CN106757532B - A kind of preparation method of graphene-based doughnut - Google Patents
A kind of preparation method of graphene-based doughnut Download PDFInfo
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- CN106757532B CN106757532B CN201611121466.2A CN201611121466A CN106757532B CN 106757532 B CN106757532 B CN 106757532B CN 201611121466 A CN201611121466 A CN 201611121466A CN 106757532 B CN106757532 B CN 106757532B
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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
Abstract
The invention discloses a kind of preparation methods of graphene-based doughnut, heat-shrinkable macromolecular fibre surface graphene-based material layer is coated with for the first time to be formed after core is the composite fibre that macromolecular fibre shell is graphene-based material layer, using composite fibre center floor height molecular fiber and the characteristic of the graphene-based material percent thermal shrinkage difference of shell in the case that be heated to stratum nucleare macromolecular fibre shrink more than 2% and shell graphene-based material heating volume change is little detaches the two, the macromolecular fibre that stratum nucleare is shunk is taken out from composite fibre then and can be obtained graphene-based doughnut.This method using be easy to get, and the heat shrink polymer fiber that can recycle compatible with textile industry be template prepare graphene-based doughnut not only facilitate it is environmentally friendly and also it is easily prepared include the graphene-based fiber of more graphene-based fibre bundles and polymorphic structure the features such as, therefore contribute to the further genralrlization application of graphene-based doughnut.
Description
Technical field
The invention belongs to Material Fields, are related to a kind of preparation method of graphene-based doughnut.
Background technology
Graphene is a kind of conductive material, excellent mechanical property (Young's modulus is up to 1.0TPa), electrical properties (electricity
Transport factor is up to 106cm2.v-1s-1), (thermal conductivity coefficient is up to 5000w.m to thermal property-1.k-1), optical property (mono-layer graphite
The visible absorption of alkene only has 2.3% and excellent mode locking characteristic), the theoretical specific surface area (2630m of super large2.g-1) and monolithic
Layer structure assigns its unique chemistry and electro-chemical activity makes graphene in electronics, information, the energy, material and biological medicine etc.
Field has great application prospect.By the graphene doughnut of graphene structure on the basis for keeping graphene inherent characteristic
On also there is good flexibility, higher surface area, thus including fields such as electrode material, energy storage material, catalysis materials
There is potential using value and is paid high attention to by people.People mainly develop to deposit graphene then on copper wire at present
It sacrifices copper line method and redox graphene and prepares graphene doughnut by coaxial spin processes, however both methods exists
Sacrifice method is expensive and coaxial spin processes since it is desired that graphene oxide is combined with solidification material and generates larger volume and become
Change and the more coarse problem in surface, therefore there is an urgent need to develop the technologies of new graphene doughnut.The application exists for the first time
The characteristic being heat-shrinked based on macromolecular fibre is proposed in the world, is coated with graphene-based material layer on macromolecular fibre first, so
Heating makes the macromolecular fibre of stratum nucleare be detached from the graphene-based material layer of shell because percent thermal shrinkage is different afterwards, then will
The macromolecular fibre of contraction takes out and obtains the technology of graphene-based doughnut from graphene-based doughnut.The technology has
Have it is of low cost, it is compatible with textile industry, prepared graphene-based doughnut can utilize tow in textile industry and
Polymorphic structure and the graphene-based doughnut for obtaining rich variety, therefore be conducive to the further hair of graphene-based doughnut
Exhibition and application.
Invention content
Technical problem:The object of the present invention is to provide a kind of preparation methods of graphene-based doughnut, by being received in heat
Contracting macromolecular fibre surface is coated with graphene-based material layer, then thermal release macromolecular fibre and prepare graphene-based hollow fibre
Dimension, have it is cheap, graphene-based doughnut is compatible with textile industry, it is easily prepared include tow, polymorphic structure stone
The features such as mertenyl doughnut, therefore contribute to the further development and popularization and application of graphene-based doughnut.
Technical solution:It is molten that a kind of preparation method of graphene-based doughnut of the present invention prepares graphene-based material first
Then above-mentioned solution coating is obtained core shell structure composite fiber on selected heat shrink polymer fiber, then heated by liquid
Composite fibre makes the graphene-based material layer of shell and the macromolecular fibre layer separation of stratum nucleare, then extracts macromolecular fibre
Out obtain graphene-based doughnut.
The graphene-based material refers to graphene and its derivative;
The heat shrink polymer fiber refers to the macromolecular fibre that fibre shrinkage is more than 2% after the heating.
The solution coating refers to dip-coating or is sprayed into selected macromolecular fibre surface and is subsequently dried and is cured
Graphene-based material layer.
The heating composite fibre refers to heating composite fibre by hot-air or the hot solvent including water.
The heating composite fibre so that the graphene-based material layer of shell and the macromolecular fibre layer separation of stratum nucleare refer to
Heating is so that the macromolecular fibre of stratum nucleare is shunk more than 2%, and then heated volume change is unknown for the graphene-based material layer of shell
It is aobvious so that the macromolecular fibre of stratum nucleare and the graphene-based material layer of shell cannot maintain Full connected and in object due to volume difference
Reason effect hypostratum is detached with stratum nucleare;
Described extract macromolecular fibre refers in the graphene-based material layer of shell and stratum nucleare macromolecular fibre heat point
The stratum nucleare macromolecular fibre of contraction is extracted out of shell graphene-based material layer by the mechanical stretching shell and stratum nucleare by from rear
Out or by the graphene-based material layer of shell exited from the macromolecular fibre of thermal contraction.
Advantageous effect:Compared with prior art, the present invention haing the following advantages:
It is macromolecular fibre shell that heat-shrinkable macromolecular fibre is coated with graphene-based material layer to form core by the present invention for the first time
After composite fibre for graphene-based material layer, the graphene-based material using macromolecular fibre layer heat shrinkable in composite fibre
Then the little characteristic of heated volume change detaches the two to layer, then takes the macromolecular fibre that stratum nucleare is shunk from composite fibre
Go out and can be obtained graphene-based doughnut.This method is mould using the heat shrink polymer fiber that is easy to get and can recycle
It is that the process that template needs chemical attack to remove copper wire facilitates ring with preparation that plate, which prepares graphene-based doughnut compared to copper wire,
The characteristic of guarantor, therefore contribute to the further genralrlization application of graphene doughnut.
Specific implementation mode
With reference to embodiment, the present invention is further illustrated.
Embodiment one:
Graphene oxide powder is prepared first.30 grams of graphite mixing 15g sodium nitrate and 750 milliliters of concentrated sulfuric acids.By mixture
It is cooled to 0 degree Celsius in ice bath, and after stirring 2h, is slowly added to 90 grams of potassium permanganate, keeps mixture temperature in mixed process
Degree is less than 5 degrees Celsius.The mixture is stirred for a hour, and is heated to room temperature by removing ice bath.1 is added in mixture
It rises distilled water and temperature in oil bath increases to 90 degrees Celsius.In addition 300 milliliters of water are added, and are stirred for one and a half hours.
The color of mixture becomes brown.Mixture is then with 30% 300 milliliters of hydrogen peroxide and 30 liters of hot water treatments and dilution.It should
Mixture is further with excessive water washing, and until the pH value of filtrate is almost neutral, subsequent filter cake vacuum drying is to obtain
Obtain graphene oxide powder.
Secondly the nylon-6 fiber for obtaining 20D, in addition prepares the graphene oxide water solution of 1 mg/ml, then will be bright and beautiful
6 fiber of synthetic fibre is with the speed of 0.1 cm/s by the graphene oxide solution of 10 centimeter lengths, and then drying at room temperature, then raises temperature to
150 degrees Celsius and keep the temperature 10 minutes, nylon-6 fiber shrink about 7.5%, be then cooled to room temperature and the nylon-6 fiber by contraction
It is taken out from composite fibre, obtains the graphene oxide doughnut that diameter is about 50 microns.The fiber can be restored further
To prepare graphene doughnut.
Embodiment two:
Method as in the first embodiment, but a concentration of 10 mg/ml of graphene oxide water solution, nylon-6 fiber it is long by 1 meter
Graphene oxide solution speed be 1 cm/s.The hollow fibre of graphene oxide that diameter is about 50 microns can equally be obtained
Dimension.
Embodiment three:
Redox graphene is prepared first.By the graphene oxide prepared in embodiment one disperse in water and with hydration
Hydrazine restores 12 hours at 80 degrees Celsius.Redox graphene is formed with black precipitate, is collected by filtration with 0.45 μm of PTFE film,
It is used in combination a large amount of water to rinse.Product is further purified by methanol, tetrahydrofuran (THF) and water with soxhlet extraction.Finally, institute
The subzero 120 degrees Celsius of freeze-dryings under 0.05 millimetres of mercury vacuum environment of the redox graphene of acquisition.Secondly 7D terylene is obtained
In addition monofilament prepares the redox graphene ethanol solution of 2 mg/mls, then by polyester monofilament with the speed of 1 point of meter per second
Degree is by the graphene oxide solution of 50 centimeter lengths, and then drying at room temperature, then raises temperature to 177 degrees Celsius and keep the temperature 30 minutes,
Polyester monofilament filament contraction about 5.6% is then cooled to room temperature and takes out the polyester monofilament of contraction from composite fibre, obtains
The graphene oxide doughnut that diameter is about 17 microns.
Example IV:
111dtex/24f terylene high convergency FDY (fully drawn yarn) are obtained first, in addition prepare the oxidation stone of 5 mg/mls
Black aqueous solution, it is then that PET High Shrinkage FDY is molten by the graphene oxide of 60 centimeter lengths with the speed of 1 point of meter per second
Then liquid is dried in vacuo 10 hours for 50 degrees Celsius, then raise temperature to 120 degrees Celsius and keep the temperature 20 minutes, terylene high convergency is drawn entirely
It stretches silk and shrinks about 22%, be then cooled to room temperature and take out the PET High Shrinkage FDY of contraction from composite fibre, obtain
The oxygen that the overall diameter formed to the graphene oxide doughnut for being about 20 microns by 24 single diameters arranged side by side is about 250 microns
Graphite alkene fibre bundle.
Embodiment five:
Zhong Fang investment companies 797dtex/20F high strength PE fibers are obtained first, in addition prepare the oxygen reduction of 7 mg/mls
Graphite aqueous solution, it is then that high strength PE fiber is molten by the redox graphene of 50 centimeter lengths with the speed of 1 meter per second
Liquid, then drying at room temperature, then raises temperature to 135 degrees Celsius and keeps the temperature 30 minutes, and high strength PE fiber shrinks about 3%, will then receive
The high strength PE fiber of contracting takes out from composite fibre, obtains the reduction-oxidation graphite for being about 73 microns by 20 single diameters arranged side by side
The redox graphene fibre bundle that the overall diameter of alkene doughnut composition is about 1460 microns.
Embodiment six:
Zhong Fang investment companies 797dtex/20F high strength PE fibers are obtained first, in addition prepare the graphene of 5 mg/mls
Hexafluoroisopropanol solution, then by high strength PE fiber with the speed of 1 point of meter per second by the graphene solution of 50 centimeter lengths, then
Composite fibre is then warming up to 135 degrees Celsius and keeps the temperature 30 minutes by drying at room temperature, and high strength PE fiber contraction about 3% is then cold
But it is taken out from composite fibre to room temperature and by the high strength PE fiber of contraction, obtains by 20 single diameters arranged side by side being about 73 microns
Graphene doughnut composition overall diameter be about 1460 microns graphene fiber beam.
Embodiment seven:
Zhong Fang investment companies 797dtex/20F high strength PE fibers are obtained first, in addition prepare the oxygen reduction of 6 mg/mls
Then graphite aqueous solution is run high strength PE fiber with the speed of 20 meter per seconds, and by nozzle by redox graphene
Aqueous solution is sprayed on high strength PE fiber, is sprayed again to high strength PE fiber with another nozzle again after running 500 meters of intervals,
Then it is dried in vacuo 24 hours for 60 degrees Celsius, then raises temperature to 135 degrees Celsius and keeps the temperature 30 minutes, high strength PE fiber is shunk about
3%, it is then cooled to room temperature and takes out the high strength PE fiber of contraction from composite fibre, obtain by 20 single straights arranged side by side
The redox graphene that the overall diameter for the redox graphene doughnut composition that diameter is about 73 microns is about 1460 microns
Fibre bundle.
Embodiment eight:
Obtain first by one side length of side be 470 microns of other both sides length of sides be 410 microns triangle spinneret orifice through 5 times
One side length of side for stretching and preparing is about 6 triangle profiled filament of polyamide fibre that 90 microns of other both sides length of sides are about 80 microns, separately
The outer graphene oxide water solution for preparing 6 mg/mls, then passes through 50 centimetres by nylon-6 fiber with the speed of 1 point of meter per second
Long graphene oxide solution, then drying at room temperature, then raises temperature to 150 degrees Celsius and keeps the temperature 10 minutes, nylon-6 fiber is received
Contraction 7.5% is then cooled to room temperature and takes out the nylon-6 fiber of contraction from composite fibre, and obtaining one side length of side is about
90 microns and graphene oxide triangle Profiled hollow fiber that in addition the both sides length of sides is about 80 microns.
Embodiment nine:
It is 400 microns to be obtained first by brachium, and width is 200 microns, and the trilobal that the radius of top arc is 100 microns is sprayed
The brachium that wire hole is stretched through 5 times and prepared is 80 microns, and width is 40 microns, and the trilobal that the radius of top arc is 20 microns is different
In addition shape nylon-6 fiber prepares the graphene oxide water solution of 8 mg/mls, then by nylon-6 fiber with the speed of 10 meter per seconds
Degree operation, and graphene oxide water solution is sprayed on nylon-6 fiber by nozzle, it is used again in addition after running 300 meters of intervals
One nozzle sprays nylon-6 fiber again, is then dried in vacuo 24 hours for 50 degrees Celsius, then raises temperature to 150 degrees Celsius simultaneously
Heat preservation 10 minutes, nylon-6 fiber shrink about 7.5%, are then cooled to room temperature and by the nylon-6 fiber of contraction from composite fibre
It takes out, it is about 80 microns to obtain brachium, and width is about 40 microns, and the trilobal abnormity that the radius of top arc is about 20 microns aoxidizes
Graphene doughnut.
Embodiment ten
111dtex/24f terylene high convergency FDY (fully drawn yarn) are obtained first, in addition prepare the oxidation stone of 5 mg/mls
Black aqueous solution, it is then that PET High Shrinkage FDY is molten by the graphene oxide of 30 centimeter lengths with the speed of 1 point of meter per second
Liquid, then 50 degrees Celsius be dried in vacuo 24 hours, composite fibre is then kept the temperature 20 minutes in 100 degrees Celsius of boiling water so that
PET High Shrinkage FDY is shunk, be then cooled to room temperature and by the PET High Shrinkage FDY of contraction from composite fibre
Middle taking-up, obtain be about by the overall diameter that the graphene oxide doughnut that 24 single diameters arranged side by side are about 20 microns forms
250 microns of graphene oxide fibre bundle.
Embodiment 11
The graphene platelet of edge carboxylated is prepared first.5 grams of graphite and 100 grams of dry ice additions contain 1000 grams of diameter
In the stainless steel capsule of 5 millimeters of stainless steel balls.Container is sealed and is fixed on planetary ball mill (F-P4000), and with 500rpm
(rev/min) speed stirs 48 hours.Then, internal pressure passes through a gas vent slow release.Pass through at the end of ball milling
Container cover is opened in air, and violent hydration reaction generation carboxylic acid is occurred by the wet steam initiation carboxylate in air and sends out sudden strain of a muscle
Light.Products obtained therefrom carries out soxhlet type to be thoroughly acidified carboxylate and remove presumable metal impurities with 1M hydrochloric acid solutions.Most
Subzero 120 degrees Celsius of freeze-dryings obtain edge carboxylated graphene nanometer sheet in 48 hours under 0.05 millimetres of mercury vacuum environment eventually
Furvous powder.Secondly 111dtex/24f terylene high convergency FDY (fully drawn yarn) are obtained, in addition by the edge carboxyl of 0.1wt%
Graphite alkene nanometer sheet passes through the evenly dispersed solution of the ultrasound acquisition in 30 minutes in isopropanol.Then by terylene high convergency FDY
It is run with the speed of 1 meter per second, and is sprayed to the edges 0.1wt% carboxylated graphene nanometer sheet aqueous isopropanol by nozzle
In terylene high convergency FDY fiber, reruns 100 meters and terylene high convergency FDY fiber is sprayed with other nozzle after being spaced, spray
After applying 5 times, 50 degrees Celsius are dried in vacuo 24 hours, then raise temperature to 120 degrees Celsius and keep the temperature 20 minutes, terylene high convergency is drawn entirely
It stretches silk and shrinks about 22%, be then cooled to room temperature and take out the PET High Shrinkage FDY of contraction from composite fibre, obtain
The overall diameter formed to the edge carboxylated graphene doughnut for being about 20 microns by 24 single diameters arranged side by side is about 250 micro-
The edge carboxylated graphene fiber beam of rice.
Embodiment 12
The halogenated graphene nanometer sheet in edge is prepared first.5 grams of graphite additions contain 1000 grams 5 millimeters of stainless steel balls of diameter
Stainless steel capsule in.Then capsule seals and five cycles charge and discharge argon gas under 0.05 millimetres of mercury vacuum pressure condition.
Hereafter, it is that chlorine is added from gas access in 8.75atm by cylinder pressure.Container is sealed and is fixed on planetary ball mill (F-
P4000 it), and with 500rpm (rev/min) speed stirs 48 hours.Successively methanol and 1M hydrochloric acid solutions carry out Soxhlet to products obtained therefrom
Extracting is thoroughly to remove small molecule organic impurities and presumable metal impurities.Finally zero under 0.05 millimetres of mercury vacuum environment
Lower 120 degrees Celsius of freeze-dryings, 48 hours furvous powder for obtaining edge chlorination graphene nanometer sheet.Secondly it is 400 to obtain by brachium
Micron, width are 200 microns, and the radius of top arc stretches the brachium prepared for 100 microns of trilobal spinneret orifice through 5 times
It it is 80 microns, width is 40 microns, the trilobal abnormity high-strength polyethylene fiber that the radius of top arc is 20 microns.Then match
Make the edge chloro graphene N of 0.1 mg/ml, N '-dimethyl formamide DMF solution.Then trilobal abnormity high intensity is poly-
Vinyl fiber is run with the speed of 1 point of meter per second, and allows fiber apart from 6 centimetres of electrostatic atomiser nozzle, is applied on electrostatic spray nozzles
Add the voltage of 8KV, and by nozzle that the edge chloro graphene DMF of 0.1 mg/ml is molten with 200 mul/min of speed
Liquid sprays on trilobal abnormity nylon-6 fiber, subsequent drying at room temperature, and repeats electrostatic spraying and drying at room temperature 10 times, then
It is warming up to 150 degrees Celsius and keeps the temperature 10 minutes, trilobal abnormity high-strength polyethylene fiber shrinks about 3%, is then cooled to room
Temperature simultaneously takes out the trilobal abnormity high-strength polyethylene fiber of contraction from composite fibre, and it is about 80 microns to obtain brachium, wide
About 40 microns of degree, the trilobal abnormity edge chloro graphene doughnut that the radius of top arc is about 20 microns.
Claims (6)
1. a kind of preparation method of graphene-based doughnut, which is characterized in that prepare graphene-based material solution first, then
Above-mentioned solution coating is obtained into core shell structure composite fiber on selected heat shrink polymer fiber, then heats composite fibre
So that the graphene-based material layer of shell is detached with the macromolecular fibre layer of stratum nucleare because of the difference of the ability of thermal contraction, then will
The macromolecular fibre of contraction, which extracts, obtains graphene-based doughnut.
2. a kind of preparation method of graphene-based doughnut according to claim 1, which is characterized in that the graphene
Sill refers to graphene and its derivative.
3. a kind of preparation method of graphene-based doughnut according to claim 1, which is characterized in that the thermal contraction
Macromolecular fibre refers to the macromolecular fibre that fibre shrinkage is more than 2% after the heating.
4. according to a kind of preparation method of graphene-based doughnut described in claim 1, which is characterized in that the solution
Coating refers to that graphene-based material solution is applied to selected macromolecular fibre surface by dip-coating or spraying and is then done
It is dry and obtain cured graphene-based material layer.
5. a kind of preparation method of graphene-based doughnut according to claim 1, which is characterized in that the heating is multiple
Condensating fiber refers to heating composite fibre by hot-air or the hot solvent including water.
6. a kind of preparation method of graphene-based doughnut according to claim 1, which is characterized in that described by high score
It refers to passing through mechanical stretching after the graphene-based material layer of shell and stratum nucleare macromolecular fibre layer thermal release that subbundle, which extracts,
Shell and stratum nucleare and the stratum nucleare macromolecular fibre of contraction is extracted out of shell graphene-based material layer or by shell
Graphene-based material layer is exited from the macromolecular fibre of thermal contraction.
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CN104150472A (en) * | 2014-08-01 | 2014-11-19 | 清华大学 | Graphene hollow nano fiber and preparation method thereof |
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