CN106571450A - Method used for preparing multilayer flexible polyacrylonitrile/bitumen carbon fiber composite material used for lithium ion battery negative electrodes via electrostatic spinning - Google Patents
Method used for preparing multilayer flexible polyacrylonitrile/bitumen carbon fiber composite material used for lithium ion battery negative electrodes via electrostatic spinning Download PDFInfo
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- CN106571450A CN106571450A CN201610934426.3A CN201610934426A CN106571450A CN 106571450 A CN106571450 A CN 106571450A CN 201610934426 A CN201610934426 A CN 201610934426A CN 106571450 A CN106571450 A CN 106571450A
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- polyacrylonitrile
- bitumen
- electrostatic spinning
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- ion battery
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Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
- H01M4/366—Composites as layered products
-
- 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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
- H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/027—Negative electrodes
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention belongs to the crossing field of petrochemical engineering and carbon nano, and relates to a method used for preparing a multilayer flexible polyacrylonitrile/bitumen carbon fiber composite material used for lithium ion battery negative electrodes via electrostatic spinning. The method comprises following steps: firstly, electrostatic spinning is adopted to prepare polyacrylonitrile fiber, a mixed solution of deoiled bitumen and polyvinylpyrrolidone is subjected to electrostatic spinning so as to prepare a blend fiber which is collected on the polyacrylonitrile fiber, the former steps are repeated so as to obtain a polyacrylonitrile/bitumen composite fiber material with a multilayer structure, and pre-oxidation and carbonization are carried out so as to obtain the multilayer flexible polyacrylonitrile/bitumen carbon fiber composite material. According to the method, polyvinylpyrrolidone is capable of improving the spinnability of the deoiled bitumen solution, the polyacrylonitrile fiber is capable of supporting molten deoiled bitumen in heat processing process, so that the composite carbon material with excellent flexibility is prepared, and when the multilayer flexible polyacrylonitrile/bitumen carbon fiber composite material is taken as a lithium ion secondary battery negative electrode material, excellent performance such as high specific capacitance and excellent cycling stability is achieved. The major characteristics of the method are that: deoiled bitumen and polyvinylpyrrolidone are used for preparing the blend fiber via electrostatic spinning, and the multilayer flexible polyacrylonitrile/bitumen carbon fiber composite material is prepared based on the supporting effect of polyacrylonitrile fiber.
Description
Technical field
The invention belongs to petrochemical industry and carbon nanometer crossing domain, are related to electrostatic spinning and prepare lithium ion battery negative
With the method for layer flexible polyacrylonitrile/asphalt-based carbon fiber composite.First polyacrylonitrile fibre is prepared by electrostatic spinning,
Again Jing electrostatic spinnings prepare blend fibre and collect fine in polyacrylonitrile the mixed solution of de-oiled asphalt and polyvinylpyrrolidone
In dimension, repeat the above steps can be prepared by the polyacrylonitrile with sandwich construction/pitch complex fiber material, then through pre-oxidation
And carbonization, layer flexible polyacrylonitrile/asphalt-based carbon fiber composite is obtained.De-oiled asphalt is improved using polyvinylpyrrolidone
The spinnability of solution, the de-oiled asphalt melted in heat treatment process is supported using polyacrylonitrile fibre, is obtained with good flexible
The complex carbon material of property, shows specific capacitance height, good cycling stability etc. excellent during as ion secondary battery cathode material lithium
Performance.
Background technology
Novel nano-material and novel preparation technology continue to bring out the new contract brought for the development of lithium ion battery
Machine.Electrostatic spinning is a kind of important technical for preparing carbon nano-fiber, and made carbon nano-fiber has that diameter is little, electric conductivity
Well, the advantages of mechanical flexibility is good, is a kind of excellent lithium ion battery negative material.
Decompression residuum content is up to 40～50wt% in crude oil in China, additional in order to be translated into light oil and other height
The chemical products of value, are typically increased economic efficiency using solvent deasphalting.With mink cell focus as raw material, using propane, butane etc.
Hydro carbons is extracted as solvent, is inevitably generated a part of de-oiled asphalt (DOA).Because DOA softening points are high, viscosity
Greatly, the shortcomings of bad adhesion, the application of DOA is limited, is normally only used as road asphalt and condiment.With organic polymer and de-
Oil asphalt is raw material, and by blending fibrous material is prepared, and using the supporting role of polyacrylonitrile fibre, prepares electrochemistry
The excellent lithium ion battery flexibility negative material of energy, is expected to open up new way for the high value added utilization of mink cell focus.
The content of the invention
Electrostatic spinning prepares the side of used as negative electrode of Li-ion battery layer flexible polyacrylonitrile/asphalt-based carbon fiber composite
Method, it is characterised in that：The DMF solution Jing electrostatic spinnings of polyacrylonitrile prepare tunica fibrosa, de-oiled asphalt and poly-
Vinylpyrrolidone solution again Jing electrostatic spinnings and collect on above-mentioned polyacrylonitrile fibre membrane.Repeat the above steps, you can
To the polyacrylonitrile/asphalt material of multilayer, then Jing after pre-oxidation and being carbonized, you can obtain used as negative electrode of Li-ion battery layer flexible
Polyacrylonitrile/asphalt-based carbon fiber composite.Its concrete preparation method is as follows：
(1) the N,N-dimethylformamide solution Jing electrostatic spinnings of polyacrylonitrile prepare tunica fibrosa；
(2) solution (toluene and alcohol mixed solvent) the Jing electrostatic spinnings of de-oiled asphalt and polyvinylpyrrolidone, and receive
Collection is on polypropylene fibre film；
(3) repeat step (1), (2) prepare the material of sandwich construction；
(4) multilayer material is pre-oxidized at 200～240 DEG C, carbonization at last 600 DEG C obtains multi-layer polypropylene nitrile/drip
Blue or green flexible composite.
When made stratiform asphaltic base flexible carbon material is used as lithium ion battery negative material, product structure is stable, discharge and recharge
Capacity is high, good cycle, and is a kind of lithium ion secondary battery negative pole material having a extensive future with good pliability
Material.
Description of the drawings
Fig. 1 is the scanning electron microscope (SEM) photograph of made composite in blend fibre and embodiment 1,2,3.
Fig. 2 is sample in 100mAg-1Cycle performance curve map under current density.
Specific embodiment
It is described as follows according to the specific embodiment that technical scheme of the present invention is taken：
Embodiment 1
Take 2g polyacrylonitrile to be dissolved in 20mL DMFs, 12h is stirred at 45 DEG C, form uniform yellowish
Color solution, spinning 1.5h (concrete spinning parameters：Spinning injector advances 2 μm of s of speed-1, between collection cylinder and spinning nozzle
Apart from 15cm, voltage 20kV, drum rotation speed 400rmin-1).Take 1g de-oiled asphalts to be dissolved in 10mL toluene, be subsequently added
0.5g polyvinylpyrrolidones and 5mL ethanol, stir 12h, using mixed solution spinning 3h (concrete spinning parameters：Spinning sample introduction
Device advances 2 μm of s of speed-1, apart from 15cm between collection cylinder and spinning nozzle, voltage 15kV, drum rotation speed 400rmin-1).Polyacrylonitrile solution spinning 1.5h is reused, the fibrous material with 3-tier architecture is prepared.Fibrous material is put into into Muffle furnace
In, 240 DEG C of pre-oxidation 2h.Material after pre-oxidation is moved in high temperature process furnances, 600 DEG C of carbonization treatments 2h, obtain stratiform knot
(" C " represents material with carbon element to asphaltic base flexible carbon material C-3L (1.5/2) of structure in sample number into spectrum, and " 3L " represents that the sample number of plies is three
Layer, spinning time ratio (polyacrylonitrile fibre：Blend fibre：Polyacrylonitrile fibre) it is 1.5:2:1.5 embodiment numbering is C-
3L(1.5/2)).Embodiment 2
The preparation of the asphaltic base flexible carbon material of layer structure is with embodiment 1.The mixed solution spinning time be adjusted to 3h its
Remaining step is same as Example 1, obtains asphaltic base flexible carbon material C-3L (1.5/3) (" C " table in sample number into spectrum of layer structure
Show material with carbon element, " 3L " represents that the sample number of plies is three layers, spinning time ratio (polyacrylonitrile fibre：Blend fibre：Polyacrylonitrile is fine
Dimension) it is 1.5:3:1.5 embodiment numbering is C-3L (1.5/3)).
Embodiment 3
The preparation of the asphaltic base flexible carbon material of layer structure is with embodiment 1.Increase spinning process, secondary polyacrylonitrile is molten
Add mixed once solution-polymerized SBR and polyacrylonitrile solution spinning, and five spinning times to be 1h after liquid spinning again, obtain stratiform
(" C " represents material with carbon element to asphaltic base flexible carbon material C-5L (1.5/2) of structure in sample number into spectrum, and " 5L " represents that the sample number of plies is
Three or five layers, spinning time ratio is 1:1:1:1:1 embodiment numbering is C-5L (1.5/2)).
Embodiment 4
With embodiment 1, difference is that the ethanol solution for using polyvinylpyrrolidone replaces blending for the preparation of contrast material
Solution, remaining step is identical with example 1, obtains contrast material CFs.
Electron microscopic observation, such as Fig. 1 are scanned to made de-oiled asphalt and polyvinylpyrrolidone blend fibre and embodiment
It is shown.Wherein a is the scanning electron microscope (SEM) photograph of blend fibre, and as can be seen from the figure blend fibre is class beading fiber, attached on fiber
The de-oiled asphalt of pupa shape.B, c, d are respectively asphaltic base flexible carbon material C-3L (1.5/2) (implementing 1), the C-3L of layer structure
(1.5/3) (implement 2), C-5L (1.5/2) (implementing 3) cross section surface sweeping electron microscope, as can be seen from the figure C-3L (1.5/2),
With three-decker, intermediate layer is blended layer to C-3L (1.5/3), and C-5L (1.5/2) is with 5 Rotating fields.
Flexible polyacrylonitrile/pitch the material with carbon element of institute's layered structure is made into battery, constant current charge-discharge test is carried out, such as
Shown in Fig. 2.In 100mAg-1Current density under, charge and discharge cycles 100 times, C-3L (1.5/2), C-3L (1.5/3), C-5L
(1.5/2), CFs respectively have 448,381,515,410mAhg-1Reversible capacity.The reversible capacity of C-3L (1.5/2) sample
The CFs capacity that de-oiled asphalt is not used relatively increases, and illustrating the addition of de-oiled asphalt can improve the performance of material.But C-
The reversible capacity of 3L (1.5/3) sample is minimum, even below the reversible capacity of CFs, it may be possible to which DOA occurs in heat treatment process
Reunite, and because de-oiled asphalt amount is more, cause aggregate larger, be unfavorable for the reaction of lithium ion.C-5L in four samples
(1.5/2) with optimal reversible capacity, still there is 515mAhg after circulating 100 times-1Reversible capacity.C-5L (1.5/2) and C-
In 3L (1.5/2) sample, PAN layers are consistent with the consumption of DOA with PVP blended layers, but the amount of each layer of C-5L (1.5/2) sample
And thickness is lower, in 5 Rotating fields observed under ESEM, the thickness that de-oiled asphalt is reunited is less relative to 3-tier architecture,
The deintercalation for being conducive to lithium ion is reacted.
Claims (3)
1. the method that electrostatic spinning prepares used as negative electrode of Li-ion battery layer flexible polyacrylonitrile/asphalt-based carbon fiber composite,
It is characterized in that：The DMF solution Jing electrostatic spinnings of polyacrylonitrile prepare tunica fibrosa, then by de-oiled asphalt and
The blend fibre of polyvinylpyrrolidonesolution solution is collected on above-mentioned polyacrylonitrile fibre membrane, repeat the above steps, you can obtain
Polyacrylonitrile/the asphalt material of multilayer, Jing after pre-oxidation and being carbonized, you can obtain used as negative electrode of Li-ion battery layer flexible poly- third
Alkene nitrile/asphalt-based carbon fiber composite, its concrete preparation method is as follows：
(1) the N,N-dimethylformamide solution Jing electrostatic spinnings of polyacrylonitrile prepare tunica fibrosa；
(2) solution (toluene and alcohol mixed solvent) the Jing electrostatic spinnings of de-oiled asphalt and polyvinylpyrrolidone, and collect
On polypropylene fibre film；
(3) repeat step (1), (2) prepare the material of sandwich construction；
(4) multilayer material is pre-oxidized at 200～240 DEG C, being carbonized at last 600 DEG C, it is soft to obtain multi-layer polypropylene nitrile/pitch
Property composite.
2. to prepare used as negative electrode of Li-ion battery layer flexible polyacrylonitrile/pitch multiple for electrostatic spinning according to claim 1
The method of condensation material, it is characterised in that：The mass fraction of polyacrylonitrile solution is 10～20% in step (1), is taken off in step (2)
The mass ratio of oil asphalt and polyvinylpyrrolidone is (1～1.5):1.15～20kV of spinning voltage, pole span 15cm.Step (1)
In the spinning time be 1～2h, the spinning time in step (2) be 2～6h.
3. to prepare used as negative electrode of Li-ion battery layer flexible polyacrylonitrile/pitch multiple for electrostatic spinning according to claim 1
The method of condensation material, it is characterised in that：Can repeat step (1) and step (2) as needed, prepare the material of more numbers of plies.
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Cited By (8)
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| CN107904699A (en) * | 2017-12-21 | 2018-04-13 | 中冶焦耐(大连)工程技术有限公司 | A kind of preparation method and application of coal tar pitch base carbon fibre |
| CN108276874A (en) * | 2018-02-05 | 2018-07-13 | 西南石油大学 | A kind of preparation method of zirconium oxide/carbon composite fibre modified epoxy coating |
| CN112853547A (en) * | 2020-07-04 | 2021-05-28 | 山东八三石墨新材料厂 | Method for further preparing electrode material of supercapacitor by treating asphalt through electrostatic spinning |
| CN113224292A (en) * | 2021-02-02 | 2021-08-06 | 江西理工大学 | High-performance lithium ion battery polyacrylonitrile carbon fiber negative electrode material and preparation method thereof |
| CN113388961A (en) * | 2021-05-18 | 2021-09-14 | 武汉科技大学 | Self-bonding micro-nano porous carbon film of asphalt and polyacrylonitrile composite nanofiber as well as preparation method and application of self-bonding micro-nano porous carbon film |
| CN113871618A (en) * | 2021-09-26 | 2021-12-31 | 山东能源集团有限公司 | Petroleum asphalt-based carbon fiber flexible electrode material and preparation method and application thereof |
| CN114122363A (en) * | 2021-11-29 | 2022-03-01 | 东北大学秦皇岛分校 | Preparation method of one-dimensional porous nitrogen-rich tin antimony-carbon negative electrode material |
| WO2023087129A1 (en) * | 2021-11-16 | 2023-05-25 | 宁波杉杉新材料科技有限公司 | Preparation method for carbon electrode material and carbon electrode material |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107904699A (en) * | 2017-12-21 | 2018-04-13 | 中冶焦耐(大连)工程技术有限公司 | A kind of preparation method and application of coal tar pitch base carbon fibre |
| CN108276874A (en) * | 2018-02-05 | 2018-07-13 | 西南石油大学 | A kind of preparation method of zirconium oxide/carbon composite fibre modified epoxy coating |
| CN112853547A (en) * | 2020-07-04 | 2021-05-28 | 山东八三石墨新材料厂 | Method for further preparing electrode material of supercapacitor by treating asphalt through electrostatic spinning |
| CN113224292A (en) * | 2021-02-02 | 2021-08-06 | 江西理工大学 | High-performance lithium ion battery polyacrylonitrile carbon fiber negative electrode material and preparation method thereof |
| CN113388961A (en) * | 2021-05-18 | 2021-09-14 | 武汉科技大学 | Self-bonding micro-nano porous carbon film of asphalt and polyacrylonitrile composite nanofiber as well as preparation method and application of self-bonding micro-nano porous carbon film |
| CN113871618A (en) * | 2021-09-26 | 2021-12-31 | 山东能源集团有限公司 | Petroleum asphalt-based carbon fiber flexible electrode material and preparation method and application thereof |
| WO2023087129A1 (en) * | 2021-11-16 | 2023-05-25 | 宁波杉杉新材料科技有限公司 | Preparation method for carbon electrode material and carbon electrode material |
| CN114122363A (en) * | 2021-11-29 | 2022-03-01 | 东北大学秦皇岛分校 | Preparation method of one-dimensional porous nitrogen-rich tin antimony-carbon negative electrode material |
| CN114122363B (en) * | 2021-11-29 | 2024-03-05 | 东北大学秦皇岛分校 | Preparation method of one-dimensional porous nitrogen-rich tin-antimony-carbon anode material |
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Application publication date: 20170419 |
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