CN105780198B - A kind of preparation method of order mesoporous carbon nano-fiber - Google Patents
A kind of preparation method of order mesoporous carbon nano-fiber Download PDFInfo
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- CN105780198B CN105780198B CN201610321026.5A CN201610321026A CN105780198B CN 105780198 B CN105780198 B CN 105780198B CN 201610321026 A CN201610321026 A CN 201610321026A CN 105780198 B CN105780198 B CN 105780198B
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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
- D01F9/24—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products from macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
Abstract
The present invention relates to a kind of preparation method and its product of the carbon nano-fiber with ordered mesopore structure.Its preparation method includes step：(1) phenolic resin, polyvinylpyrrolidone, parents notion, inorganic salts, ethanol are configured to solution according to a certain percentage；(2) electrostatic spinning prepares carbon nano-fiber precursor；(3) solidification of carbon nano-fiber precursor；(4) carbonization, pickling obtain carbon nano-fiber.This method technique is simple, cost is cheap, is adapted to large-scale continuous production.Prepared carbon nano-fiber contains abundant order mesoporous, and duct is 300 900nm parallel to fiber direction of principal axis, fibre diameter, and aperture can be adjustable in 3 20nm, and mesoporous is 80 97%, and specific surface area is 100 1000m2/ g, there is potential application in capacitor, lithium battery, catalyst carrier, pharmaceutical carrier, adsorbent etc..
Description
Technical field：
The invention belongs to nanoporous technical field of carbon fiber preparation, is related to a kind of fine with order mesoporous nanoporous carbon
The preparation method and its product of dimension.
Background technology
Porous carbon material is due to high specific surface area and flourishing porosity, preferable chemical stability, excellent
The cycle life and environment friendly of high-temperature stability, high conductance and length, therefore it is widely used in water and air
The fields such as purification, gas separation, catalysis, chromatogram, energy storage.Nanoporous Carbon fibe is as a kind of new porous carbon
Material, has higher outer surface, shorter hole depth and more homogeneous pore-size distribution and the distinctive higher shaping of fibrous material
With knitting property, it has the mass transfer rate significantly increased in adsorbing separation field, has higher energy in energy storage field
Storage density and Geng Gao high rate performance are measured, there is higher load factor and catalytic effect in catalytic field.
According to classification of the IUPAC (IUPAC) to aperture, the hole of porous carbon material can be divided into
Micropore (aperture is less than 2nm), mesopore (aperture is between 2nm and 50nm) and macropore (aperture is more than 50nm).Numerous studies table
Bright, the mesopore in Carbon Materials can not only adsorb organic macromolecule material (such as vitamin, dyestuff, humic acid, dextrin etc.), so that
The field that sewage disposal, chemical products and food decolourize etc. to be related to macromolecular is applied, and its wider duct and higher
Specific surface area can realize the high-efficient carrier of catalyst, can play Studies On The Shape-selective Catalysis as catalyst carrier.In recent years,
Carbon Materials with central hole structure double layer capacitor, fuel storage device, sensor, lithium battery, receive microreactor, even make
Also get growing concern for and apply for the new application such as bacterium and pharmaceutical carrier field.Therefore, with central hole structure
Nano carbon fiber will have broader practice prospect.
At present, mesopore nano carbon fiber typically uses nanometer shaping-later stage activation method, template-nanometer method of forming and polymerization
Its mixed-nanometer method of forming of thing.Nanometer shaping-later stage activation method be first to obtain nano carbon fiber, then carry out the later stage activate to obtain
Porous nano Carbon fibe.Ji Hyun Kim etc. use K2CO3Polyacrylonitrile-radical nano carbon fiber is activated, what is obtained porous receives
Pore size distribution during rice Carbon fibe exists between 2-7nm, specific surface area 187-704m2/g(Journal of Industrial and
Engineering Chemistry, 25, (2015) 192-198).Patent (200580045720.9) describes a kind of using golden
Category atmosphere performs etching the method to form mesopore to Carbon fibe, has 20-30nm mesopore on gained nano carbon fiber periphery..
Template-nanometer the method for forming, then it is that template is had been added in raw material presoma, is formed after fiber, mould is washed by solvent
Plate, obtain mesopore nano carbon fiber.The organic salt or inorganic salts of template including metal, the oxide of metal oxide and silicon,
Compound.The nano silicons such as Ji Sun Im, which are added in polyacrylonitrile solution, carries out electrostatic spinning, through pre-oxidation, high temperature
Mesopore nano carbon fiber, specific surface area 90-207m are obtained after charing and washing2/g(Journal of Industrial
And Engineering Chemistry, 15, (2009) 914-918).Organic blending-nanometer the method for forming, is by the way that it is blended
Fiberizing after its organic polymer, the macromolecule that addition is removed by high temperature obtain mesopore nano carbon fiber.Zeng Yue etc.
Copolymerized macromolecule nanometer pellet is blended into polyacrylonitrile solution and carries out electrostatic spinning, is just obtained in 3- through pre-oxidizing, carbonizing
The nano carbon fiber of pore size distribution, fibre diameter 100-400nm, specific surface area 104-535m during 6nm is present2/ g, mesoporous 38-
84% (Materials Letters, 161, (2015) 587-590).Patent (application number：200610052381.3) describe one
Other high-molecular copolymers are blended in kind in polyacrylonitrile, then prepare mesopore, large hole nano Carbon fiber using electrostatic spinning technique
The method of dimension.The assembly of N myristoyl Pidolidones is incorporated into polypyrrole nanofibers by patent (201210168735.6)
In, direct high-temperature process obtains chiral mesopore nano carbon fiber, specific surface area 38-277m2/g.Later stage activation is more prone to shape
Into micropore, aperture is difficult to control, and pore size distribution is wider.The nano carbon fiber specific surface area that organic blending-nanometer method of forming obtains is past
It is past relatively low.By contrast, this thinking of the template-nanometer method of forming is readily obtained the higher Nano carbon of small-bore mesopore, mesoporous
Fiber, there is certain controllability to aperture.But the hole typically resulted in is unordered hole, needs to use hydrofluoric acid using silicon systems template
Etc. hazardous agents.
The content of the invention：
The invention provides one kind to use metal inorganic salt and block copolymer as collaborative template and phenolic resin for charcoal
The preparation method and its product of the porous nano Carbon fibe with ordered mesoporous structure of presoma.This method technique is simple, adopts
It is cheap that template, cost just can be washed away with general diluted acid.Prepared nanoporous Carbon fibe contains abundant order mesoporous, duct
It is homogeneous, adjustable parallel to fiber direction of principal axis, average fibre diameter 300-700nm, aperture, specific surface area 100-1000m2/
g.Regulate and control hole knot by adjusting the ratio of metal inorganic salt/block copolymer/phenolic resin and spinning technology parameter in spinning solution
Structure and pore-size distribution.
A kind of method for preparing order mesoporous nano carbon fiber provided by the invention, is comprised the steps of：
(1) by the preparation of the ethanol solution of phenolic resin/polyvinylpyrrolidone/triblock copolymer/inorganic salts
First block copolymer is dissolved in absolute ethyl alcohol, the stirring to obtain homogeneous solution at 10-60 DEG C.After 10min, add
Metal inorganic salt, continue stirring to being completely dissolved.Then phenolic resin ethanol solution is added, continues to stir 2-5h.Finally, add
Polyvinylpyrrolidone, 10-20h is stirred, obtains uniform solution.Deaeration processing is carried out to mixed solution, then sealed at room temperature
Stand 1-3 days and obtain spinning solution.
(2) electrostatic spinning prepares carbon nano-fiber precursor；
Gained spinning solution is loaded into injection device and carries out electrostatic spinning, fltting speed 5-10uL/min, voltage 10-
35kV, two-stage spacing are 10-25cm, and spinning environment temperature is 20-35 DEG C, humidity 20%-50%.
(3) solidification of carbon nano-fiber precursor；
As-spun fibre is solidified into 1-24h in the case where being handled in 100-180 DEG C of moving air, heating rate is 1-5 DEG C/min.
(4) carbonization, pickling obtain carbon nano-fiber.
The carbonization of precursor be in an inert atmosphere (nitrogen, argon gas) with 1-3 DEG C/min to rise to 700-1100 DEG C of constant temperature 1-5 small
When, take out sample after its natural cooling afterwards.Concentration is used afterwards as 2-10wt.% hydrochloric acid, nitric acid, oxalic acid, sulfuric acid leaching
Stain stirs 1-3 days, is then washed to filtrate repeatedly as neutrality.Drying obtains porous nano Carbon fibe.
As preferable technical scheme：
A kind of preparation method of the carbon nano-fiber with ordered mesopore structure as described above, it is characterised in that phenolic aldehyde tree
Fat is thermosetting resin, mean molecule quantity 500-2500g/mol.
A kind of preparation method of the carbon nano-fiber with ordered mesopore structure as described above, it is characterised in that parents are common
Polymers is triblock copolymer, refers mainly to EO, PO, the EO for including P103, P85, F127, P123, type copolymer.
A kind of preparation method of the carbon nano-fiber with ordered mesopore structure as described above, it is characterised in that phenolic aldehyde tree
The ratio of fat and block copolymer is 2: 1-1: 5.
A kind of preparation method of the carbon nano-fiber with ordered mesopore structure as described above, it is characterised in that polyethylene
The mass fraction of pyrrolidones is 3%-6%.
A kind of preparation method of the carbon nano-fiber with ordered mesopore structure as described above, it is characterised in that inorganic salts
For magnesium nitrate, magnesium acetate, magnesium chloride, nickel nitrate, cobalt nitrate, aluminum nitrate, ferric nitrate, ferric acetate, iron chloride, nickel chloride, nitric acid
At least one of copper.
A kind of preparation method of the carbon nano-fiber with ordered mesopore structure as described above, it is characterised in that inorganic salts
Ratio with phenolic resin is 1: 2-5: 1.
Electrospinning porous carbon fiber product as described above, it is characterised in that resulting product is Jie of the diameter in 300-700nm
Hole carbon fiber, the carbon fiber contain the mesoporous of ordered arrangement, and duct is parallel to fiber direction of principal axis, and aperture can in 3-20nm
Adjust, mesoporous 80-97%, specific surface area 100-1000m2/g。
Advantages of the present invention is as follows：
Using phenolic resin as carbon precursor, metal inorganic salt, block copolymer is that collaborative template passes through electrostatic spinning technique
It is a kind of to prepare the new method with ordered mesoporous structure nano Carbon fibe, this method technique with reference to high temperature carbonization and washing process
Simply, cost is cheap, and carbon yield is high, and pollution is few, based on industrial production, is carried for the large-scale production of high-quality porous carbon fiber
An easy process route is supplied.The nano carbon fiber prepared using the above method has abundant mesopore, mesoporous height, hole
Along fiber direction of principal axis ordered arrangement, specific surface area is high, and chemical stability is good, is adapted to large-scale continuous production in road.
Brief description of the drawings
Fig. 1 is the gained nano carbon fiber SEN photos of example 2
Fig. 2 is the gained nano carbon fiber graph of pore diameter distribution of example 2.
Fig. 3 is the gained nano carbon fiber TEM photos of example 2.
Embodiment
The invention will be further elucidated with reference to specific embodiments, it should be understood that these embodiments are merely to illustrate this hair
It is bright and be not necessarily limited to the scope of the present invention.In addition, it is to be understood that after the content of the invention lectured has been read, art technology
Personnel 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
Fixed scope.
Embodiment 1：
A kind of method for preparing order mesoporous nano carbon fiber, is comprised the steps of：
(1) by the preparation of the ethanol solution of phenolic resin/polyvinylpyrrolidone/triblock copolymer/inorganic salts
First block copolymer F127 is dissolved in absolute ethyl alcohol, the stirring to obtain homogeneous solution at -10 DEG C.After 10min, add
Enter magnesium nitrate, the mass ratio of inorganic salts and phenolic resin is 1: 2.Continue stirring to being completely dissolved.Then phenolic resin is added
The ratio of ethanol solution (mean molecule quantity 500), phenolic resin and block copolymer is 1: 2.Continue to stir 2h.Finally, add
Enter polyvinylpyrrolidone, the mass fraction of polyvinylpyrrolidone is 3%.10h is stirred, obtains uniform solution.It is molten to mixing
Liquid carries out deaeration processing, and then sealing and standing obtains spinning solution in 1 day at room temperature.
(2) electrostatic spinning prepares carbon nano-fiber precursor；
Gained spinning solution is loaded into injection device and carries out electrostatic spinning, fltting speed 5uL/min, voltage 10kV, two
Level spacing is 10cm, and spinning environment temperature is 20 DEG C, humidity 50%.
(3) solidification of carbon nano-fiber precursor；
Solidify 21h under as-spun fibre is handled in 100 DEG C of moving airs, heating rate is 1 DEG C/min.
(1) carbonization, pickling obtain carbon nano-fiber.
The carbonization of precursor is to rise to 700 DEG C of constant temperature 1 hour in nitrogen atmosphere with 1 DEG C/min, treats its natural cooling afterwards
After take out sample.Use concentration to be stirred 3 days for 2wt.% salt acid dip afterwards, be then washed to filtrate repeatedly as neutrality.Dry
It is dry to obtain porous nano Carbon fibe.
The a diameter of 300-500nm of gained electrospinning porous carbon fiber, mesoporous to concentrate on 10nm, duct has along fiber direction of principal axis
Sequence arranges, mesoporous 87%, specific surface area 103m2/g。
Embodiment 2：
A kind of method for preparing order mesoporous nano carbon fiber, is comprised the steps of：
(1) by the preparation of the ethanol solution of phenolic resin/polyvinylpyrrolidone/triblock copolymer/inorganic salts
First block copolymer P123 is dissolved in absolute ethyl alcohol, the stirring to obtain homogeneous solution at 45 DEG C.After 10min, add
Enter iron chloride, the mass ratio of inorganic salts and phenolic resin is 2: 1.Continue stirring to being completely dissolved.Then phenolic resin is added
The ratio of ethanol solution (mean molecule quantity 1000), phenolic resin and block copolymer is 2: 3.Continue to stir 3h.Finally, add
Enter polyvinylpyrrolidone, the mass fraction of polyvinylpyrrolidone is 4%.13h is stirred, obtains uniform solution.It is molten to mixing
Liquid carries out deaeration processing, and then sealing and standing obtains spinning solution in 1.5 days at room temperature.
(2) electrostatic spinning prepares carbon nano-fiber precursor；
Gained spinning solution is loaded into injection device and carries out electrostatic spinning, fltting speed 10uL/min, voltage 15kV, two
Level spacing is 12cm, and spinning environment temperature is 25 DEG C, humidity 40%.
(3) solidification of carbon nano-fiber precursor；
Solidify 16h under as-spun fibre is handled in 120 DEG C of moving airs, heating rate is 2 DEG C/min.
(4) carbonization, pickling obtain carbon nano-fiber.
The carbonization of precursor is in argon gas atmosphere, rises to 800 DEG C of constant temperature 2 hours with 2 DEG C/min, treats its natural cooling afterwards
After take out sample.Use concentration to be stirred 2 days for 4wt.% hydrogen nitrate dipping afterwards, be then washed to filtrate repeatedly as neutrality.Dry
It is dry to obtain porous nano Carbon fibe.
The a diameter of 100-600nm of gained electrospinning porous carbon fiber, mesoporous to concentrate on 5nm, duct has along fiber direction of principal axis
Sequence arranges, mesoporous 90%, specific surface area 488m2/g。
Embodiment 3：
A kind of method for preparing order mesoporous nano carbon fiber, is comprised the steps of：
(1) by the preparation of the ethanol solution of phenolic resin/polyvinylpyrrolidone/triblock copolymer/inorganic salts.
First block copolymer F127 is dissolved in absolute ethyl alcohol, the stirring to obtain homogeneous solution at 50 DEG C, after 10min, added
Enter magnesium chloride, the mass ratio of inorganic salts and phenolic resin is 3: 1.Continue stirring to being completely dissolved.Then phenolic resin is added
The ratio of ethanol solution (mean molecule quantity 1500), phenolic resin and block copolymer is 1: 2.Continue to stir 4h.Finally, add
Enter polyvinylpyrrolidone, the mass fraction of polyvinylpyrrolidone is 5%.16h is stirred, obtains uniform solution.It is molten to mixing
Liquid carries out deaeration processing, and then sealing and standing (2) day obtains spinning solution at room temperature.
(2) electrostatic spinning prepares carbon nano-fiber precursor；
Gained spinning solution is loaded into injection device and carries out electrostatic spinning, fltting speed is 20 μ L/min, voltage 20kV, two
Level spacing is 15cm, and spinning environment temperature is 28 DEG C, humidity 20%.
(3) solidification of carbon nano-fiber precursor；
Solidify 10h under as-spun fibre is handled in 140 DEG C of moving airs, heating rate is 3 DEG C/min.
(1) carbonization, pickling obtain carbon nano-fiber.
The carbonization of precursor is in argon gas atmosphere, rises to 900 DEG C of constant temperature 3 hours with 3 DEG C/min, treats its natural cooling afterwards
After take out sample.Use concentration to be stirred 1 day for 6wt.% oxalic acid dipping afterwards, be then washed to filtrate repeatedly as neutrality.Dry
It is dry to obtain porous nano Carbon fibe.
The a diameter of 500-650nm of gained electrospinning porous carbon fiber, mesoporous to concentrate on 4nm, duct has along fiber direction of principal axis
Sequence arranges, mesoporous 80%, specific surface area 989m2/g。
Embodiment 4：
A kind of method for preparing order mesoporous nano carbon fiber, is comprised the steps of：
(1) by the preparation of the ethanol solution of phenolic resin/polyvinylpyrrolidone/triblock copolymer/inorganic salts
First block copolymer F127 is dissolved in absolute ethyl alcohol, the stirring to obtain homogeneous solution at 55 DEG C.After 10min, add
Enter aluminum nitrate, the mass ratio of inorganic salts and phenolic resin is 3: 1.Continue stirring to be completely dissolved then add phenolic resin second
The ratio of alcoholic solution (mean molecule quantity 2000), phenolic resin and block copolymer is 2: 5.Continue to stir 5h.Finally, add
Polyvinylpyrrolidone, the mass fraction of polyvinylpyrrolidone is 5%.18h is stirred, uniform solution is obtained, to mixed solution
Deaeration processing is carried out, then sealing and standing obtains spinning solution in 2.5 days at room temperature.
(2) electrostatic spinning prepares carbon nano-fiber precursor；
Gained spinning solution is loaded into injection device and carries out electrostatic spinning, fltting speed 30uL/min, voltage 30kV, two
Level spacing is 18cm, and spinning environment temperature is 30 DEG C, humidity 30%.
(3) solidification of carbon nano-fiber precursor；
Solidify 5h under as-spun fibre is handled in 160 DEG C of moving airs, heating rate is 4 DEG C/min.
(1) carbonization, pickling obtain carbon nano-fiber.
The carbonization of precursor is in argon gas atmosphere, rises to 1000 DEG C of constant temperature 4 hours with 2 DEG C/min, treats that it is naturally cold afterwards
But sample is taken out afterwards.Use concentration to be stirred 3 days for 8wt.% salt acid dip afterwards, be then washed to filtrate repeatedly as neutrality.
Drying obtains porous nano Carbon fibe.
Gained electrospinning porous carbon fiber a diameter of 500-700, mesoporous to concentrate on 3nm and 15nm, duct is along fiber axis side
To ordered arrangement, mesoporous 95%, specific surface area 840m2/g。
Embodiment 5：
A kind of method for preparing order mesoporous nano carbon fiber, is comprised the steps of：
(1) by the preparation of the ethanol solution of phenolic resin/polyvinylpyrrolidone/triblock copolymer/inorganic salts.
First block copolymer P123 is dissolved in absolute ethyl alcohol, the stirring to obtain homogeneous solution at 60 DEG C.After 10min, add
Enter magnesium acetate, the mass ratio of inorganic salts and phenolic resin is 5: 1.Continue stirring to being completely dissolved.Then phenolic resin is added
The ratio of ethanol solution (mean molecule quantity 2500), phenolic resin and block copolymer is 1: 3.Continue to stir 6h.Finally, add
Enter polyvinylpyrrolidone, the mass fraction of polyvinylpyrrolidone is 6%.20h is stirred, obtains uniform solution.It is molten to mixing
Liquid carries out deaeration processing, and then sealing and standing obtains spinning solution in 3 days at room temperature.
(2) electrostatic spinning prepares carbon nano-fiber precursor；
Gained spinning solution is loaded into injection device and carries out electrostatic spinning, fltting speed 10uL/min, voltage 35kV, two
Level spacing is 20cm, and spinning environment temperature is 35 DEG C, humidity 35%.
(3) solidification of carbon nano-fiber precursor；
Solidify 1h under as-spun fibre is handled in 180 DEG C of moving airs, heating rate is 5 DEG C/min.
(1) carbonization, pickling obtain carbon nano-fiber.
The carbonization of precursor is in nitrogen atmosphere, rises to 1100 DEG C of constant temperature 5 hours with 3 DEG C/min, treats that it is naturally cold afterwards
But sample is taken out afterwards.Use concentration to be stirred 2 days for 10wt.% hydrogen nitrate dipping afterwards, be then washed to filtrate repeatedly as neutrality.
Drying obtains porous nano Carbon fibe.
Gained electrospinning porous carbon fiber a diameter of 500-900nm, mesoporous to concentrate on 20nm and 5nm, duct is along fiber axis
Direction ordered arrangement, mesoporous 97%, specific surface area 604m2/g。
Claims (9)
1. a kind of preparation method of the carbon nano-fiber with ordered mesopore structure, it is characterised in that its preparation method includes following
Several steps：
(1) phenolic resin, polyvinylpyrrolidone, parents notion, inorganic salts, ethanol are configured to according to a certain percentage molten
Liquid；
(2) electrostatic spinning prepares carbon nano-fiber precursor；
(3) solidification of carbon nano-fiber precursor；
(4) carbonization, pickling obtain carbon nano-fiber.
2. a kind of preparation method of carbon nano-fiber with ordered mesopore structure according to claim 1, its feature exist
In phenolic resin be thermosetting resin, mean molecule quantity 500-2500.
3. a kind of preparation method of carbon nano-fiber with ordered mesopore structure according to claim 1, its feature exist
It is triblock copolymer in parents notion, the triblock copolymer is selected from P103, P85, F127, P123.
4. a kind of preparation method of carbon nano-fiber with ordered mesopore structure according to claim 1, its feature exist
It is 2: 1-1: 5 in the ratio of phenolic resin and parents notion, the mass fraction of polyvinylpyrrolidone is 3%-6%.
5. a kind of preparation method of carbon nano-fiber with ordered mesopore structure according to claim 1, its feature exist
In inorganic salts be magnesium nitrate, magnesium acetate, magnesium chloride, nickel nitrate, cobalt nitrate, aluminum nitrate, ferric nitrate, ferric acetate, iron chloride, chlorination
At least one of nickel, copper nitrate.
6. a kind of preparation method of carbon nano-fiber with ordered mesopore structure according to claim 1, its feature exist
In the ratio of inorganic salts and phenolic resin be 1: 1-1: 5.
7. a kind of preparation method of carbon nano-fiber with ordered mesopore structure according to claim 1, its feature exist
It is in the electrostatic spinning process parameter：Fltting speed is 5-10 μ L/min, and voltage 10-35kV, two-stage spacing is 10-
25cm, spinning environment temperature are 20-35 DEG C, humidity 20%-50%.
8. a kind of preparation method of carbon nano-fiber with ordered mesopore structure according to claim 1, its feature exist
In：Described solidification is to rise to 100-180 DEG C of constant temperature 1-24 hour with 1-5 DEG C/min, carbonization be in an inert atmosphere, wherein,
Inert atmosphere is nitrogen atmosphere or argon gas atmosphere, and 700-1100 DEG C of constant temperature 1-5 hour is risen to 1-3 DEG C/min, treats it certainly afterwards
Sample is so taken out after cooling, described pickling uses concentration to stir dipping for 2-10wt.% hydrochloric acid, nitric acid, oxalic acid or sulfuric acid
1-3 days, filtrate is then washed to repeatedly as neutrality, drying obtains carbon nano-fiber.
9. a kind of carbon nano-fiber with ordered mesopore structure, it is characterised in that the carbon nano-fiber is by claim 1
Prepared by described preparation method, the carbon nano-fiber is mesoporous carbon fiber of the diameter in 300-700nm, and the carbon fiber contains
Ordered arrangement it is mesoporous, and duct is parallel to fiber direction of principal axis, aperture 3-20nm, mesoporous 80-97%, specific surface area
100-1000m2/g。
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| CN101955180A (en) * | 2010-10-09 | 2011-01-26 | 复旦大学 | Method for preparing ordered mesoporous carbon material by direct self-assembly |
| CN103882559A (en) * | 2014-03-13 | 2014-06-25 | 中国科学院化学研究所 | High-specific surface porous carbon fiber, preparation method and application of carbon fiber |
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| "酚醛基纳米炭纤维的电纺制备及其形貌控制研究";盛杰等;《炭素技术》;20160428;第35卷(第2期);第23-27页 * |
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