CN108385209A - The preparation method of porous filamentous nanocarbon - Google Patents
The preparation method of porous filamentous nanocarbon Download PDFInfo
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- CN108385209A CN108385209A CN201810174916.7A CN201810174916A CN108385209A CN 108385209 A CN108385209 A CN 108385209A CN 201810174916 A CN201810174916 A CN 201810174916A CN 108385209 A CN108385209 A CN 108385209A
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- pan
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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
- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
Abstract
The invention discloses a kind of preparation methods of porous PAN base nano carbon fibres, include the following steps：PVP and PAN are weighed respectively, DMF is added, and heating stirring dissolves to obtain PVP and PAN solution；It is fixed on electrostatic spinning machine by PVP and PAN solution inhalation syringes, then syringe, is that sandwich layer carries out coaxial electrostatic spinning using PAN solution as cortex, PVP solution；The tunica fibrosa being spun into heats into the water, and hollow PAN nanofibers are dried to obtain after flushing；Hollow PAN nanofibers are pre-oxidized；Under nitrogen protection, 500~700 DEG C are warming up to the heating rate of 1~5 DEG C/min, then 800~1000 DEG C is warming up to the heating rate of 1~10 DEG C/min, carbonized, then be down to room temperature naturally to get porous PAN base nano carbon fibres.The present invention prepares the nanofiber with unique microcellular structure and larger specific surface area by electrospinning process, has broader practice foreground in fields such as catalysis, battery diaphragm, high efficiency filters.
Description
Technical field
The present invention relates to technical field of nano material, and in particular to a kind of preparation method of porous filamentous nanocarbon.
Background technology
Porous carbon material have flourishing nano aperture, high specific surface area, excellent electric conductivity and bioaffinity,
Many excellent properties such as high temperature resistant, creep resistant, conduction, heat conduction and far infrared radiation, in absorption, catalysis, medicine, the energy, environmental protection
Equal fields all have purposes even irreplaceable extensively.With the deep development of nanometer science and technology, people are to nanometer
More stringent requirements are proposed for structure design, synthesis, performance and the application of material.
However, the nano aperture and charcoal skeleton of existing most of porous carbon materials are random arrangements in size and spatially
, such as activated carbon, activated carbon fiber, carbon aerogels etc.；Existing process of preparing can not be constructed and provide novel forms
With the nanostructure of special tectonic, the performance of nano material and application field is made to be restricted.
Therefore, there is an urgent need for the porous structures within the scope of nanoscale to carry out developmental research, makes the preparation skill of carbon nano-material
Art develops towards ordered structure and the direction cut out.
Invention content
The technical problem to be solved in the present invention is to provide a kind of preparation methods of porous filamentous nanocarbon, have to prepare
The porous PAN base nano carbon fibres of the nanostructure of novel forms and special tectonic.
In order to solve the above technical problems, the technical thought of the present invention is as follows：
It first passes through electrostatic spinning technique and realizes polymer/polymer, polymer/inorganic object and inorganic matter/inorganic matter composite Nano
The preparation of fiber obtains the controllable macromolecular fibre of size by high-pressure electrostatic, then passes through the works such as pre-oxidation, the charing of optimization
The porous filamentous nanocarbon of the nanostructure with novel forms and special tectonic is prepared in skill measure.
The specific technical solution that the present invention uses for：
A kind of preparation method of porous filamentous nanocarbon is designed, is included the following steps：
（1）It weighs PVP and PAN respectively, is added DMF, stirring and dissolving obtains the PVP of a concentration of 0.05~0.3 g/mL at 60~80 DEG C
With PAN solution；
（2）It is fixed on electrostatic spinning machine by PVP and PAN solution inhalation syringes, then syringe, using PAN solution as skin
Layer, PVP solution are that sandwich layer carries out coaxial electrostatic spinning；
（3）The tunica fibrosa being spun into heats into the water, and hollow PAN nanofibers are dried to obtain after flushing；
（4）Hollow PAN nanofibers are pre-oxidized, the pre-oxidizing conditions are：
Under the air conditions of flowing, 150 DEG C, constant temperature 3h are warming up to from room temperature with the heating rate of 1 DEG C/min, then with 0.5~2
DEG C/heating rate of min is warming up to 250~300 DEG C, keep Temperature fall after 1~5 h；
（5）Under atmosphere of inert gases, 500~700 DEG C are warming up to the heating rate of 1~5 DEG C/min, then with 1~10 DEG C/
The heating rate of min is warming up to 800~1000 DEG C, is carbonized, then is down to room temperature naturally to get porous PAN bases Nano carbon fibers
Dimension.
Preferably, the step（2）In, the propeller fltting speed control of the electrostatic spinning machine is 0.1~0.3mL/
The positive voltage control of h, the spinning are 15~25kV, and vacuum cavitations are -5~0kV.
Preferably, the step（3）In, the temperature control of the heating is 50~70 DEG C, and time control is 5~7 hours；
The temperature control of the drying is 60~80 DEG C, and time control is 5~7 hours.
Preferably, the step（5）In, the inert gas is at least one in ammonia, nitrogen, hydrogen, argon gas
Kind；The time control of the charing is 0.2~3h.
Compared with prior art, the beneficial technical effect of the present invention lies in：
1. the present invention by electrospinning process prepares the nanofiber with porous structure, in catalysis, battery diaphragm, efficiently
There is broader practice foreground in the fields such as filtering.
2. the formed nano aperture of porous filamentous nanocarbon and charcoal skeleton that the present invention prepares have in size and spatially
Sequence arranges, and has unique, novel microcellular structure and larger specific surface area, thus has more unique surface nature, can
Applied to fields such as adsorbing separation, catalyst carrier, filtering, biological organization materials.
3. constructing for multiple material one-dimensional nano structure not only may be implemented using high-voltage electrostatic spinning technology in the present invention, and
And may be implemented the size of nanostructure, pattern it is adjustable controllable.
Description of the drawings
Fig. 1 is that the SEM of porous PAN base nano carbon fibres schemes；
Fig. 2 is the adsorption-desorption isothermal curve graph of porous PAN base nano carbon fibres；
Fig. 3 is the BJH graph of pore diameter distribution of porous PAN base nano carbon fibres.
Specific implementation mode
Illustrate the specific implementation mode of the present invention with reference to the accompanying drawings and examples, but following embodiment is used only in detail
It describes the bright present invention in detail, does not limit the scope of the invention in any way.
Involved instrument and equipment is routine instrument device unless otherwise instructed in the examples below；Involved
Reagent is commercially available conventional reagent unless otherwise instructed；Involved test method is unless otherwise instructed conventional method.
Embodiment one：The preparation method of porous PAN base nano carbon fibres
1. weighing suitable polyvinylpyrrolidone（PVP）And polyacrylonitrile（PAN）, it is separately added into appropriate dimethylformamide
（DMF）, 70 DEG C of water-baths are set, is that 500 r/min or so carry out heating magnetic agitation dissolving with rotating speed, is configured to certain density molten
Liquid；
Wherein, a concentration of 0.05~0.3 g/mL of PVP and PAN.
2. by the solution inhalation syringe prepared, while ensureing in syringe tube without bubble.Syringe is fixed on
On the propulsion system device of electrostatic spinning machine；
3. being that sandwich layer carries out coaxial electrostatic spinning using PAN solution as cortex, PVP solution；
Positive voltage is 15~25kV when spinning, and negative pressure is -5~0kV；The fltting speed of two propellers is 0.2 mL/h；Solution
The spinning time is 12 hours；
4. the tunica fibrosa being spun into is placed in the beaker for being loaded with distilled water.60 DEG C of heating water baths 6 hours；
5. then with distilled water flushing 5 times, then with alcohol rinse one time, it is placed in surface plate and is placed in 70 DEG C of baking ovens 6 hours,
Obtain hollow PAN nanofibers；
It is pre-oxidized 6. hollow PAN nanofibers are placed in tube furnace, pre-oxidizing conditions are：
Under the air conditions of flowing, tube furnace is warming up to 150 DEG C, constant temperature 3h from room temperature with the heating rate of 1 DEG C/min, then with
The heating rate of 0.5~2 DEG C/min is warming up to 250~300 DEG C, keeps Temperature fall after 1~5 h, when temperature drops to room temperature,
Close oxygen supply equipment；
7. opening the valve of nitrogen cylinder, under flowing nitrogen protection, tube furnace is from room temperature with the heating rate liter of 1~5 DEG C/min
Temperature is warming up to 900 DEG C to 600 DEG C, then with the heating rate of 1~10 DEG C/min, carbonizes 0.2~3h at this temperature, is down to naturally
Room temperature is to get to porous PAN base nano carbon fibres.
Embodiment two：Detect the surface topography of porous PAN base nano carbon fibres
The microstructure of porous PAN base nano carbon fibres sample uses 250 scanning electrons of Quanta of FEI Co. of Czech production
Microscope（SEM）It is tested.
Testing result is shown in Fig. 1.
As shown in Figure 1：Material keeps the orderly shape of fiber after charing, and high polymer nanometer fiber fragments into short at high temperature
Fiber, even in fiber diameter distribution, for 600 nm or so, hollow structure inside, pore size distribution is uniform.Due to non-carbon after charing
Atom is eliminated in the form of gas molecule, and carbon fiber skeleton surface becomes coarse, and material base is provided for specific surface area.
Embodiment three：Detect the pore structure of porous PAN base nano carbon fibres
Pore structure utilizes the full-automatic specific surface areas of 2QDS-MP-30 and Porosimetry of Quantachrome companies of U.S. production
The N of determination sample2Then adsorption-desorption isothermal utilizes Brunauer-Emmett-Teller（BET）Method calculates specific surface
Product SBET, micro pore surface area S is calculated with t-plot methodsmicWith micro pore volume Vmic。
The N of porous PAN base nano carbon fibres sample2Adsorption-desorption isothermal is as shown in Figure 2.
As shown in Figure 2：
With the increase of carbonization-activation temperature, sample is to N2Adsorbance increase.Adsorbance is with opposite pressure under low relative pressure
Power P/P0Increase steeply rise, with further increasing for relative pressure, adsorbance growth become slow, and occur one suction
Attached platform, with the presence of micropore in the material illustrated.
The thermoisopleth belongs to IV class adsorption isotherm, shows that sample belongs to micropore and Carbon Materials that are mesoporous and depositing, opposite
There is larger desorption and lags winding in pressure when being 0.4, this is because initially happens is that single layer and multilayer in middle hole wall
Absorption, then has occurred capillary condensation in duct.
According to N2Adsorption-desorption isothermal uses the pore size distribution curve that BJH methods are calculated, as shown in figure 3, from figure
In as can be seen that obtain there are mesoporous and macropore in carbon nano-fiber, aperture concentrates on 4 nm or so.
Physical absorption is the effect due to adsorbent surface gravitational field, and multilayer absorption can generally occur, can be by the side BET
Method quantitatively calculates the specific surface area of material by the monolayer adsorption amount of material.According to the adsorption-desorption isothermal that test obtains, meter
Calculation obtains the pore structure parameter of material, is listed in table 1.
The specific surface area and pore volume of 1 sample of table
。
As it can be seen from table 1
Obtained carbon fiber specific surface area is up to 1115.682 m2/ g, micropore specific area account for 95.8%, this is because BET compares table
The contribution that area test method micropore compares surface area is bigger.Pore volume is up to 0.5051m3/ g, the material tool illustrated
There are high-specific surface area and high porosity.
The present invention is described in detail above in conjunction with drawings and examples, still, those of skill in the art
Member is it is understood that without departing from the purpose of the present invention, can also carry out each design parameter in above-described embodiment
Change, forms multiple specific embodiments, is the common variation range of the present invention, is no longer described in detail one by one herein.
Claims (6)
1. a kind of preparation method of porous filamentous nanocarbon, includes the following steps：
（1）PVP and PAN are weighed respectively, DMF are added, stirring and dissolving obtains a concentration of 0.05~0.3 g/ respectively at 60~80 DEG C
PVP the and PAN solution of mL；
（2）PVP and PAN solution obtained by upper step is distinguished in inhalation syringe, then syringe is fixed on electrostatic spinning machine, with
PAN solution is cortex, PVP solution is that sandwich layer carries out coaxial electrostatic spinning；
（3）The tunica fibrosa being spun into heats into the water, and hollow PAN nanofibers are dried to obtain after flushing；
（4）The hollow PAN nanofibers of gained are pre-oxidized again, the pre-oxidizing conditions are：
Under the air conditions of flowing, 150 DEG C, constant temperature 3h are warming up to from room temperature with the heating rate of 1 DEG C/min, then with 0.5~2
DEG C/heating rate of min is warming up to 250~300 DEG C, keep Temperature fall after 1~5 h；
（5）Under atmosphere of inert gases, 500~700 DEG C are warming up to the heating rate of 1~5 DEG C/min, then with 1~10 DEG C/
The heating rate of min is warming up to 800~1000 DEG C, is carbonized, then is down to room temperature naturally to get porous PAN bases Nano carbon fibers
Dimension.
2. the preparation method of more carbon nano-fibers according to claim 1, which is characterized in that the step（2）In, it is described
The propeller fltting speed control of electrostatic spinning machine is 0.1~0.3mL/h, and the positive voltage control of the spinning is 15~25kV,
Vacuum cavitations are -5~0kV.
3. the preparation method of porous filamentous nanocarbon according to claim 1, which is characterized in that the step（3）In, institute
The temperature control for stating heating is 50~70 DEG C, and time control is 5~7 hours.
4. the preparation method of porous filamentous nanocarbon according to claim 1, which is characterized in that the step（3）In, institute
The temperature control for stating drying is 60~80 DEG C, and time control is 5~7 hours.
5. the preparation method of porous filamentous nanocarbon according to claim 1, which is characterized in that the step（5）In, institute
It is at least one of ammonia, nitrogen, hydrogen, argon gas to state inert gas.
6. the preparation method of porous filamentous nanocarbon according to claim 1, which is characterized in that the step（5）In, institute
The time control for stating charing is 0.2~3h.
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Cited By (7)
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| CN109305806A (en) * | 2018-11-07 | 2019-02-05 | 郑州新世纪材料基因组工程研究院有限公司 | A kind of preparation method of three-dimensional porous material |
| CN109505037A (en) * | 2018-11-08 | 2019-03-22 | 华南理工大学 | A kind of composite reinforcing material and preparation method thereof with inierpeneirating network structure |
| CN109505035A (en) * | 2018-10-30 | 2019-03-22 | 肇庆市华师大光电产业研究院 | A kind of preparation method of lithium-sulfur cell diaphragm material |
| CN111188095A (en) * | 2020-01-08 | 2020-05-22 | 苏州大学 | Triangular hollow porous fiber and preparation method thereof |
| CN111235698A (en) * | 2020-03-24 | 2020-06-05 | 北华大学 | Preparation method and application of nitrogen-doped porous carbon fiber material |
| CN113123014A (en) * | 2021-04-14 | 2021-07-16 | 闽江学院 | Raw lacquer/PAN nano fiber film and preparation method thereof |
| CN115948821A (en) * | 2023-02-21 | 2023-04-11 | 江南大学 | Hollow, porous and multi-layer polyacrylonitrile-based carbon fiber and preparation method thereof |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109505035A (en) * | 2018-10-30 | 2019-03-22 | 肇庆市华师大光电产业研究院 | A kind of preparation method of lithium-sulfur cell diaphragm material |
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| CN109505037A (en) * | 2018-11-08 | 2019-03-22 | 华南理工大学 | A kind of composite reinforcing material and preparation method thereof with inierpeneirating network structure |
| CN109505037B (en) * | 2018-11-08 | 2021-09-21 | 华南理工大学 | Composite reinforced material with interpenetrating network structure and preparation method thereof |
| CN111188095A (en) * | 2020-01-08 | 2020-05-22 | 苏州大学 | Triangular hollow porous fiber and preparation method thereof |
| CN111235698A (en) * | 2020-03-24 | 2020-06-05 | 北华大学 | Preparation method and application of nitrogen-doped porous carbon fiber material |
| CN113123014A (en) * | 2021-04-14 | 2021-07-16 | 闽江学院 | Raw lacquer/PAN nano fiber film and preparation method thereof |
| CN115948821A (en) * | 2023-02-21 | 2023-04-11 | 江南大学 | Hollow, porous and multi-layer polyacrylonitrile-based carbon fiber and preparation method thereof |
| CN115948821B (en) * | 2023-02-21 | 2023-09-22 | 江南大学 | Hollow, porous and multi-layer polyacrylonitrile-based carbon fiber and preparation method thereof |
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