
(1) pitch is dissolved in tetrahydrofuran solution, pitch Solute mass fraction is 5-70%, and polyacrylonitrile is dissolved in N, N- diformazan
In yl acetamide solution, polyacrylonitrile Solute mass fraction is 6-35%, and two kinds of solution obtain spinning solution after being mixed,
Wherein the mass ratio of pitch and polyacrylonitrile is 2:7-35:3；
(2) spinning solution receives distance 12-25 cm, fltting speed 0.5-3 in spinning voltage 8-18 Kv, humidity 10-60%
Electrostatic spinning is carried out under the spinning condition of ml/h, obtains nascent non-woven fabrics；
(3) nascent non-woven fabrics is subjected to pre-oxidation treatment, pre-oxidation treatment condition are as follows: under air atmosphere, throughput 20-80
Ml/min is warming up to the heating rate of 0.5-5 DEG C/min in 100-160 DEG C of holding 1-7h, the heating of 0.5-5 DEG C later/min
Speed is warming up to 230-290 DEG C of holding 1-7h；
(4) pre-oxidation non-woven fabrics is subjected to carbonization treatment, i.e., in an inert gas atmosphere, with the heating rate liter of 5-15 DEG C/min
After temperature to 700-1300 DEG C of holding 1-10h, it is cooled to room temperature, obtains high-specific surface area polyacrylonitrile carbon fiber non-woven fabrics.
3. a kind of preparation method of high-specific surface area polyacrylonitrile carbon fiber non-woven fabrics as claimed in claim 2, feature exist
In the pitch be one of asphalt, coal tar pitch.
4. a kind of preparation method of high-specific surface area polyacrylonitrile carbon fiber non-woven fabrics as claimed in claim 2, feature exist
In the inert gas atmosphere be high pure nitrogen or argon gas.
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Cited By (9)
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|---|---|---|---|---|
| CN109727781A (en) * | 2019-01-07 | 2019-05-07 | 北京化工大学常州先进材料研究院 | A kind of self-supporting flexible super capacitor electrode material and preparation method |
| CN111485328A (en) * | 2020-03-18 | 2020-08-04 | 浙江恒澜科技有限公司 | Preparation method and device of flame-retardant nanofiber composite material |
| CN112853547A (en) * | 2020-07-04 | 2021-05-28 | 山东八三石墨新材料厂 | Method for further preparing electrode material of supercapacitor by treating asphalt through electrostatic spinning |
| CN113388961A (en) * | 2021-05-18 | 2021-09-14 | 武汉科技大学 | Self-bonding micro-nano porous carbon film of asphalt and polyacrylonitrile composite nanofiber as well as preparation method and application of self-bonding micro-nano porous carbon film |
| CN113871618A (en) * | 2021-09-26 | 2021-12-31 | 山东能源集团有限公司 | Petroleum asphalt-based carbon fiber flexible electrode material and preparation method and application thereof |
| CN114122363A (en) * | 2021-11-29 | 2022-03-01 | 东北大学秦皇岛分校 | Preparation method of one-dimensional porous nitrogen-rich tin antimony-carbon negative electrode material |
| CN114232215A (en) * | 2021-12-20 | 2022-03-25 | 西安工程大学 | Preparation method and application of asphalt-based carbon nanofiber multistage non-woven fabric with three-dimensional cavity structure |
| CN114481369A (en) * | 2022-02-16 | 2022-05-13 | 浙江大学 | Preparation method of graphene fiber with high graphite crystallinity |
| CN114808197A (en) * | 2022-04-20 | 2022-07-29 | 山东大学 | Integrated two-phase asphalt-based carbon nanofiber and preparation method and application thereof |
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| CN113388961A (en) * | 2021-05-18 | 2021-09-14 | 武汉科技大学 | Self-bonding micro-nano porous carbon film of asphalt and polyacrylonitrile composite nanofiber as well as preparation method and application of self-bonding micro-nano porous carbon film |
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Application publication date: 20190104 |