CN107059248A - A kind of graphene oxide monolayer modifies the preparation method of polyacrylonitrile nanofiber film - Google Patents
A kind of graphene oxide monolayer modifies the preparation method of polyacrylonitrile nanofiber film Download PDFInfo
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- CN107059248A CN107059248A CN201710198655.8A CN201710198655A CN107059248A CN 107059248 A CN107059248 A CN 107059248A CN 201710198655 A CN201710198655 A CN 201710198655A CN 107059248 A CN107059248 A CN 107059248A
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- graphene oxide
- polyacrylonitrile nanofiber
- film
- nanofiber film
- modifies
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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
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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
- D04H1/40—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
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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
- 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
Abstract
The present invention relates to the preparation method that a kind of graphene oxide monolayer modifies polyacrylonitrile nanofiber film, including：(1) polyacryl-nitrile spinning fluid is prepared, polyacrylonitrile nanofiber film is obtained by electrostatic spinning；(2) prepare graphene oxide and sprawl solution；Then graphene oxide is sprawled into solution and spreads over the water surface, obtain monolayer graphene oxide, by compressing sliding barrier, obtain graphene oxide film；(3) LB technologies are utilized, the graphene oxide film of the water surface is transferred on polyacrylonitrile nanofiber film by film balance, produced.The present invention realizes graphene oxide in the regulation and control of the molecular level on polyacrylonitrile surface, arrangement, assembling and modified, realize the modification to polyacrylonitrile nanofiber surface molecular level, it can be widely applied to textile, biological medicine, functional material,, there are good practical value and potential value in the fields such as water process；Simple to operate, mild condition of the invention, while preparation process nontoxic pollution-free.
Description
Technical field
The invention belongs to functional material preparation field, more particularly to a kind of graphene oxide monolayer modification polyacrylonitrile
The preparation method of nano fibrous membrane.
Background technology
Material-the graphene of " changing 21 century ", because of the performance such as its excellent mechanics and conduction, grinds as material science
Study carefully one of the focus in field.By taking the excellent mechanical property of graphene as an example, its modulus is up to up to 1Tpa, tensile strength
240Gpa, is most strong material known at this stage.The development for being found to be nanofiber reinforcement of graphene provides brand-new
Opportunity.Surface of graphene oxide has abundant functional group, good dispersion, so as to easily form more preferably interface cohesion shape
State, prepares High-performance graphite oxide alkene enhancing composite.
At present, the high-performance and multifunction of PAN base carbon fibres have become national economy major areas equipment technology
In the urgent need to.By the modification to PAN base carbon fibres, fiber can be made to obtain different mechanics, calorifics, electricity, magnetics, light
The highest tensile strength of the functions such as, moisture absorption, such as PAN base carbon fibres only reaches the 4%~5% of theoretical value, by fiber
Modified, improving its tensile strength still has very high potential.For from method of modifying, the modification of PAN base carbon fibres changes including chemistry
Property and physical modification, chemical modification mainly has that modification by copolymerization, chemical reaction are modified and chemical surface treatment is modified.Physical modification master
For having from method of modifying, the modification of PAN base carbon fibres includes chemical modification and physical modification, and chemical modification mainly has altogether
Poly- modified, chemical reaction is modified and chemical surface treatment is modified.Physical modification mainly has high-energy ray modification, blending and modifying and surpassed
Sound wave is modified.Spinning solution is concentrated mainly on from the modification of PAN base carbon fibres from the point of view of the preparation process of PAN base carbon fibres to change
Property and precursor be modified.But because fiber surface activity point is less, graphene oxide is grafted in Multi-scale model prepared by this method
Density is small, skewness, can not ensure with the bond strength of fiber, while the chloride process prepared has larger poison to people
Evil, it is more difficult to promote production application.Meanwhile, above method can not all carry out the arrangement, regulation and control and design of molecular level at interface.
The content of the invention
The technical problems to be solved by the invention are to provide a kind of graphene oxide monolayer modification polyacrylonitrile nano
The preparation method of tunica fibrosa, this method is simple to operate, mild condition, while preparation process nontoxic pollution-free.
A kind of graphene oxide monolayer of the present invention modifies the preparation method of polyacrylonitrile nanofiber film, including：
(1) polyacryl-nitrile spinning fluid is prepared, polyacrylonitrile nanofiber film is obtained by electrostatic spinning；
(2) prepare graphene oxide and sprawl solution；Then graphene oxide is sprawled into solution and spreads over the water surface, obtain single point
Sublayer graphene oxide, by compressing sliding barrier, obtains graphene oxide film；
(3) LB technologies are utilized, the graphene oxide film of the water surface is transferred to by polyacrylonitrile nanofiber by film balance
On film, graphene oxide monolayer modification polyacrylonitrile nanofiber film is obtained.
The solvent of polyacryl-nitrile spinning fluid in the step (1) is N,N-dimethylformamide.
The mass concentration of polyacryl-nitrile spinning fluid in the step (1) is 0.01mg/ml~1mg/ml.
Electrostatic spinning process condition in the step (1) is：1~10V of positive voltage, negative voltage -10~-1V, spinning speed
Spend 0.1-1ml/h, 10~20cm of distance.
Spreading solvent in the step (2) is volume ratio 1:4~1:6 pure water and the mixed solution of methanol.
The mass concentration that graphene oxide in the step (2) sprawls solution is 0.1mg/ml~0.2mg/ml.
The translational speed of the sliding barrier of compression in the step (2) is 0.8cm/min~1.2cm/min.
The impregnating speed of film balance in the step (3) be 0.5~2.0mm/min, pull rate be 0.1mm/min~
0.3mm/min。
The present invention by graphene oxide sprawl solution by syringe carefully spread over the water surface, obtain swimming in the water surface
Sparse monolayer graphene oxide, by compressing sliding barrier, reduces water surface area, the graphene oxide of the water surface is compressed, with shape
Into fine and close film, obtain swimming in the graphene oxide film of water surface monolayer arrangement；Then Langmuir- is utilized
Blodgett (LB) technology, is transferred to polyacrylonitrile by the fine and close graphene oxide film for swimming in the water surface by film balance and receives
On rice fiber, graphene oxide modification polyacrylonitrile nanofiber film is obtained.
The present invention with LB self-assembling techniques, can be achieved graphene oxide molecular level it is controllable, orderly be self-assembled to
Polyacrylonitrile nanofiber, by the design in molecular level, prepares a kind of graphene oxide monolayer modification polypropylene
Nitrile nanofibre film, possess two kinds of excellent functions of material simultaneously and for deep functional nano-fiber provide it is a kind of newly
Method, this graphene oxide monolayer modification polyacrylonitrile nanofiber film prepared by the present invention, method is simple, can batch
Production, is a kind of brand-new nanofiber reinforcement, therefore in field of Environment Protection, medical dialysis, wastewater treatment, desalinization, work(
The fields such as energy material all have broad application prospects.
Beneficial effect
(1) present invention realize graphene oxide the molecular level on polyacrylonitrile surface regulation and control, arrange, assemble and repair
Decorations, realize the modification to polyacrylonitrile nanofiber surface molecular level, have obtained a kind of containing single point of graphene oxide
Sublayer coating polyacrylonitrile nanofiber film, can be widely applied to textile, biological medicine, functional material, the field such as water process,
There are good practical value and potential value；
(2) preparation method of the present invention is simple, experiment condition is gentle, in production process is prepared, not using toxic reagent,
Avoid environmental pollution.
Brief description of the drawings
Fig. 1 schemes for unmodified polyacrylonitrile nanofiber film SEM；
Fig. 2 schemes for amplification 1.8k graphene oxide monolayer coating polyacrylonitrile nanofiber film SEM；
Fig. 3 schemes for amplification 10k graphene oxide monolayer coating polyacrylonitrile nanofiber film SEM.
Embodiment
With reference to specific embodiment, the present invention is expanded on further.It should be understood that these embodiments are merely to illustrate the present invention
Rather than limitation the scope of the present invention.In addition, it is to be understood that after the content of the invention lectured has been read, people in the art
Member can make various changes or modifications to the present invention, and these equivalent form of values equally fall within the application appended claims and limited
Scope.
Embodiment 1
The preparation of polyacrylonitrile nanofiber film, comprises the following steps：
Step 1：0.4g polyacrylonitrile powders accurately are weighed, magnetic force in 60 DEG C of waters bath with thermostatic control is dissolved in 5ml DMF
12h is stirred, the spinning solution of 0.08g/ml clear homogeneous is obtained.
Step 2：It is respectively positive voltage 7v, negative voltage -8v, spinning speed 0.5ml/h, spinning distance to adjust spinning parameter
18cm。
Step 3：Polyacrylonitrile nanofiber film is prepared using method of electrostatic spinning, 10min is stood afterwards, constant temperature is placed into and does
37 DEG C of dryings in dry case, obtain polyacrylonitrile nanofiber film.Fig. 1 schemes for unmodified polyacrylonitrile nanofiber film SEM.
Embodiment 2
Graphene oxide sprawls the preparation of solution, comprises the following steps：
First, 1.0mg/ml graphene oxide water solution 3.0ml is configured, 15.0ml first is then added in above-mentioned solution
Alcohol, stirs 20min, and the graphene oxide for obtaining final concentration of 0.167mg/ml sprawls solution.
Embodiment 3
The preparation of monolayer graphene oxide, comprises the following steps：
Take the above-mentioned graphene oxides of 10.0ml to sprawl solution, drop by drop carefully spread in LB tanks with injection
The water surface, tank area is 10*20cm, stands 20 minutes, after the methanol volatilization of the water surface is complete, mobile sliding barrier, and speed is
1.0cm/min, when the distance for being moved to sliding barrier is 1cm, stops movement, stands, wait monolayer graphene oxide film
It is self-assembly of.
Embodiment 4
The preparation of graphene oxide monolayer coating polyacrylonitrile nanofiber film, comprises the following steps：
Polyacrylonitrile nanofiber film is cut into the sample of 5cm*2.5cm specifications, by controlling film balance parameter, set
Impregnating speed be 1.0mm/min by polyacrylonitrile nanofiber film immersion in LB tanks, the length below immersed in liquid level is
4cm, waits liquid level stabilizing after 20 minutes, lifts polyacrylonitrile nanofiber film with 0.2mm/min pull rate, realize the water surface
Monolayer graphene oxide is transferred to polyacrylonitrile nanofiber film surface, obtains graphene oxide monolayer and applies strata third
Alkene nitrile nanofibre film.Then, its appearance structure is observed under a scanning electron microscope, and such as Fig. 2 is amplification 1.8k oxidation stone
Black alkene monolayer coating polyacrylonitrile nanofiber film SEM figures；Fig. 3 is amplification 10k graphene oxide monolayer coating
Polyacrylonitrile nanofiber film SEM schemes.Contrasted by Fig. 1 with Fig. 2, can substantially find that the present invention obtains a kind of graphene oxide
The polyacrylonitrile nanofiber film of monolayer modification, is compareed with Fig. 3 by Fig. 2 and also will become apparent from graphene oxide and successfully modify
Polyacrylonitrile nanofiber film.
Claims (8)
1. a kind of graphene oxide monolayer modifies the preparation method of polyacrylonitrile nanofiber film, including：
(1) polyacryl-nitrile spinning fluid is prepared, polyacrylonitrile nanofiber film is obtained by electrostatic spinning；
(2) prepare graphene oxide and sprawl solution；Then graphene oxide is sprawled into solution and spreads over the water surface, obtain monolayer
Graphene oxide, by compressing sliding barrier, obtains graphene oxide film；
(3) LB technologies are utilized, the graphene oxide film of the water surface is transferred on polyacrylonitrile nanofiber film by film balance,
Obtain graphene oxide monolayer modification polyacrylonitrile nanofiber film.
2. a kind of graphene oxide monolayer according to claim 1 modifies the preparation side of polyacrylonitrile nanofiber film
Method, it is characterised in that：The solvent of polyacryl-nitrile spinning fluid in the step (1) is N,N-dimethylformamide.
3. a kind of graphene oxide monolayer according to claim 1 modifies the preparation side of polyacrylonitrile nanofiber film
Method, it is characterised in that：The mass concentration of polyacryl-nitrile spinning fluid in the step (1) is 0.01mg/ml~1mg/ml.
4. a kind of graphene oxide monolayer according to claim 1 modifies the preparation side of polyacrylonitrile nanofiber film
Method, it is characterised in that：Electrostatic spinning process condition in the step (1) is：1~10V of positive voltage, negative voltage -10~-1V,
Spinning speed 0.1-1ml/h, 10~20cm of distance.
5. a kind of graphene oxide monolayer according to claim 1 modifies the preparation side of polyacrylonitrile nanofiber film
Method, it is characterised in that：Spreading solvent in the step (2) is volume ratio 1:4~1:6 pure water and the mixed solution of methanol.
6. a kind of graphene oxide monolayer according to claim 1 modifies the preparation side of polyacrylonitrile nanofiber film
Method, it is characterised in that：The mass concentration that graphene oxide in the step (2) sprawls solution is 0.1mg/ml~0.2mg/
ml。
7. a kind of graphene oxide monolayer according to claim 1 modifies the preparation side of polyacrylonitrile nanofiber film
Method, it is characterised in that：The translational speed of the sliding barrier of compression in the step (2) is 0.8cm/min~1.2cm/min.
8. a kind of graphene oxide monolayer according to claim 1 modifies the preparation side of polyacrylonitrile nanofiber film
Method, it is characterised in that：The impregnating speed of film balance in the step (3) is 0.5~2.0mm/min, and pull rate is
0.1mm/min~0.3mm/min.
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Cited By (5)
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| CN109046042A (en) * | 2018-08-17 | 2018-12-21 | 东华大学 | A kind of composite nanometer filtering film and its preparation and application |
| CN109046041A (en) * | 2018-08-17 | 2018-12-21 | 东华大学 | A kind of composite nanometer filtering film and its preparation and application |
| CN109778351A (en) * | 2019-03-08 | 2019-05-21 | 东华大学 | A kind of molybdenum oxide nanofiber of macroscopic view and its preparation and application |
| CN113097384A (en) * | 2021-03-31 | 2021-07-09 | 南京大学 | Method for preparing two-dimensional molecular monolayer |
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| CN109778351A (en) * | 2019-03-08 | 2019-05-21 | 东华大学 | A kind of molybdenum oxide nanofiber of macroscopic view and its preparation and application |
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| CN113097384B (en) * | 2021-03-31 | 2023-11-21 | 南京大学 | Method for preparing two-dimensional molecular monolayer |
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