CN110067035A - A kind of electrostatic spinning and preparation method thereof of hydrophobic graphene composite high-molecular fiber - Google Patents
A kind of electrostatic spinning and preparation method thereof of hydrophobic graphene composite high-molecular fiber Download PDFInfo
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- CN110067035A CN110067035A CN201910398658.5A CN201910398658A CN110067035A CN 110067035 A CN110067035 A CN 110067035A CN 201910398658 A CN201910398658 A CN 201910398658A CN 110067035 A CN110067035 A CN 110067035A
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- 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
-
- 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
- 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
- D01F6/52—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 carboxylic acids or unsaturated esters
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- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Mechanical Engineering (AREA)
- Inorganic Fibers (AREA)
- Artificial Filaments (AREA)
Abstract
The present invention relates to field of nanometer material technology more particularly to a kind of electrostatic spinning preparation methods of hydrophobic graphene composite high-molecular fiber.With graphene, hydrophobic polymeric is raw material, carries out the electrostatic spinning that electrostatic spinning obtains hydrophobic graphene composite high-molecular fiber by the method for electrostatic spinning.The present invention overcomes the agglomeration traits after high molecular material and graphene mixed dissolution, and the problems such as existing spinning is discontinuous, not at silk when preparing composite fibre with the method for electrostatic spinning, electrostatic spinning preparation method of the invention is quick and easy, reaction time is short, graphene content is high, and fibrous material is environmental-friendly, and application field is wide, industrialization degree is high, and practical value is significant.
Description
Technical field
The present invention relates to field of nanometer material technology more particularly to a kind of electrostatic spinnings of hydrophobic graphene composite high-molecular fiber
Preparation method.
Background technique
Graphene nano material includes single-layer graphene and multi-layer graphene, i.e., by carbon atom by honeycomb close-packed arrays and
At only one or multiple carbon atom thickness two-dimensional sheet crystalline material.Compared with other carbon materials, graphene has had
Beauty big pi-conjugated system and most thin single layer atomic thickness structure, this make graphene possess very excellent and unique light,
Physical properties and the chemical property such as electricity, heat, machinery.
Graphene and fibrous material it is compound, the functional fibre material of building has excellent absorption, catalysis, photo-thermal and electricity
Etc. performances.Many about graphene fiber preparation method at present, wherein electrostatic spinning is the common method for preparing nanofiber.
The preparation of composite nano fiber higher for graphene content easily leads to fiber since graphene is larger in lateral size
Fracture or not at silk, prepare it is larger, so not having relevant report and studying.
Summary of the invention
It is an object of that present invention to provide a kind of electrostatic spinnings and preparation method thereof of hydrophobic graphene composite high-molecular fiber.
To achieve the above object, the invention adopts a technical scheme as:
A kind of electrostatic spinning preparation method of hydrophobic graphene composite high-molecular fiber, with graphene, hydrophobic polymeric is
Raw material carries out the Static Spinning that electrostatic spinning obtains hydrophobic graphene composite high-molecular fiber by the method for electrostatic spinning
Silk.
Specifically:
(1) graphene, high molecular material are dissolved in organic solvent, and 10h is stirred to react in 70 DEG C, obtain spinning solution；
(2) by above-mentioned acquisition spinning solution, water bath sonicator 4h, the method for then passing through electrostatic spinning carry out electrostatic at room temperature
Spinning；
The electrostatic spinning nozzle is 10-20cm in receiving receiver distance, and spinning flow velocity is 2.0-4.0mL/h；And
It is carried out under conditions of 12-23kv voltage.
In the spinning solution by mass percentage, high molecular material 5%-30%, graphene 0.1%-3%, surplus are
Organic solvent.
The high molecular material is polymethyl methacrylate or polyacrylonitrile；Preferably polymethyl methacrylate；
Organic solvent is dimethylformamide or dimethyl acetamide；Preferably dimethylformamide.
The graphene is graphene subparticle, and lateral partial size is not more than 2 μm；Generally at 0.5 μm -2 μm；Graphene
Particle is smaller, and electrospun fibers continuity is better.
A kind of electrostatic spinning of the hydrophobic graphene composite high-molecular fiber of the method preparation gained, prepares according to the method
Obtain the electrostatic spinning of hydrophobic graphene composite high-molecular fiber.
Principle: the present invention utilizes the suction-operated between hydrophobic polymeric material polymethyl methacrylate and graphene
Power prepares fiber filament by electrostatic spinning, and graphene is wrapped in polymethylmethacrylate fibers, to be formed hydrophobic
Graphene composite high-molecular fibrous material.
The present invention has the advantage that
The electrostatic spinning for the hydrophobic graphene composite high-molecular fiber that the method for the present invention obtains is quick and easy, the reaction time
Short, graphene content is high, and fibrous material is environmental-friendly；Specifically:
1. electrostatic spinning preparation method of the invention overcomes high molecular material by water bath sonicator method and graphene is mixed
Dissolved agglomeration traits are closed,
2. and by adjust high molecular material account for mass concentration and spinning voltage in spinning solution, overcome electrostatic
The method of spinning prepares the problems such as existing spinning is discontinuous, not at silk when graphene composite fibre,
3. the graphene content that the method for the present invention obtains electrostatic spinning is high, fibrous material is environmental-friendly, and application field is wide,
Industrialization degree is high, and practical value is significant.
Detailed description of the invention
Fig. 1 is electrostatic spinning apparatus schematic diagram provided in an embodiment of the present invention；
Fig. 2 is the fiber condition schematic diagram of different polymethyl methacrylate dosage preparations provided in an embodiment of the present invention,
It is macromolecular fibre SEM image prepared by embodiment 4 that wherein figure A, which is macromolecular fibre SEM image figure B prepared by embodiment 1,；
Fig. 3 is the fiber condition schematic diagram of graphene dosage provided in an embodiment of the present invention preparation, wherein figure A is embodiment
The macromolecular fibre SEM image figure B of 1 preparation is macromolecular fibre SEM image prepared by embodiment 2, schemes C for the preparation of embodiment 3
Macromolecular fibre SEM image；
Fig. 4 is the fiber condition schematic diagram that under different voltages provided in an embodiment of the present invention prepared by electrostatic spinning, wherein scheming A
It is macromolecular fibre SEM image prepared by embodiment 5 for macromolecular fibre SEM image figure B prepared by embodiment 3, figure C is to implement
Macromolecular fibre SEM image prepared by example 6；
Fig. 5 is the fiber condition schematic diagram of different high molecular materials and solvent preparation provided in an embodiment of the present invention, wherein
Macromolecule is macromolecule: polymethyl methacrylate, solvent: dimethylformamide in left figure；Macromolecule in right figure: polypropylene
Nitrile, solvent: dimethyl acetamide.
Specific embodiment
A specific embodiment of the invention is described further below in conjunction with example, it is noted that retouch in this place
The specific embodiment stated is simply to illustrate that with the present invention is explained, it is not limited to the present invention.
For the present invention with graphene, hydrophobic polymeric is raw material, and the system of nano fibrous membrane is carried out by the method for electrostatic spinning
Standby, after overcoming high molecular material and graphene mixed dissolution agglomeration traits, and it is multiple being prepared with the method for electrostatic spinning
The problems such as existing spinning is discontinuous, not at silk when condensating fiber, electrostatic spinning preparation method of the invention is quick and easy, when reaction
Between it is short, graphene content is high, and fibrous material is environmental-friendly, and application field is wide, and industrialization degree is high, and practical value is significant.
Graphene used by following embodiments is graphene subparticle, and particles used transverse direction partial size is less than 2 μm.
Embodiment 1
A kind of electrostatic spinning preparation method of hydrophobic graphene modified high-molecular fiber, includes the following steps:
(1) graphene, polymethyl methacrylate and solvent dimethylformamide are mixed and heated to 70 DEG C of heating stirrings
10h, as mass fraction, graphene 0.1%, polymethyl methacrylate 20%, surplus is solvent dimethylformamide；
(2) then by the spinning solution under room temperature environment water bath sonicator 4h；Spinning solution after ultrasound is fitted into syringe,
Referring to Fig. 1, receiver is set, puts up electrostatic spinning apparatus, spray head is 10-20cm in receiving receiver distance；
(3) electrostatic spinning is carried out under conditions of 12kv voltage, spinning flow velocity 2.0-4.0mL/h, and then is obtained hydrophobic
The electrostatic spinning (referring to fig. 2,3) of graphene modified high-molecular fiber.
Embodiment 2
A kind of electrostatic spinning preparation method of hydrophobic graphene modified high-molecular fiber, includes the following steps:
(1) graphene, polymethyl methacrylate and solvent dimethylformamide are mixed and heated to 70 DEG C of heating stirrings
10h, as mass fraction, graphene 1.5%, polymethyl methacrylate 20%, surplus is solvent dimethylformamide；
(2) then by the spinning solution in water bath sonicator 4h；Spinning solution after ultrasound is fitted into syringe, sets reception
Device, puts up electrostatic spinning apparatus, and spray head is 10-20cm in receiving receiver distance；
(3) carry out electrostatic spinning under conditions of 12kv voltage, spinning flow velocity 2.0-4.0mL/h (referring to Fig. 3).
Embodiment 3
A kind of electrostatic spinning preparation method of hydrophobic graphene modified high-molecular fiber, includes the following steps:
(1) graphene, polymethyl methacrylate and solvent dimethylformamide are mixed and heated to 70 DEG C of heating stirrings
10h, as mass fraction, graphene 3%, polymethyl methacrylate 20%, surplus is solvent dimethylformamide；
(2) then by the spinning solution under room temperature environment water bath sonicator 4h；Spinning solution after ultrasound is fitted into syringe,
Receiver is set, electrostatic spinning apparatus is put up, spray head is 10-20cm in receiving receiver distance；
(3) carry out electrostatic spinning under conditions of 12kv voltage, spinning flow velocity 2.0-4.0mL/h (referring to Fig. 3,4).
Embodiment 4
A kind of electrostatic spinning preparation method of hydrophobic graphene modified high-molecular fiber, includes the following steps:
(1) graphene, polymethyl methacrylate and solvent dimethylformamide are mixed and heated to 70 DEG C of heating stirrings
10h, as mass fraction, graphene 0.1%, polymethyl methacrylate 10%, surplus is solvent dimethylformamide；
(2) then by the spinning solution in water bath sonicator 4h；Spinning solution after ultrasound is fitted into syringe, sets reception
Device, puts up electrostatic spinning apparatus, and spray head is 10-20cm in receiving receiver distance；
(3) electrostatic spinning (referring to fig. 2) is carried out under conditions of 12kv voltage, spinning flow velocity 2.0-4.0mL/h.
Embodiment 5
A kind of electrostatic spinning preparation method of hydrophobic graphene modified high-molecular fiber, includes the following steps:
(1) graphene, polymethyl methacrylate and solvent dimethylformamide are mixed and heated to 70 DEG C of heating stirrings
10h, as mass fraction, graphene 3%, polymethyl methacrylate 20%, surplus is solvent dimethylformamide；
(2) then by the spinning solution in water bath sonicator 4h；Spinning solution after ultrasound is fitted into syringe, sets reception
Device, puts up electrostatic spinning apparatus, and spray head is 10-20cm in receiving receiver distance；
(3) electrostatic spinning (referring to fig. 4) is carried out under conditions of 16kv voltage, spinning flow velocity 2.0-4.0mL/h.
Embodiment 6
A kind of electrostatic spinning preparation method of hydrophobic graphene modified high-molecular fiber, includes the following steps:
(1) graphene, polymethyl methacrylate and solvent dimethylformamide are mixed and heated to 70 DEG C of heating stirrings
10h, as mass fraction, graphene 3%, polymethyl methacrylate 20%, surplus is solvent dimethylformamide；
(2) then by the spinning solution in water bath sonicator 4h；Spinning solution after ultrasound is fitted into syringe, sets reception
Device, puts up electrostatic spinning apparatus, and spray head is 10-20cm in receiving receiver distance；
(3) electrostatic spinning (referring to fig. 4) is carried out under conditions of 23kv voltage, spinning flow velocity 2.0-4.0mL/h.
Embodiment 7
A kind of electrostatic spinning preparation method of hydrophobic graphene modified high-molecular fiber, includes the following steps:
(1) graphene, polyacrylonitrile and solvent dimethyl acetamide are mixed and heated to 70 DEG C of heating stirring 10h, by matter
Score meter is measured, graphene 0.1%, polyacrylonitrile 10%, surplus is solvent dimethyl acetamide；
(2) then by the spinning solution in water bath sonicator 4h；Spinning solution after ultrasound is fitted into syringe, sets reception
Device, puts up electrostatic spinning apparatus, and spray head is 10-20cm in receiving receiver distance；
(3) carry out electrostatic spinning under conditions of 12kv voltage, spinning flow velocity 2.0-4.0mL/h (referring to Fig. 5).
From above-mentioned Fig. 2-5
A) the influence of polymethyl methacrylate dosage:
Macromolecular fibre film prepared by embodiment 1,4 carries out Electronic Speculum observation, polymethyl methacrylate additional amount difference
It is prepared by 10%, 20% additive amount, other conditions are identical, and the fibre density prepared is shown in Fig. 2, it can be seen that with
The increase of polymethyl methacrylate content, fiber are finer and close.
B) the influence of graphene dosage:
Macromolecular fibre film prepared by embodiment 1-3 carries out Electronic Speculum observation, graphene additional amount presses 0.1% respectively,
1.5%, prepared by 3% additive amount, and other conditions are identical, and the fibre morphology prepared is shown in Fig. 3, it can be seen that with stone
The increase of black alkene content still has fibre morphology although the continuity of fiber is deteriorated.
C) the influence of voltage:
Macromolecular fibre film prepared by embodiment 3,5,6 carries out Electronic Speculum observation, respectively with the electricity of 12kv, 16kv, 23kv
Pressure carries out electrostatic spinning, remaining condition is identical, and the fibre morphology prepared is shown in Fig. 4, it can be seen that with the raising of voltage,
Fibre diameter reduces, and configuration of surface is roughening.
D) the influence of high molecular material and solvent:
Macromolecular fibre film prepared by embodiment 4,7 carries out Electronic Speculum observation, and selecting high molecular material is respectively poly- methyl
Methyl acrylate and polyacrylonitrile and solvent are respectively prepared by dimethylformamide and dimethyl acetamide.The fibre prepared
Dimension form is shown in Fig. 5, it can be seen that different high molecular materials and solvent can make fiber consistency and diameter change, and equal
With good fibre morphology.
High molecular material can be replaced with into polypropylene by polymethyl methacrylate according to the record of above-described embodiment simultaneously
Nitrile, such high molecular material substance have hydrophobicity, chain characteristic, can be made up of admixed graphite alkene particle and electrostatic spinning
Hydrophobic graphene composite film, and then be replaced mutually and be able to achieve the present invention；In addition, solvent can be replaced by dimethylformamide
For dimethyl acetamide, which is polar non-proton organic solvent, can dissolve above-mentioned high molecular material preparation and contain stone
Hydrophobic graphene composite film is made for electrostatic spinning in the spinning solution of black alkene and high molecular material.
It should be pointed out that the above specific embodiment is only illustrative of the invention and is not intended to limit the scope of the invention,
After having read the present invention, those skilled in the art fall within power appended by the application to the modification of various equivalent forms of the invention
Benefit requires limited range.
Claims (7)
1. a kind of electrostatic spinning preparation method of hydrophobic graphene composite high-molecular fiber, it is characterised in that: hydrophobic with graphene
Macromolecule is raw material, carries out electrostatic spinning by the method for electrostatic spinning and obtains hydrophobic graphene composite high-molecular fiber
Electrostatic spinning.
2. the electrostatic spinning preparation method of hydrophobic graphene composite high-molecular fiber according to claim 1, it is characterised in that:
(1) graphene, high molecular material are dissolved in organic solvent, and 10h is stirred to react in 70 DEG C, obtain spinning solution；
(2) by above-mentioned acquisition spinning solution, water bath sonicator 4h, the method for then passing through electrostatic spinning carry out electrostatic spinning at room temperature.
3. the electrostatic spinning preparation method of hydrophobic graphene composite high-molecular fiber as described in claim 1 or 2, feature exist
In: the electrostatic spinning nozzle is 10-20cm in receiving receiver distance, and spinning flow velocity is 2.0-4.0mL/h；And in 12-
It is carried out under conditions of 23kv voltage.
4. the electrostatic spinning preparation method of hydrophobic graphene composite high-molecular fiber as described in claim 1 or 2, feature exist
In: in the spinning solution by mass percentage, high molecular material 5%-30%, graphene 0.1%-3%, surplus are organic molten
Agent.
5. the electrostatic spinning preparation method of hydrophobic graphene composite high-molecular fiber according to claim 4, it is characterised in that:
The high molecular material is polymethyl methacrylate or polyacrylonitrile；Organic solvent is dimethylformamide or dimethylacetamide
Amine.
6. the electrostatic spinning preparation method of hydrophobic graphene composite high-molecular fiber according to claim 4, it is characterised in that:
The graphene is graphene subparticle, and lateral partial size is not more than 2 μm.
7. a kind of electrostatic spinning of the hydrophobic graphene composite high-molecular fiber of claim 1 the method preparation gained, feature
It is: prepares the electrostatic spinning of hydrophobic graphene composite high-molecular fiber by claim 1 method.
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Cited By (2)
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| CN113402809A (en) * | 2021-05-27 | 2021-09-17 | 北京汽车研究总院有限公司 | Porous graphene honeycomb core material and preparation method and application thereof |
| CN113832610A (en) * | 2021-09-27 | 2021-12-24 | 武汉大学 | Flexible super-stretching super-hydrophobic electronic device substrate and preparation method and application thereof |
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Application publication date: 20190730 |