CN106495142B - By the method for furfural resin preparation class grapheme material, class grapheme material and application thereof - Google Patents
By the method for furfural resin preparation class grapheme material, class grapheme material and application thereof Download PDFInfo
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- CN106495142B CN106495142B CN201610993436.4A CN201610993436A CN106495142B CN 106495142 B CN106495142 B CN 106495142B CN 201610993436 A CN201610993436 A CN 201610993436A CN 106495142 B CN106495142 B CN 106495142B
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- C01B32/00—Carbon; Compounds thereof
- C01B32/05—Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
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- H—ELECTRICITY
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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- 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
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- C01P2002/20—Two-dimensional structures
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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Abstract
The invention discloses a kind of methods by furfural resin preparation class grapheme material, pass through pyrolysismethod, it will be that raw material obtains, recyclable regenerative, degradable biological resin furfural resin by plant, under the action of additive, curing agent, it is handled by specific pyrolytic process, class grapheme material is prepared.Using technical solution of the present invention, obtain the class grapheme material with six sides or the netted two-dimentional three-dimensional crystalline structure of pentagonal, because specific atomic structure has the superelevation mechanical strength for the graphene that matches in excellence or beauty, with the excellent properties for surmounting graphene, its application is not only in the alternative grapheme material in the fields such as heat-barrier material, padded coaming, electronics and mechanical devices, and solve a great problem of puzzlement graphene lithium battery material, it is particularly suitable as the material of lithium metal and lithium ion cell electrode.The low-cost, high-volume production that can be realized such grapheme material by the preparation method, makes the material obtain batch application, has significant economic benefit.
Description
Technical field
The present invention relates to technical field of material more particularly to a kind of sides by furfural resin preparation class grapheme material
Method, meanwhile, further relate to the class grapheme material and application thereof obtained by this method.
Background technique
Graphene (Graphene) is the only one layer of atomic thickness for being stripped out from graphite material, being made of carbon atom
Two dimensional crystal, Univ Manchester UK physicist An Deliegaimu in 2004 and Constantine's Nuo Woxiao love,
Graphene is isolated in success from graphite, it was demonstrated that it can be with individualism.Graphene is that current nature is most thin, intensity is highest
Material, breaking strength is 200 times higher than best steel, while it also has good elasticity, and stretch range can reach itself
The 20% of size, in addition, graphene is almost fully transparent, the light of absorption 2.3%, and very fine and close, even most
Small gas atom (helium atom) can not also penetrate, therefore its purposes is very extensive, be electronics, optics, magnetics, biomedicine,
One of the forward position material of the fields such as energy storage most application potential is particularly suitable as the substitute of silicon, manufactures ultra micro transistor npn npn,
For producing following supercomputer, and be suitable as the raw material of transparent electron product, make transparent touch display screen,
Luminescent screen and solar panel etc..
Graphene possesses very attractive application prospect, China is to grapheme material as a kind of " miracle material "
Flow of research position is at the forefront in the world, and in recent years in flexible touch screen and field of compound material, grapheme material displays industrialization daybreak for the first time
Light, the field of electronic devices such as energy storage, sensor, chip form research hotspot, but graphene battery field, due to existing six side
The properties such as two-dimensional graphene material nanometer high-specific surface area itself are incompatible with the technical system of present lithium ion battery industry
Problem causes the limitation application in lithium ion battery.
In addition, the technology of preparing problem of graphene is the maximum " roadblock " for hindering graphene to realize potential value.It is graceful thorough
The professors of this especially big extract graphene for the first time, are directly to remove from graphite, but this original method can not
For large-scale industrial production；Most coastal waters nurse and Team Member have found by accident a kind of simple and easy prepares the new of graphene
Method, by the way that graphite flake to be placed in plastic adhesive tape, folded adhesive tape clings the two sides of graphite flake, tears adhesive tape, thin slice with
Be divided into two, constantly repeat this process, so that it may obtain more and more thinner graphite flake, but this method is for realizing batch
Production is difficult.
Summary of the invention
To solve the shortcomings of the prior art, class grapheme material is prepared by furfural resin the present invention provides a kind of
Method, the class grapheme material being prepared using renewable, degradable biological resin, performance and application match in excellence or beauty even super
More grapheme material, and there is the advantage that can be mass-produced and apply.
To achieve the above object, the method provided by the invention by furfural resin preparation class grapheme material, including it is following
Step:
A, 100 parts of furfural resin are taken, boron phosphate 2-4 parts of addition, 4-5 parts of phosphoric acid monoamine, 3-6 parts of aluminum phosphate and curing agent 2-
It 3 parts, is preheated to 26-38 DEG C and is sufficiently stirred, obtain furfural mixture；
B, furfural mixture is warming up to 60-100 DEG C, keeps the temperature 8 hours, then be warming up to 100-130 DEG C, keep the temperature 6 hours, into
Row solidification；
C, the furfural mixture after solidification is subjected to vacuum carburization, graphitization: at vacuum degree -0.1MPa, slowly heated up,
200 DEG C are risen to by room temperature with 4 minutes 1-2 DEG C of heating rates, 8-10min minutes are kept the temperature, then with 2-3 DEG C of heating in 2 minutes
Speed is warming up to 200-300 DEG C, keeps the temperature 9-12min minutes, is warming up to 300-650 DEG C with 5 minutes 1-3 DEG C of heating rates, protects
It is 12-15 minutes warm, it is warming up to 650-1000 DEG C with 6 minutes 3-4 DEG C of heating rates, keeps the temperature 10-13 minutes, then with 1 minute 5-6
DEG C heating rate be warming up to 1000-1600 DEG C, keep the temperature 40-45 minutes, be finally warming up to 1 minute 8-10 DEG C of heating rate
It 1600-2400 DEG C, is graphitized；
D, after vacuum carburization, graphitization, it is cooled to 30-40 DEG C, obtains class grapheme material product through micromechanics partition method.
As the restriction to above-mentioned technical proposal, curing agent described in step a is one in oxalic acid, phosphate or methenamine
Kind.
As the restriction to above-mentioned technical proposal, the step a is preheated using solar water heater.
As the restriction to above-mentioned technical proposal, mixing time described in step a is 10-12 minutes.
As the restriction to above-mentioned technical proposal, the step c carries out vacuum carburization using vacuum carburization furnace.
Method by furfural resin preparation class grapheme material of the invention is by pyrolysismethod, will be raw material by plant
Obtaining, recyclable regenerative, degradable biological resin furfural resin, under the action of additive, curing agent, by specific
The class grapheme material with the netted two-dimentional three-dimensional crystalline structure in six sides or pentagonal, the material is prepared in pyrolytic process processing
Though the structure of material is different from the hexagon single layer structure of grapheme material, the material can be made to obtain the superelevation power for the graphene that matches in excellence or beauty
Intensity is learned, and surmounts the excellent properties of graphene, apply alternative or even surmounts grapheme material, and passes through the preparation side
Method can be realized the low-cost, high-volume production of material, such grapheme material is made to obtain batch application, solve graphene application
Limitation bottleneck.
Meanwhile the present invention also provides a type grapheme material, it is prepared by method as described above.
The present invention also provides the purposes of above-mentioned class grapheme material, the class graphene material obtained by method as described above
Material is used as heat-barrier material, padded coaming, electronics and mechanical devices, lithium battery material.
The class grapheme material that preparation method through the invention obtains has six sides or the netted two dimension of pentagonal three-dimensional brilliant
Body structure, and do not need to pass through chemically or physically as graphene with a big interior band gap in its cellular construction
To open band gap, this atomic configuration enriches people to the understanding of carbon structure, and imparts such grapheme material for modification
Excellent performance.
The thermal stability of the class grapheme material of acquisition is high, can withstand up to 3000 DEG C of temperature, and it is special to have
Physical mechanical property, and break resistance more better than the grapheme material of six side two dimensional crystal structures and rebound toughness, and
Anti- load-bearing capacity etc., therefore it is suitable for heat-barrier material and padded coaming.Six sides of the material or the netted two dimension of pentagonal are three-dimensional brilliant
Body structure can not only be rolled into using six while or carbocyclic ring but also can be stacked into as the semiconductor carbon nanometer tube of structural motif when five
Stable three-dimensional carbon block structure, and this three-dimensional carbon material has the band gap bigger than carbon hexatomic ring and biggish body elasticity mould
Amount, can be applied to lightweight semiconductor film membrane module, electronics and mechanical devices and strain amplifier etc., especially in the electricity of nanoscale
Extensive purposes is obtained in son and mechanical devices.In addition, such grapheme material belongs to low crystallization charcoal, unique two dimension and three
Structure is tieed up with more abundant microstructure, biggish specific surface area, higher porosity, convenient for electrolyte to electrode
Dipping infiltration and electronics transmission and electrolyte flowing, be conducive to form electric double layer between electrolyte and electrode, make electrode
Material comes into full contact with electrolyte, reduces ion diffusion length and diffusional resistance, while providing conductive network structure, electronics is made to exist
It is quickly transmitted in entire electrode, there is electron conduction more higher than metal oxide and good conductivity, had excellent
Good adsorptivity, can attract deposit a large amount of electrolyte, therefore be widely used in battery electrode, super capacitor etc., the big, charge and discharge with power
Speed is fast, charge and discharge often, the advantages such as length in cruise duration, long service life.It is particularly suitable for production lithium metal and lithium-ion electric
Pond electrode material, when being embedded in lithium in the material, lithium ion can be intercalation into quickly in the aperture between microcrystalline coating neutralization, and because of this
It is mixed with phosphate mixture in class grapheme material structure, to dramatically increase battery reversible capacity, lithium battery reversible capacity can be made
Reach 529-568mA.h/g；And dendritic growth in lithium ion and lithium metal battery can be inhibited, chemical property is promoted, is mentioned
High lithium battery capacity really realizes charging more than ten minutes, i.e., to solve a great problem of puzzlement graphene lithium battery material
Can continue a journey thousands of kilometers of effect, be with a wide range of applications.
It will be successfully that raw material obtains, recyclable regenerative by plant, can in conclusion using technical solution of the present invention
The class graphene with the netted two-dimentional three-dimensional crystalline structure in six sides or pentagonal is prepared in the bio-resin furfural resin of degradation
Material, the specific atoms structure of the material assigns the superelevation mechanical strength that material matches in excellence or beauty graphene, and surmounts the excellent of graphene
Performance, application not only can in fields such as heat-barrier material, padded coaming, lightweight semiconductor film membrane module, electronics and mechanical devices
Substitute grapheme material, and solve puzzlement graphene lithium battery material a great problem, be particularly suitable as lithium metal and
The excellent material of lithium ion cell electrode.It can be realized the low-cost, high-volume of such grapheme material by the preparation method
Production makes the material obtain batch application, solves the limitation bottleneck of graphene application, has significant economic benefit.
Specific embodiment
Below in conjunction with the embodiment of the present invention, technical scheme in the embodiment of the invention is clearly and completely described,
Obviously, described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Based in the present invention
Embodiment, every other embodiment obtained by those of ordinary skill in the art without making creative efforts, all
Belong to the scope of protection of the invention.
Embodiment
The present embodiment is related to type grapheme material and its preparation method and application.
By the method for furfural resin preparation class grapheme material, comprising the following steps:
A, furfural resin is added in reaction kettle, addition boron phosphate, phosphoric acid monoamine, aluminum phosphate and curing agent use the sun
Energy water heater is preheated to 26-38 DEG C of stirring 10-12 minutes, obtains uniformly mixed furfural mixture；
B, furfural mixture is put into mold and promotes greenhouse, be warming up to 60-100 DEG C, keep the temperature 8 hours, then be warming up to
100-130 DEG C, 6 hours are kept the temperature, is solidified；
C, the furfural mixture after being fully cured is put into vacuum carburization furnace and carries out vacuum carburization: vacuumizing, in vacuum degree-
It under 0.1MPa, slowly heats up, rises to 200 DEG C by room temperature with 4 minutes 1-2 DEG C of heating rates, keep the temperature 8-10min minutes, then
It is warming up to 200-300 DEG C with 2 minutes 2-3 DEG C of heating rates, 9-12min minutes are kept the temperature, with 5 minutes 1-3 DEG C of heating rates
It is warming up to 300-650 DEG C, keeps the temperature 12-15 minutes, 650-1000 DEG C is warming up to 6 minutes 3-4 DEG C of heating rates, keeps the temperature 10-
13 minutes, then it is warming up to 1000-1600 DEG C with 1 minute 5-6 DEG C of heating rate, 40-45 minutes are kept the temperature, finally with 1 minute 8-
10 DEG C of heating rate is warming up to 1600-2400 DEG C, is graphitized；
D, after vacuum carburization, graphitization, it is cooled to 30-40 DEG C, through micromechanics partition method, carries out mechanical stripping by the required number of plies
From separation, the class grapheme material product of the required number of plies is obtained.
The proportion of each raw material component is as shown in the table in preparation method:
By the identical class grapheme material of structure is prepared shown in upper table, such grapheme material is detected with six sides
Or the netted two-dimentional three-dimensional crystalline structure of pentagonal, different from the hexagon single layer structure of grapheme material, and its cellular construction
In with a big interior band gap.
The class grapheme material of acquisition is tested for the property, 3000 DEG C of temperature can be withstood up in terms of thermal stability
Degree has break resistance more better than the grapheme material of six side two dimensional crystal structures and rebound toughness and anti-load energy
Power, therefore it is suitable for heat-barrier material and padded coaming.
The six of such grapheme material while or the netted two-dimentional three-dimensional crystalline structure of pentagonal can not only be rolled into six while or
Five side carbocyclic rings are the semiconductor carbon nanometer tube of structural motif, but also can be stacked into stable three-dimensional carbon block structure, and this
The three-dimensional carbon material of kind has the band gap bigger than carbon hexatomic ring and biggish bulk modulus, can be applied to lightweight semiconductive thin film
Device, electronics and mechanical devices and strain amplifier etc. can especially obtain in the electronics of nanoscale and mechanical devices wide
General application.
Such grapheme material belongs to low crystallization charcoal, two dimension and three-dimensional structure and permeates convenient for dipping of the electrolyte to electrode
The flowing of transmission and electrolyte with electronics, is conducive to form electric double layer between electrolyte and electrode, has than metal oxide
Higher electron conduction and good conductivity have excellent adsorptivity, and can attract deposit a large amount of electrolyte, be widely used in battery
Electrode, super capacitor etc., have that power is big, charge/discharge speed is fast, charge and discharge often, length in cruise duration, long service life etc. it is excellent
Gesture.
Such grapheme material is particularly suitable as the making material of lithium metal and lithium ion cell electrode, is embedded in material
When lithium, lithium ion can be intercalation into quickly in the aperture between microcrystalline coating neutralization, and because being mixed with phosphate mixture in material structure,
To dramatically increase battery reversible capacity, lithium battery reversible capacity can be made to reach 529-568mA.h/g；And lithium ion can be inhibited
And the dendritic growth in lithium metal battery, chemical property is promoted, lithium battery capacity is improved, really realizes charging more than ten minutes,
Can continue a journey thousands of kilometers of effect.
In conclusion using the method for the invention by furfural resin preparation class grapheme material, acquisition has six sides
Or the class grapheme material of the netted two-dimentional three-dimensional crystalline structure of pentagonal, there is the superiority for matching in excellence or beauty or even surmounting grapheme material
Can, application can not only be replaced in fields such as heat-barrier material, padded coaming, lightweight semiconductor film membrane module, electronics and mechanical devices
It for grapheme material, and solves a great problem of puzzlement graphene lithium battery material, is production lithium metal and lithium-ion electric
The excellent material of pond electrode.The low-cost, high-volume production that can be realized such grapheme material by the preparation method, makes this
Material obtains batch application, solves the limitation bottleneck of graphene application, has significant economic benefit.
Claims (6)
1. a kind of method by furfural resin preparation class grapheme material, which comprises the following steps:
A, it takes 100 parts of furfural resin, boron phosphate 2-4 parts, 4-5 parts of phosphoric acid monoamine, 3-6 parts of aluminum phosphate and 2-3 parts of curing agent is added,
It is preheated to 26-38 DEG C and is sufficiently stirred, obtain furfural mixture；The curing agent is in oxalic acid, phosphate or methenamine
It is a kind of；
B, furfural mixture is warming up to 60-100 DEG C, keeps the temperature 8 hours, then be warming up to 100-130 DEG C, keep the temperature 6 hours, consolidate
Change；
C, the furfural mixture after solidification is subjected to vacuum carburization, graphitization: at vacuum degree -0.1MPa, slowly heated up, with 4
The heating rate of 1-2 DEG C of minute rises to 200 DEG C by room temperature, 8-10min minutes is kept the temperature, then with 2 minutes 2-3 DEG C of heating rates
It is warming up to 200-300 DEG C, keeps the temperature 9-12min minutes, 300-650 DEG C is warming up to 5 minutes 1-3 DEG C of heating rates, keeps the temperature 12-
15 minutes, be warming up to 650-1000 DEG C with 6 minutes 3-4 DEG C of heating rates, keep the temperature 10-13 minutes, then with 1 minute 5-6 DEG C
Heating rate is warming up to 1000-1600 DEG C, keeps the temperature 40-45 minutes, is finally warming up to 1 minute 8-10 DEG C of heating rate
It 1600-2400 DEG C, is graphitized；
D, after vacuum carburization, graphitization, it is cooled to 30-40 DEG C, obtains class grapheme material product through micromechanics partition method.
2. the method according to claim 1 by furfural resin preparation class grapheme material, it is characterised in that: the step
A is preheated using solar water heater.
3. the method according to claim 1 by furfural resin preparation class grapheme material, it is characterised in that: step a institute
Stating mixing time is 10-12 minutes.
4. the method according to claim 1 by furfural resin preparation class grapheme material, it is characterised in that: the step
C carries out vacuum carburization using vacuum carburization furnace.
5. a type grapheme material, it is characterised in that: be prepared by method described in claim 1.
6. the purposes of a type grapheme material, it is characterised in that: the class graphene material obtained by method described in claim 1
Material is used as heat-barrier material, padded coaming, electronics and mechanical devices, lithium battery material.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610993436.4A CN106495142B (en) | 2016-11-11 | 2016-11-11 | By the method for furfural resin preparation class grapheme material, class grapheme material and application thereof |
| KR1020170148702A KR20180053250A (en) | 2016-11-11 | 2017-11-09 | Method for preparing graphene-like material from furfural resin, graphene-like material, and use thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610993436.4A CN106495142B (en) | 2016-11-11 | 2016-11-11 | By the method for furfural resin preparation class grapheme material, class grapheme material and application thereof |
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| Publication Number | Publication Date |
|---|---|
| CN106495142A CN106495142A (en) | 2017-03-15 |
| CN106495142B true CN106495142B (en) | 2019-01-08 |
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| CN201610993436.4A Active CN106495142B (en) | 2016-11-11 | 2016-11-11 | By the method for furfural resin preparation class grapheme material, class grapheme material and application thereof |
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| Country | Link |
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| KR (1) | KR20180053250A (en) |
| CN (1) | CN106495142B (en) |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112142042B (en) * | 2020-11-06 | 2022-02-11 | 无极县世易新材料科技有限公司 | Preparation method of biomass graphene |
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2016
- 2016-11-11 CN CN201610993436.4A patent/CN106495142B/en active Active
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| CN106495142A (en) | 2017-03-15 |
| KR20180053250A (en) | 2018-05-21 |
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Effective date of registration: 20201130 Address after: 241000 No.32 Chunjiang Road, Qingshui street, Jiujiang District, Wuhu City, Anhui Province Patentee after: Yang Jiawei Address before: 052460 a1-2701, 336 Heping East Road, Shijiazhuang City, Hebei Province Patentee before: SHIJIAZHUANG WORLDWIDE FURFURAL & FURFURYL ALCOHOL Co.,Ltd. |
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Effective date of registration: 20230814 Address after: 052400 North City Industrial Zone, Wuji County, Shijiazhuang, Hebei Patentee after: SHIJIAZHUANG WORLDWIDE FURFURAL & FURFURYL ALCOHOL Co.,Ltd. Address before: 241000 No.32 Chunjiang Road, Qingshui street, Jiujiang District, Wuhu City, Anhui Province Patentee before: Yang Jiawei |