CN109546110B - Preparation method and preparation device of composite graphite electrode - Google Patents
Preparation method and preparation device of composite graphite electrode Download PDFInfo
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- CN109546110B CN109546110B CN201811344670.XA CN201811344670A CN109546110B CN 109546110 B CN109546110 B CN 109546110B CN 201811344670 A CN201811344670 A CN 201811344670A CN 109546110 B CN109546110 B CN 109546110B
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/0007—Electro-spinning
- D01D5/0015—Electro-spinning characterised by the initial state of the material
- D01D5/003—Electro-spinning characterised by the initial state of the material the material being a polymer solution or dispersion
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/0007—Electro-spinning
- D01D5/0061—Electro-spinning characterised by the electro-spinning apparatus
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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
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
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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
- H01M4/364—Composites as mixtures
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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
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
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- 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
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- 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 embodiment of the application shows a preparation method and a preparation device of a composite graphite electrode, which comprises the following steps: uniformly mixing graphite oxide and N-dimethylformamide, and adding a high-molecular polymer, urea and a zinc salt compound to obtain an electrostatic spinning solution; pouring the electrostatic spinning solution into an injector for electrostatic spinning to obtain composite nano-fibers; oxidizing the composite nano-fiber in oxygen, transferring the oxidized composite nano-fiber to a carbonization furnace, and heating and carbonizing the oxidized composite nano-fiber to obtain porous composite nano-fiber; dissolving graphene and porous composite nanofiber in a solution, and uniformly mixing to obtain a composite graphite electrode precursor solution; the composite graphite electrode prepared by the preparation method of the composite graphite electrode has the advantages of large specific capacity, good cycle stability and high rate.
Description
Technical Field
The invention relates to the technical field of composite graphite electrode preparation, in particular to a preparation method and a preparation device of a composite graphite electrode.
Background
Graphene is an important semiconductor material, and due to its small size, high specific surface area and multiple adsorption sites, the surface energy and activity of graphene are increased. Compared with other conventional semiconductor materials, the material has higher luminous efficiency and higher electron migration rate, so that the material is applied to a luminous material and an electronic device material. Due to its excellent electron conductivity and catalytic properties, there has been much research in electrochemical sensing in recent years. Meanwhile, since the surface of graphene contains more hydroxyl groups and the like, the preparation method of the graphene nanofiber, which is an adsorption material commonly used for preparing heavy metal ions, generally comprises a precipitation method, a hydrothermal method, an electrochemical deposition method and a sol-gel method. However, these methods all have some problems to different extents, such as agglomeration of the product prepared by precipitation method, high requirements of hydrothermal method for experimental equipment, and high cost of raw materials of sol-gel method although the reaction process is controllable. Moreover, the products prepared by the methods are mostly nano particles or nano films. At present, the lithium battery motor material adopted commercially only has a graphite carbon material, but the theoretical capacity of graphite is only 372mAh/g, and compared with the graphite carbon material, although some transition metal oxides have high specific capacity, huge volume change and serious particle agglomeration can occur in the lithium intercalation and deintercalation process, so that the charge and lithium ion transmission and diffusion performance is poor, and the cycling stability and rate capability as an electrode material are poor.
Disclosure of Invention
In order to overcome the problems in the related art, the invention provides a preparation method and a preparation device of a composite graphite electrode, which solve the problem that the electrode in the prior art cannot simultaneously give consideration to specific capacity, circulation and multiplying power.
The first aspect of the embodiment of the invention discloses a preparation method of a composite graphite electrode, which comprises the following steps:
uniformly mixing graphite oxide and N-dimethylformamide, adding a high molecular polymer, urea and a zinc salt compound, heating to a preset temperature, and stirring to obtain an electrostatic spinning solution;
pouring the electrostatic spinning solution into an injector for electrostatic spinning to obtain composite nano fibers;
oxidizing the composite nano-fiber in oxygen, transferring the oxidized composite nano-fiber to a carbonization furnace, and heating and carbonizing the oxidized composite nano-fiber to obtain porous composite nano-fiber;
dissolving graphene and the porous composite nanofiber in a solution, and uniformly mixing to obtain a composite graphite electrode precursor solution;
and drying the composite graphite electrode precursor solution, and then calcining to obtain the composite graphite electrode.
Optionally, the high molecular polymer is a mixture of polyacrylonitrile and polymethyl methacrylate.
Optionally, the mass ratio of the polyacrylonitrile to the polymethyl methacrylate is 1:3-2: 1.
Optionally, the zinc salt compound is a mixture of zinc nitrate, zinc oxalate and zinc chloride.
Optionally, the predetermined temperature is 65 ℃ to 75 ℃.
Optionally, after the mixture is heated to the preset temperature and stirred for 5-6 hours, the mixture is kept still for 12 hours, and then the electrostatic spinning solution is obtained.
Optionally, the electrostatic spinning has an applied voltage of 25kv, a curing distance of 16cm, a forwarding speed of 0.3mL/h, a temperature of 45 ℃ and a humidity of 65%.
Optionally, the weight concentration ratio of the graphene to the porous composite nanofiber is 1:4-2: 1.
The preparation method of the composite graphite electrode provided by the first aspect is applied, wherein graphite oxide and N-dimethylformamide are uniformly mixed, a high molecular polymer, urea and a zinc salt compound are added, and the mixture is heated to a preset temperature and stirred to obtain an electrostatic spinning solution; pouring the electrostatic spinning solution into an injector for electrostatic spinning to obtain composite nano fibers; oxidizing the composite nano-fiber in oxygen, transferring the oxidized composite nano-fiber to a carbonization furnace, and heating and carbonizing the oxidized composite nano-fiber to obtain porous composite nano-fiber; dissolving graphene and the porous composite nanofiber in a solution, and uniformly mixing to obtain a composite graphite electrode precursor solution; the preparation method of the composite graphite electrode comprises the steps of firstly preparing an electrostatic spinning solution, then preparing composite nanofibers, then preparing porous composite nanofibers, and then mixing the porous composite nanofibers and graphene to enable the graphene to enter pores of the porous composite nanofibers to prepare the composite graphite electrode.
According to a second aspect of the present disclosure, there is provided a composite graphite electrode preparation apparatus, the apparatus comprising: syringe and electrostatic discharge ware, the syringe set up in one side of electrostatic discharge ware, the top of syringe is provided with the feeder, the inside of feeder with the inside of syringe is linked together, the one end of keeping away from electrostatic discharge ware of syringe is provided with the air pump, the inside of syringe with the inside of electrostatic discharge ware is linked together, electrostatic discharge ware includes static shell, static inner shell, static needle holding chamber, static needle and discharger, the static inner shell set up in the inside of static shell, static needle holding chamber set up in the inside of static inner shell, the static needle set up in the inside of static needle holding chamber, the discharger set up in the outside of static shell, the discharger with the static needle electricity is connected.
Optionally, the number of the injectors is multiple, and the plurality of injectors are circumferentially distributed on the outer side of the electrostatic releaser.
The composite graphite electrode preparation device shown in the second aspect is used for electrostatic spinning to prepare composite nanofibers, when the composite graphite electrode preparation device is used, an electrostatic spinning solution is poured into an injector from a feeder, then the feeder is closed, an air pump is started, the electrostatic spinning solution is extruded into an electrostatic releaser from the injector, a discharger is started, the discharger releases high voltage, the needle point of an electrostatic needle is enriched with charges by the high voltage, droplets of the electrostatic spinning solution with the charges are stretched under the action of an electric field, and the composite nanofibers in a non-woven state are formed at the bottom of the electrostatic releaser. The formed composite nano-fiber is used for preparing a composite graphite electrode.
Drawings
In order to more clearly explain the technical solution of the present application, the drawings needed to be used in the embodiments will be briefly described below, and it is obvious to those skilled in the art that other drawings can be obtained according to the drawings without creative efforts.
Fig. 1 is a schematic flow chart of a method for preparing a composite graphite electrode according to an embodiment of the present invention;
fig. 2 is an overall schematic diagram of a composite graphite electrode manufacturing apparatus according to an embodiment of the present invention.
Detailed Description
In order to make those skilled in the art better understand the technical solution of the present invention, the technical solution in the embodiment of the present invention will be clearly and completely described below with reference to the drawings in the embodiment of the present invention, and it is obvious that the described embodiment is only a part of the embodiment of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example one
Referring to fig. 1, a method for preparing a composite graphite electrode according to an embodiment of the present invention is characterized by comprising the following steps:
uniformly mixing graphite oxide and N-dimethylformamide, adding a high molecular polymer, urea and a zinc salt compound, heating to a preset temperature, and stirring to obtain an electrostatic spinning solution;
pouring the electrostatic spinning solution into an injector for electrostatic spinning to obtain composite nano fibers;
oxidizing the composite nano-fiber in oxygen, transferring the oxidized composite nano-fiber to a carbonization furnace, and heating and carbonizing the oxidized composite nano-fiber to obtain porous composite nano-fiber;
dissolving graphene and the porous composite nanofiber in a solution, and uniformly mixing to obtain a composite graphite electrode precursor solution;
and drying the composite graphite electrode precursor solution, and then calcining to obtain the composite graphite electrode.
The electrostatic spinning provides a unique technology for preparing micro-nano fibers, the aperture and the porosity of the obtained electrospun fibers can be controlled, and the method is often applied to various aspects including tissue engineering, drug delivery, catalyst carriers, gas storage, sensors and the like, and is the most economical and convenient method for preparing nano fibers in the most research at present. The zinc oxide nano fiber prepared by adopting the electrostatic spinning technology has the advantages of simple and easy operation, large specific surface area, high porosity, good uniformity, easy film formation and the like, so the product can be repeatedly used when being used for manufacturing a composite electrode.
The preparation method of the composite graphite electrode provided by the embodiment one comprises the steps of uniformly mixing graphite oxide and N-dimethylformamide, adding a high molecular polymer, urea and a zinc salt compound, heating to a preset temperature, and stirring to obtain an electrostatic spinning solution; pouring the electrostatic spinning solution into an injector for electrostatic spinning to obtain composite nano fibers; oxidizing the composite nano-fiber in oxygen, transferring the oxidized composite nano-fiber to a carbonization furnace, and heating and carbonizing the oxidized composite nano-fiber to obtain porous composite nano-fiber; dissolving graphene and the porous composite nanofiber in a solution, and uniformly mixing to obtain a composite graphite electrode precursor solution; the preparation method of the composite graphite electrode comprises the steps of firstly preparing an electrostatic spinning solution, then preparing composite nanofibers, then preparing porous composite nanofibers, and then mixing the porous composite nanofibers and graphene to enable the graphene to enter pores of the porous composite nanofibers to prepare the composite graphite electrode.
Embodiment two is a method for preparing a composite graphite electrode provided in a preferred embodiment of the present invention, and is characterized in that the method for preparing the composite graphite electrode includes the following steps:
uniformly mixing graphite oxide and N-dimethylformamide, adding a high molecular polymer, urea and a zinc salt compound, heating to a preset temperature, and stirring to obtain an electrostatic spinning solution;
pouring the electrostatic spinning solution into an injector for electrostatic spinning to obtain composite nano fibers;
oxidizing the composite nano-fiber in oxygen, transferring the oxidized composite nano-fiber to a carbonization furnace, and heating and carbonizing the oxidized composite nano-fiber to obtain porous composite nano-fiber;
dissolving graphene and the porous composite nanofiber in a solution, and uniformly mixing to obtain a composite graphite electrode precursor solution;
and drying the composite graphite electrode precursor solution, and then calcining to obtain the composite graphite electrode.
Wherein the high molecular polymer is a mixture of polyacrylonitrile and polymethyl methacrylate. The high molecular polymer is a macromolecular substance with the relative molecular mass of more than 10-10 generally, and the number of atoms contained in the molecule is usually tens of thousands, hundreds of thousands or even millions of molecules. Polyacrylonitrile and polymethyl methacrylate are easily dissolved in a solvent to prepare an electrospinning solution having excellent properties.
Embodiment three is a method for preparing a composite graphite electrode according to a preferred embodiment of the present invention, and the method for preparing the composite graphite electrode includes the following steps:
uniformly mixing graphite oxide and N-dimethylformamide, adding a high molecular polymer, urea and a zinc salt compound, heating to a preset temperature, and stirring to obtain an electrostatic spinning solution;
pouring the electrostatic spinning solution into an injector for electrostatic spinning to obtain composite nano fibers;
oxidizing the composite nano-fiber in oxygen, transferring the oxidized composite nano-fiber to a carbonization furnace, and heating and carbonizing the oxidized composite nano-fiber to obtain porous composite nano-fiber;
dissolving graphene and the porous composite nanofiber in a solution, and uniformly mixing to obtain a composite graphite electrode precursor solution;
and drying the composite graphite electrode precursor solution, and then calcining to obtain the composite graphite electrode.
Wherein the mass ratio of the polyacrylonitrile to the polymethyl methacrylate is 1:3-2: 1. Tests prove that when the mass ratio of polyacrylonitrile to polymethyl methacrylate is 1:3-2:1, the prepared electrostatic spinning solution is easier to carry out electrostatic spinning treatment.
The fourth embodiment of the present invention provides a method for preparing a composite graphite electrode, which is characterized by comprising the following steps:
uniformly mixing graphite oxide and N-dimethylformamide, adding a high molecular polymer, urea and a zinc salt compound, heating to a preset temperature, and stirring to obtain an electrostatic spinning solution;
pouring the electrostatic spinning solution into an injector for electrostatic spinning to obtain composite nano fibers;
oxidizing the composite nano-fiber in oxygen, transferring the oxidized composite nano-fiber to a carbonization furnace, and heating and carbonizing the oxidized composite nano-fiber to obtain porous composite nano-fiber;
dissolving graphene and the porous composite nanofiber in a solution, and uniformly mixing to obtain a composite graphite electrode precursor solution;
and drying the composite graphite electrode precursor solution, and then calcining to obtain the composite graphite electrode.
Wherein the zinc salt compound is a mixture of zinc nitrate, zinc oxalate and zinc chloride. The zinc salt compound can increase metal ions in the solution, and the prepared electrode has better stability and better anti-interference performance under the action of heavy metal ion zinc.
Embodiment five is a method for preparing a composite graphite electrode provided in a preferred embodiment of the present invention, and is characterized in that the method for preparing the composite graphite electrode includes the following steps:
uniformly mixing graphite oxide and N-dimethylformamide, adding a high molecular polymer, urea and a zinc salt compound, heating to a preset temperature, and stirring to obtain an electrostatic spinning solution;
pouring the electrostatic spinning solution into an injector for electrostatic spinning to obtain composite nano fibers;
oxidizing the composite nano-fiber in oxygen, transferring the oxidized composite nano-fiber to a carbonization furnace, and heating and carbonizing the oxidized composite nano-fiber to obtain porous composite nano-fiber;
dissolving graphene and the porous composite nanofiber in a solution, and uniformly mixing to obtain a composite graphite electrode precursor solution;
and drying the composite graphite electrode precursor solution, and then calcining to obtain the composite graphite electrode.
Wherein the predetermined temperature is 65 ℃ to 75 ℃.
Embodiment six is a method for preparing a composite graphite electrode provided in a preferred embodiment of the present invention, and is characterized in that the method for preparing the composite graphite electrode includes the following steps:
uniformly mixing graphite oxide and N-dimethylformamide, adding a high molecular polymer, urea and a zinc salt compound, heating to a preset temperature, and stirring to obtain an electrostatic spinning solution;
pouring the electrostatic spinning solution into an injector for electrostatic spinning to obtain composite nano fibers;
oxidizing the composite nano-fiber in oxygen, transferring the oxidized composite nano-fiber to a carbonization furnace, and heating and carbonizing the oxidized composite nano-fiber to obtain porous composite nano-fiber;
dissolving graphene and the porous composite nanofiber in a solution, and uniformly mixing to obtain a composite graphite electrode precursor solution;
and drying the composite graphite electrode precursor solution, and then calcining to obtain the composite graphite electrode.
And heating to a preset temperature, stirring for 5-6h, and standing for 12h to obtain the electrostatic spinning solution.
Embodiment seven is a method for preparing a composite graphite electrode according to a preferred embodiment of the present invention, and the method for preparing the composite graphite electrode includes the following steps:
uniformly mixing graphite oxide and N-dimethylformamide, adding a high molecular polymer, urea and a zinc salt compound, heating to a preset temperature, and stirring to obtain an electrostatic spinning solution;
pouring the electrostatic spinning solution into an injector for electrostatic spinning to obtain composite nano fibers;
oxidizing the composite nano-fiber in oxygen, transferring the oxidized composite nano-fiber to a carbonization furnace, and heating and carbonizing the oxidized composite nano-fiber to obtain porous composite nano-fiber;
dissolving graphene and the porous composite nanofiber in a solution, and uniformly mixing to obtain a composite graphite electrode precursor solution;
and drying the composite graphite electrode precursor solution, and then calcining to obtain the composite graphite electrode.
Wherein the weight concentration ratio of the graphene to the porous composite nanofiber is 1:4-2: 1.
A second aspect shows an apparatus for preparing a composite graphite electrode, referring to fig. 2, the apparatus for electrospinning, the apparatus comprising: a syringe 1 and an electrostatic discharger 2, the syringe 1 being disposed at one side of the electrostatic discharger 2, the top of the syringe 1 is provided with a feeder 11, the inside of the feeder 11 is communicated with the inside of the syringe 1, an air pump 12 is arranged at one end of the injector 1 far away from the electrostatic releaser 2, the interior of the injector 1 is communicated with the interior of the electrostatic releaser 2, the electrostatic discharger 2 comprises an electrostatic outer shell 21, an electrostatic inner shell 22, an electrostatic needle accommodating cavity 23, an electrostatic needle 24 and a discharger 25, the electrostatic inner casing 22 is disposed inside the electrostatic outer casing 21, the electrostatic needle accommodating chamber 23 is disposed inside the electrostatic inner casing 22, the electrostatic needle 24 is disposed inside the electrostatic needle accommodating cavity 23, the discharger 25 is disposed outside the electrostatic housing 21, and the discharger 25 is electrically connected to the electrostatic needle 24. When the electrostatic spinning solution spinning device is used, the electrostatic spinning solution is poured into the injector 1 from the feeder 11, then the feeder 11 is closed, the air pump 12 is started, the electrostatic spinning solution is extruded into the electrostatic releaser 2 from the injector 1, the discharger 25 is started, the discharger 25 releases high voltage, the high voltage enables the needle point of the electrostatic needle 24 to gather charges, droplets of the electrostatic spinning solution with the charges are stretched under the action of an electric field, and the composite nanofibers in a non-woven state are formed at the bottom of the electrostatic releaser 2. The formed composite nano-fiber is used for preparing a composite graphite electrode.
The number of the injectors 1 is multiple, and the injectors 1 are circumferentially distributed on the outer side of the electrostatic releaser 2. Multiple syringes 1 can improve the efficiency of injection.
Other embodiments of the present application will be apparent to those skilled in the art from consideration of the specification and practice of the application disclosed herein. This application is intended to cover any variations, uses, or adaptations of the invention following, in general, the principles of the application and including such departures from the present disclosure as come within known or customary practice within the art to which the invention pertains. It is intended that the specification and examples be considered as exemplary only, with a true scope and spirit of the application being indicated by the following claims.
It will be understood that the present application is not limited to the precise procedures described above and shown in the drawings, and that various modifications and changes may be made without departing from the scope thereof. The scope of the application is limited only by the appended claims.
Claims (8)
1. The preparation method of the composite graphite electrode is characterized by comprising the following steps of:
uniformly mixing graphite oxide and N-dimethylformamide, adding a high molecular polymer, urea and a zinc salt compound, heating to a preset temperature, and stirring to obtain an electrostatic spinning solution;
pouring the electrostatic spinning solution into an injector for electrostatic spinning to obtain composite nano fibers;
oxidizing the composite nano-fiber in oxygen, transferring the oxidized composite nano-fiber to a carbonization furnace, and heating and carbonizing the oxidized composite nano-fiber to obtain porous composite nano-fiber;
dissolving graphene and the porous composite nanofiber in a solution, and uniformly mixing to obtain a composite graphite electrode precursor solution;
and drying the composite graphite electrode precursor solution, and then calcining to obtain the composite graphite electrode.
2. The method for preparing a composite graphite electrode according to claim 1, wherein the high molecular polymer is a mixture of polyacrylonitrile and polymethyl methacrylate.
3. The preparation method of the composite graphite electrode as claimed in claim 2, wherein the mass ratio of the polyacrylonitrile to the polymethyl methacrylate is 1:3-2: 1.
4. The method according to claim 2, wherein the zinc salt compound is a mixture of zinc nitrate, zinc oxalate and zinc chloride.
5. The method of claim 1, wherein the predetermined temperature is 65 ℃ to 75 ℃.
6. The method for preparing a composite graphite electrode according to claim 1, wherein the electrostatic spinning solution is obtained after the heating to the predetermined temperature, the stirring for 5-6 hours and the standing for 12 hours.
7. The method for preparing a composite graphite electrode according to claim 1, wherein the electrospinning has an applied voltage of 25kv, a solidification distance of 16cm, a forwarding speed of 0.3mL/h, a temperature of 45 ℃ and a humidity of 65%.
8. The method for preparing a composite graphite electrode according to claim 1, wherein the weight ratio of the graphene to the porous composite nanofibers is 1:4-2: 1.
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