CN107475793A - A kind of preparation method of graphene oxide parcel polyacrylonitrile composite nano fiber - Google Patents
A kind of preparation method of graphene oxide parcel polyacrylonitrile composite nano fiber Download PDFInfo
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- CN107475793A CN107475793A CN201610401906.3A CN201610401906A CN107475793A CN 107475793 A CN107475793 A CN 107475793A CN 201610401906 A CN201610401906 A CN 201610401906A CN 107475793 A CN107475793 A CN 107475793A
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- graphene oxide
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- polyacrylonitrile
- electrostatic spinning
- parcel
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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
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/0007—Electro-spinning
- D01D5/0015—Electro-spinning characterised by the initial state of the material
- D01D5/003—Electro-spinning characterised by the initial state of the material the material being a polymer solution or dispersion
-
- 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
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/44—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds
- D01F6/54—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds of polymers of unsaturated nitriles
Abstract
The invention discloses a kind of preparation method of graphene oxide parcel polyacrylonitrile composite nano fiber, its step is：（1）Prepare the N of graphene oxide, N dimethylformamide dispersion liquids；（2）Polyacrylonitrile fibril is added to step（1）Solution in, be made electrostatic spinning solution；（3）Using step（2）Gained electrostatic spinning solution carries out electrostatic spinning, and the nanofiber of collection is dried, and produces graphene oxide parcel polyacrylonitrile composite nano fiber.The present invention prepares graphene oxide parcel polyacrylonitrile composite nano fiber by electrostatic spinning technique, solve during preparing graphene oxide composite nano fiber, the problem of graphene oxide is encapsulated in fibrous inside, and performance is restricted, the nanofiber diameter of preparation is in 500 ~ 600nm.
Description
Technical field
The invention belongs to the preparation field of composite, more particularly to a kind of preparation method of graphene oxide parcel polyacrylonitrile composite nano fiber.
Background technology
With the continuous progress and development of science and technology, traditional monocomponent nanocomposite material can not meet its application requirement in sciemtifec and technical sphere.In recent years, the researcher in many nanosecond science and technology fields is directed to the research of composite nano materials, by certain technology that its is compound such as excellent in mechanical performance, the significant nano material of thermal property by the nano material of difference in functionality, prepares the nano material of functionalization.
Graphene is by carbon atom with sp2The monoatomic layer of hydridization connection is formed, and is the most thin two-dimensional material having now been found that.Graphene oxide is the derivative of graphene, and its lamellar structure contains abundant oxy radical, and this special structure makes it contain many excellent physicochemical properties, such as high specific surface area and excellent heat conductivility, good biocompatibility.Because containing abundant oxy radical in structure, graphene oxide can be dispersed stably in most of polar organic solvents, and this is advantageous to, and graphene oxide is compound with other materials, the performance of reinforcing material.At present, graphene oxide composite nano fiber is used widely in fields such as optics, catalysis, filtering and cell scaffold materials.
Preparing graphene oxide composite nano fiber has a variety of methods, including self-assembling technique, chemical vapour deposition technique, electrostatic spinning technique.Compared with other method, electrostatic spinning technique, which prepares stannic oxide/graphene nano fiber, has the advantages such as simple to operate, mature preparation process.Reported in spite of seminar and graphene oxide composite nano fiber (Song J are successfully prepared by electrostatic spinning technique, Gao H, Zhu G, et al.The preparation and characterization of polycaprolactone/graphene oxide biocomposite nanofiber scaffolds and their application for directing cell behaviors [J] .Carbon, 2015,95:1039-1050；Wang Q,Du Y,Feng Q,et al.Nanostructures and surface nanomechanical properties of polyacrylonitrile/graphene oxide composite nanofibers by electrospinning[J].Journal of Applied Polymer Science,2013,128(2):1152-1157), but the graphene oxide of sheet is normally encapsulated in fibrous inside so that the excellent performance of graphene oxide is difficult to play, and seriously limits the application of graphene oxide composite material.
The content of the invention
Object of the present invention is to provide a kind of preparation method of graphene oxide parcel polyacrylonitrile composite nanofiber membrane, methods described is simple to operate, reproducible, and the fiber is wrapped up by the exposed graphene oxide of large area.
A kind of preparation method of graphene oxide parcel polyacrylonitrile composite nanofiber membrane of the present invention, including step in detail below：
Step (1)：The preparation of graphene oxide dispersion
Graphene oxide is placed in DMF solution, by ultrasonic lift-off processing, obtains graphene oxide dispersion；
Step (2)：The preparation of electrostatic spinning solution
Polyacrylonitrile fibril is added in the dispersion liquid of step (1), heating stirring, produces electrostatic spinning solution；
Step (3)：Graphene oxide wraps up the preparation of polyacrylonitrile composite nano fiber
Electrostatic spinning solution in step (2) is removed into bubble, nano fibrous membrane is obtained by electrostatic spinning technique, is dried, is produced.
Preferably, in the step (1), the concentration of graphene oxide dispersion is 1.0~5.0mg/ml.
Preferably, in the step (1), the ultrasonic lift-off processing time is 15~30min.
Preferably, in the step (2), heating-up temperature is 40~60 DEG C, and mixing speed is 150~200rpm/min.
Preferably, in the step (2), polyacrylonitrile fibril accounts for the 8%~15% of electrostatic spinning solution mass fraction.
Preferably, in the step (3), electrospinning parameters：Spinning temperature is 23 DEG C, and humidity 40%, voltage 15kV, fltting speed is 1.0~3.0ml/L, and it is 10~15cm to receive distance, and syringe needle is No. 21 flat mouth pins.
The advantage of the invention is that：
(1) different size of graphene oxide layer is obtained using ultrasonic stripping conditions ingenious in design, graphene oxide parcel polyacrylonitrile composite nano fiber is prepared by electrostatic spinning technique, solve during preparing graphene oxide composite nano fiber, the problem of graphene oxide is encapsulated in fibrous inside, and performance is restricted.
(2) technical operation is simple, reproducible.
Brief description of the drawings
Fig. 1 is the shape appearance figure of the graphene oxide layer obtained after the ultrasound of the embodiment of the present invention 1 is peeled off.
Fig. 2 is the scanning electron microscope (SEM) photograph of the graphene oxide parcel polyacrylonitrile composite nano fiber obtained by the embodiment of the present invention 2.
Fig. 3 is the transmission electron microscope picture of the graphene oxide parcel polyacrylonitrile composite nano fiber obtained by the embodiment of the present invention 3.
Embodiment
With reference to specific implementation example, the present invention is expanded on further.
Embodiment 1
(1) 5mL N is measured, N-dimethylformamide is in screw socket vial, add 5mg graphene oxides, sealed after screw socket vial is screwed with sealed membrane, sonic oscillation 15 minutes, graphene oxide dispersion is made, its pattern is as shown in figure 1, obtained graphene oxide sheet size is between 0.30-1.58 μm after peeling off；
(2) 0.40g polyacrylonitrile fibrils are weighed to be added in graphene oxide dispersion, magnetic force heating stirring 12 hours under 40 DEG C, 150r/min, spinning solution is made；
(3) spinning solution is stood and removes bubble, carry out electrospinning in the electric spinning equipment built, electrospinning parameters are set：Spinning temperature is 23 DEG C, and humidity 40%, voltage 15kV, fltting speed 1.0ml/L, it is 10cm to receive distance, and syringe needle is No. 21 flat mouth pins, that is, obtains the polyacrylonitrile composite nano fiber of graphene oxide cladding, and its scanning electron microscope (SEM) photograph is as shown in Figure 2.
Embodiment 2
(1) 5mL DMF is measured in screw socket vial, 15mg graphene oxides is added, is sealed after screw socket vial is screwed with sealed membrane, sonic oscillation 30 minutes, and graphene oxide dispersion is made；
(2) 0.75g polyacrylonitrile fibrils are weighed to be added in graphene oxide dispersion, magnetic force heating stirring 12 hours under 50 DEG C, 180r/min, spinning solution is made；
(3) spinning solution is stood and removes bubble, carry out electrospinning in the electric spinning equipment built, electrospinning parameters are set：Spinning temperature is 23 DEG C, and humidity 40%, voltage 15kV, fltting speed 3.0ml/L, it is 15cm to receive distance, and syringe needle is No. 21 flat mouth pins, that is, obtains the polyacrylonitrile composite nano fiber of graphene oxide cladding, and its transmission electron microscope picture is as shown in Figure 3.
Embodiment 3
(1) 5mL DMF is measured in screw socket vial, 10mg graphene oxides is added, is sealed after screw socket vial is screwed with sealed membrane, sonic oscillation 20 minutes, and graphene oxide dispersion is made；
(2) 0.60g polyacrylonitrile fibrils are weighed to be added in graphene oxide dispersion, magnetic force heating stirring 12 hours under 55 DEG C, 180r/min, spinning solution is made；
Spinning solution is stood and removes bubble, carries out electrospinning in the electric spinning equipment built, electrospinning parameters are set：Spinning temperature is 23 DEG C, and humidity 40%, voltage 15kV, fltting speed 2.0ml/L, it is 12cm to receive distance, and syringe needle is No. 21 flat mouth pins, that is, obtains the polyacrylonitrile composite nano fiber of graphene oxide cladding.
Claims (6)
1. a kind of preparation method of graphene oxide parcel polyacrylonitrile composite nanofiber membrane, it is characterised in that comprise the following steps：
Step（1）：The preparation of graphene oxide dispersion
Graphene oxide is placed in DMF solution, by ultrasonic lift-off processing, obtains graphene oxide dispersion；
Step（2）：The preparation of electrostatic spinning solution
Polyacrylonitrile fibril is added to step（1）Dispersion liquid in, heating stirring, produce electrostatic spinning solution；
Step（3）：Graphene oxide wraps up the preparation of polyacrylonitrile composite nano fiber
By step（2）In electrostatic spinning solution remove bubble, nano fibrous membrane is obtained by electrostatic spinning technique, is dried, is produced.
2. the preparation method of graphene oxide parcel polyacrylonitrile composite nanofiber membrane as claimed in claim 1, it is characterised in that step（1）In, the concentration of graphene oxide dispersion is 1.0 ~ 5.0mg/ml.
3. the preparation method of graphene oxide parcel polyacrylonitrile composite nanofiber membrane as claimed in claim 1, it is characterised in that step（1）In, the ultrasonic lift-off processing time is 15 ~ 30min.
4. the preparation method of graphene oxide parcel polyacrylonitrile composite nanofiber membrane as claimed in claim 1, it is characterised in that step（2）In, heating-up temperature is 40 ~ 60 DEG C, and mixing speed is 150 ~ 200rpm/min.
5. the preparation method of graphene oxide parcel polyacrylonitrile composite nanofiber membrane as claimed in claim 1, it is characterised in that step（2）In, polyacrylonitrile fibril accounts for the 8% ~ 15% of electrostatic spinning solution mass fraction.
6. the preparation method of graphene oxide parcel polyacrylonitrile composite nanofiber membrane as claimed in claim 1, it is characterised in that step（3）In, electrospinning parameters：Spinning temperature is 23 DEG C, and humidity 40%, voltage 15kV, fltting speed is 1.0 ~ 3.0ml/L, and it is 10 ~ 15cm to receive distance, and syringe needle is No. 21 flat mouth pins.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108295675A (en) * | 2018-02-10 | 2018-07-20 | 河南省科学院能源研究所有限公司 | A kind of antibacterial air filter film and preparation method thereof based on polyacrylonitrile/graphene oxide/tea polyphenol compound |
| CN108771981A (en) * | 2018-06-04 | 2018-11-09 | 郑州新世纪材料基因组工程研究院有限公司 | Graphene composite material and its preparation method and application, graphene-carbon nano-fiber film and preparation method thereof |
| CN109914037A (en) * | 2019-03-29 | 2019-06-21 | 中原工学院 | A kind of preparation method of non-woven nano-graphene/polyacrylonitrile non-woven fabrics |
| CN111593493A (en) * | 2020-05-27 | 2020-08-28 | 西安工程大学 | Composite nanofiber membrane and preparation method and application thereof |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102586951A (en) * | 2012-01-18 | 2012-07-18 | 浙江大学 | Preparation method for composite carbon fiber based on graphene/ polyacrylonitrile |
| CN102586952A (en) * | 2012-01-09 | 2012-07-18 | 东华大学 | Method for preparing graphene-reinforced polyacrylonitrile carbon fibers |
| CN104332640A (en) * | 2014-11-06 | 2015-02-04 | 中国科学院金属研究所 | Preparation method of thermally-reduced graphene oxide/nano carbon fiber composite electrode for full-vanadium flow battery |
| CN104649260A (en) * | 2015-02-09 | 2015-05-27 | 清华大学 | Preparation method of graphene nano fibers or nanotubes |
| CN104674384A (en) * | 2015-02-12 | 2015-06-03 | 中国科学院城市环境研究所 | Three-dimensional oil-water separating material based on static spinning technology and preparation method thereof |
| CN105568401A (en) * | 2015-12-12 | 2016-05-11 | 大连理工大学 | Ultrasonic atomization assisted electrospinning technique |
-
2016
- 2016-06-08 CN CN201610401906.3A patent/CN107475793A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102586952A (en) * | 2012-01-09 | 2012-07-18 | 东华大学 | Method for preparing graphene-reinforced polyacrylonitrile carbon fibers |
| CN102586951A (en) * | 2012-01-18 | 2012-07-18 | 浙江大学 | Preparation method for composite carbon fiber based on graphene/ polyacrylonitrile |
| CN104332640A (en) * | 2014-11-06 | 2015-02-04 | 中国科学院金属研究所 | Preparation method of thermally-reduced graphene oxide/nano carbon fiber composite electrode for full-vanadium flow battery |
| CN104649260A (en) * | 2015-02-09 | 2015-05-27 | 清华大学 | Preparation method of graphene nano fibers or nanotubes |
| CN104674384A (en) * | 2015-02-12 | 2015-06-03 | 中国科学院城市环境研究所 | Three-dimensional oil-water separating material based on static spinning technology and preparation method thereof |
| CN105568401A (en) * | 2015-12-12 | 2016-05-11 | 大连理工大学 | Ultrasonic atomization assisted electrospinning technique |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108295675A (en) * | 2018-02-10 | 2018-07-20 | 河南省科学院能源研究所有限公司 | A kind of antibacterial air filter film and preparation method thereof based on polyacrylonitrile/graphene oxide/tea polyphenol compound |
| CN108295675B (en) * | 2018-02-10 | 2020-01-24 | 河南省科学院能源研究所有限公司 | Antibacterial air filter membrane based on polyacrylonitrile/graphene oxide/tea polyphenol compound and preparation method thereof |
| CN108771981A (en) * | 2018-06-04 | 2018-11-09 | 郑州新世纪材料基因组工程研究院有限公司 | Graphene composite material and its preparation method and application, graphene-carbon nano-fiber film and preparation method thereof |
| CN109914037A (en) * | 2019-03-29 | 2019-06-21 | 中原工学院 | A kind of preparation method of non-woven nano-graphene/polyacrylonitrile non-woven fabrics |
| CN111593493A (en) * | 2020-05-27 | 2020-08-28 | 西安工程大学 | Composite nanofiber membrane and preparation method and application thereof |
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Application publication date: 20171215 |